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Metallurgical design of high-strength

austenitic Fe-C-Mn steels with excellent


formability (METALDESIGN)
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European Commission
Research Fund for Coal and Steel
Metallurgical design of high-strength
austenitic Fe-C-Mn steels with excellent
formability (METALDESIGN)
A. Ferraiuolo, A. Smith
Centro Sviluppo Materiali
Via di Castel Romano 100, 00128 Rome RM, ITALY
J. G. Sevillano, F. de las Cuevas
CEIT
Paseo de Manuel Lardizabal, 15, 20018 San Sebastin, SPAIN
P. Karjalainen
University of Oulu
Pentti Kaiteran Katu 1, FI-90014 Oulu, FINLAND
G. Pratolongo
Duferco
Rue des Rivaux 2, 7100 La Louvire, BELGIUM
H. Gouveia, M. Mendes Rodrigues
ISQ
Taguspark-Oeiras, Av. Prof. Dr. Cavaco Silva 33, Porto Salvo, Portugal
Contract No RFSR-CT-2005-00030
1 July 2005 to 31 December 2009
Final report
Directorate-General for Research and innovation
2012 EUR 25063 EN
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Luxembourg: Publications Office of the European Union, 2012
ISBN 978-92-79-22205-4
doi:10.2777/14874
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3

Table of Contents
Final summary..............................................................................................................................5
WP1 Testing material supply and basic metallurgical characterisation of cast materials.........13
Task 1.1 Definition of the TWIP steel compositions matrix to be investigated based on the
reference TWIP steel composition Fe-Mn-Al-Si and newer TWIP steel compositions (high C
and N).........................................................................................................................................13
Task 1.1.1 Selection of TWIP steels to be investigated.............................................................13
Task 1.1.2 Definition of the TWIP steels compositions matrix.................................................14
Task 1.2 Laboratory VIM ingot casting.....................................................................................16
Task 1.3 - Solidification structure characterisation....................................................................16
WP2: Fundamental investigations on the physical metallurgy of TWIP steels.........................23
Task 2.1 Measure of SFE by means of Transmission Electron Microscopy observations of
extended nodes. Evaluation of Ms
>
temperature...................................................................23
Task 2.1.1: Measure of SFE by means of TEM observation of extended nodes.......................23
Task 2.1.2 Evaluation of the Md of TWIP steel variants...................................................26
Task 2.2: Characterization of recrystallization behaviour .........................................................27
Task 2.2.1 Critical strain for DRX initiation, flow stress, peak stress,......................................27
Task 2.2.2 Recrystallization kinetics under different cold rolling schedule..............................41
Task 2.2.3 Modelling of recrystallization behaviour of TWIP steels by modifying the available
mathematical models for austenitic steels and the relevant constitutive equations...................45
Task 2.3 Study of the precipitation at equilibrium by means isothermal treatments. Precipitates
analysis by means of electron microscopy techniques (SEM-EDX, extraction replica for TEM).
....................................................................................................................................................48
Task 2.4 Industrial feasibility of hot and cold processing route of TWIP steels.......................58
WP3 Study of the deformation mechanisms and strain hardening behaviour...........................69
Task 3.1 Characterization of mechanical properties in relation with the microstructure,
dominating deformation mechanism, strain rate and temperature.............................................69
Task 3.1.1 Static uniaxial tensile tests to investigate the deformation mechanisms transition
(deformation twinning -->dislocation glide) and strain hardening behaviour..........................69
Task 3.1.1.1 Quasi static tensile tests and strain hardening behaviour analysis........................69
Task 3.1.1.2 Characterization of austenite phase stability and microstructural evolution in.....75
Task 3.1.1.3 Investigation on TWIP steel embrittlement...........................................................83
Task 3.1.2 Dynamic Tensile Properties....................................................................................91
Task 3.1.3. Torsion tests in the 20C-450C temperature range: stress-strain behaviour at large
strains.........................................................................................................................................94
Task 3.1.4 Hot ductility curves in the temperature range 700 1300 C by means of a Gleeble
simulator...................................................................................................................................101
Task 3.1.5. Study of the influence of grain size in the tensile stress-strain behaviour of TWIP
steels (Hall-Petch behaviour)...................................................................................................105
Task 3.2 Bending fatigue tests to determine the fatigue strength and cyclic softening/hardening
behaviour and to analyse the crack initiation/propagation stages............................................109
Task 3.3 Evaluation of impact strength by means of Charpy tests at different temperature.111
Task 3.4 Plain strain compression tests....................................................................................113
WP 4 Basic characterisation of application properties: formability, weldability and coating
ability........................................................................................................................................115
Task 4.1 Formability characterisation by means of Erichsen test and High-velocity forming
tests...........................................................................................................................................115



4

Task 4.1.1 Erichsen test ..........................................................................................................115
Task 4.1.2 High-velocity forming tests.................................................................................116
Task 4.2 Laboratory coating tests and coating layer characterisation...................................117
Task 4.3 Characterization of Weldability.............................................................................121
WP5: Industrial trial .................................................................................................................135
Task 5.1 Selection of the most interesting TWIP steel variant, for automotive applications, on
the basis of the previous WPs results.......................................................................................135
Task 5.2 Coil supplying and material processing (hot and cold rolling, annealing treatments,
pickling and coating)................................................................................................................137
Objectives of the project..........................................................................................................143
Exploitation and impact of the research results.......................................................................145
List of figures and tables..........................................................................................................145
List of References.....................................................................................................................151



5

Final summary
Twinning induced plasticity (TWIP) steels are austenitic steels characterised by good combination
between high tensile properties and high ductility. This behaviour is due to the characteristic high work
hardening rate determined by the occurrence of deformation induced twinning during deformation.
These properties are extremely attractive for automobile applications expecially for parts devoted to
energy absorption (crashworthiness) and for structural reinforcement (body in white).
TWIP steels are characterised by
Austenite phase stability obtained with carbon and high manganese content (typically
>16%).
Low stacking fault energies (SFE) leading to the ability to be deformed by means of
both dislocation slip and mechanical twinning. The relative intensity of deformation
mechanisms depends upon the chemical composition (mainly the carbon and
manganese contents) .
The main objectives of this project are:
1. To complete the understanding of the TWIP steel metallurgy particularly for what regard
the following fields:
Solidification microstructure;
Recrystallization behaviour (dynamic and static) and texture formation.
Tensile properties and work hardening ability, precipitation behaviour as a function of
the steel chemical composition and its influence on the strip properties.
Influence of steel chemical composition on microstructure, mechanical properties,
strain hardening behaviour as well as on application properties such as formability,
weldability and coatability.

2. To design a metallurgically based manufacturing route (hot/cold rolling process, annealing
treatment) taking into account the specific capability of the DUFERCO plants.


WP1: Testing material supply and basic metallurgical characterisation of cast materials
This research started on defining the basic rules for the metallurgical design of TWIP steels. Five
TWIP steel variants were selected on the basis of austenitic phase and low SFE. The variants were of
two main type Fe-Mn-Si-C-N and Fe-Mn-Al-Si-C.


Table FS1: Chemical composition of the TWIP steels casted at vacuum induction melting (%wt).


Of these five TWIP variants the first variant (TWIP1) revealed a mixed primary solidification structure
with austenite+ferrite. The ferrite phase is stable also at room temperature (Fv=6%). The remaining 4
TWIP steel variants (TWIP2-3-4-5) revealed a fully austenitic dendritic solidification. The austenitic
phase is stable down to room temperature. Microsegregation associated to dendritic solidification
determine zone with lower local SFE (low Mn and C). In these zones the presence of -martensite was
detected.



6

WP2: Fundamental investigation on the physical metallurgy of TWIP steels
The investigations carried out on the physical metallurgy of TWIP steels revealed the following results:

Task 2.1.1
The SFE of TWIP2 steel was measured by means of TEM of extended nodes size produced by
interaction of extended dislocations.
The average SFE value for TWIP2 steel resulted of 21.4 mJ /m
2
. The standard deviation of SFE values is
consistent with other measurements reported in literature.
The comparison with thermodynamical model reveal that the Dumay model gives the best correlation
with the measured SFE for TWIP2. The model of Dumay predicts that the variant TWIP 1, 3, 4 and 5
should have SFE values below 18 mJ m
-2
.

Task 2.1.2
The temperature for deformation induced transformation M
d30

was evaluated for TWIP2, TWIP3


and TWIP5 and the values are respectively -170C, -145C and -72C. These results again confirm that
TWIP 2 and TWIP3 are the steel grades revealing the best microstructural stability and TWIP effect
during deformation even at quite low temperature.

Task 2.2.1
Hot deformation resistance of high-Mn TWIP steels is dependent on Mn content (strengthening about 2
MPa/wt%) and increases with increasing Al alloying up to 6% (strengthening about 12 MPa/wt%). Nb
and N in the contents used here in steels have a minor influence. The austenitic high-Mn TWIP steels
exhibit higher deformation resistance than those of low-C, C-Mn-Nb and austenitic stainless steels.
Flow stress curves exhibit broad stress peaks at quite low strains. However, the completion of DRX
occurs slowly. Very fine grain size is obtained as a result of DRX. SRX kinetics of TWIP steels is faster
than that of Type 304 and C-Mn-Nb steels and slower than that of low-C steels. Mn is the main element
retarding the rate of SRX and Al has only a minor contribution. The regression equation for the static
recrystallization kinetics for TWIP steels can be used to predict the SRX rate under given conditions.
Grain size is refined effectively by SRX.

Task 2.2.2
Recrystallized grain sizes of TWIP steel of 22% Mn - 0.6% C (in mass-%) cold rolled in the range
of 40%-70% reductions and isothermally annealed in the temperature range 600 C T 900 C are
very small, D 2 m.
At 450C the effect of annealing is very weak. After some seconds there is some hardening (static
ageing by solid solution segregation to dislocations) and a very weak softening thereafter,
attributable to recovery, without any noticeable metallographic changes.
Above 700 C, recrystallization is complete in less than nine minutes and takes less than ten
seconds above 800 C. At 900 C T 1100 C, the kinetics observed only corresponds to grain
growth.
Recrystallization and grain growth textures are very weak. Consequently, the elastic and plastic
anisotropies of annealed TWIP sheets will be negligible.
Although there is no apparent texture change from recrystallization to grain growth, there is a
strong change in the grain boundary composition. The fraction of 3 twin boundaries increases
suddenly from 14% to 40% when grain growth starts and it remains constant thereafter
independently of the grain size reached.
An empirical equation of grain growth for this steel has been obtained with an apparent activation
energy QGG =363 60 kJ /mol and an exponent nGG 3.9.



7

Task 2.2.3
Physically based recrystallization models have been applied to the experimental data for cold rolled and
annealed TWIP steel. Several models were considered with different assumptions for the nucleation
behaviour and boundary velocity behaviour. All the models have assumed that grain boundary mobility
was controlled by interaction with manganese solute atoms. The possible influence of twins on the
recrystallization process was not considered. From the modelling results the following conclusions can
be drawn:

The model which best described the experimental data assumed that the nucleation was site
saturated and the grain boundary velocity decreased with time due to static recovery.
Comparison of this model with more experimental data revealed good agreement when the
nucleation density was a free model parameter.
Imposing an average nucleation density and recalculating recrystallization curves still gave
reasonable agreement with experimental results.

Task 2.3
The precipitation behavior of TWIP steel depends on one side on the C, N, and other elements carbide-
nitride formers (Ti, Al, Nb, V) content. On the other side the precipitation behavior is strongly affected
by thermodynamic stability of austenite in the range 500-700C. Infact the ternary system Fe-Mn-C
under particular conditions of temperature and chemical composition forese that the austenite could
partially transform in ferrite+carbides (pearlite like structure).
The study carried out on TWIP steels by SEM-EDS and STEM-EDS allows to state the following
conclusions:
Both TWIP1 and TWIP4 show, at temperature below 700C the tendency of austenite to
destabilize and to forme ferrite+carbide structures. These observation is in agreement with other
results achieved on TWIP1-4 and confirm that the austenite stability of these steel grades is
lower with respect to reference grade TWIP2 (Fe-22Mn-0.6C);
TWIP2 and TWIP3 show a similar behavior. Both steel variants revealed a massive carbide
precipitation of cementite type (Fe, Mn)
3
C in the range 500-700C. No ferrite phase was
detected in the range 500-700C.
TWIP5 variant reveals a very stable structure: no massive carbide precipitation was detected in
the range 500-700C. The precipitated particles are constituted of cementite carbides and fine
(Ti,Al) carbo-nitrides. No ferrite phase was detected even after long soaking time in the range
500-700C.
Task 2.4
The task 2.4 was focused on demonstrating the feasibility of TWIP steel production at Duferco La
Louviere steel works and to define the industrial conditions for TWIP steel processing. The results of
the study allowed to conclude that TWIP steel hot rolling is feasible at Duferco La Louviere plant,
provided that a dedicated operating practice, quite different from conventional low C-Mn steel, can be
adopted. This is the result from the point of view of plant capability.
On the other side the impact on the production schedule due to the insertion of a mini-program of TWIP
steel has been evaluated in terms of costs, time, fuel consumption, etc. Summarising the operating
practice for hot rolling process of TWIP steel production at DLL are:
Slab dimensions: thickness 250mm, width 1000mm, length 5000mm;
Slab discharging temperature range: 1180-1220C;
Entry finishing temperature range: >1040C;
Finishing rolling temperature: 900-920C;



8

Hot band thickness achievable >4.0 mm;
Coiling temperature: 450-500C.
Hot rolled strip pickling: conventional pickling process as adopted for C-Mn steel (HCl acid).


WP3: Study of the deformation mechanisms and strain hardening behaviour

Task 3.1.1.1
All the TWIP steel variants investigated revealed excellent tensile properties. However significant
differences are present in terms of deformation mechanisms and microstructural evolution during
deformation. The tensile properties resulted to be quite sensitive to the specimen surface preparation but
the investigation of this phenomena is reported in the task 3.1.1.3.
Temperature effect
The tensile properties of TWIP steel grades show a quite similar behaviour at increasing temperature
with only some quantitative differences. The yield stress is slightly affected by temperature while the
tensile strength is significantly influenced by temperature. This means that at higher temperature the
Ys/UTS ratio tends to increase due to progressive change of the deformation mechanism
(twinningdislocation glide) and a consequent reduction of the strain hardening ability and elongation
is detected.
Strain rate effect
For equivalent plastic strain below 0.25, the behaviour of TWIP steels is very similar at room
temperature and the strain rate influence on the strength is very weak. Only at very high strain rates
( 200 >
&
s
-1
) there is a small strain rate induced increment of the flow stress.
Strain hardening ability
The main characteristic of a true TWIP steel (TWIP2 and TWIP3) is the presence of a intermediate
stage in the strain hardening curve the instantaneous coefficient n increase with strain. This should be
related to the effect of deformation induced twinning occurring after the first stage of the curve
predominated by dislocation glide. The new twins act as barriers to dislocation motion, and lead to an
increase in strain hardening rate. Depending on the extent of twinning, this leads to the observed overall
hardening rate.
The other TWIP grades (TWIP1,4,5) are characterised by a lower austenite stability and this is
demonstrated by the occurrence of martensite ( or ) during deformation or presence of ferrite also at
zero strain as for TWIP1.
The strain hardening of TWIP 1,4,5 grades show a slight different behaviour as a function of strain, due
to the complex combination of deformation mechanisms (twinning+dislocations) and deformation
induced phases (-martensite and -martensite).

Task 3.1.1.2
The results of this task can be summarized in the following topics:
TWIP2 and TWIP3 are characterized by largest stability of austenite phase under deformation
from 250C down to -180C. Within this temperature range the deformation induced twinning
represent the main deformation mechanism. At temperature of 350C both steels do not reveal
deformation induced twinning.
TWIP1, TWIP4 and TWIP5 XRD pattern analysis revealed the occurrence during deformation
at room temperature in addition of deformation induced twinning (TWIP effect) even formation
of second martensitic phases ( and ). This tendency became stronger at low temperature due
to decrease of SFE. Since the fraction of epsilon martensite increases continuously with strain,
it is suggested that alpha martensite forms directly from austenite and not through the two-step
transformation where epsilon martensite is the intermediate phase. The occurrence of
deformation induced twinning disappears before 250C.



9

Task 3.1.1.3
The results achieved can be summarized in the following points:
The results of the investigations carried out in the present task 3.1.1.3 allow to argue that the
embrittlement problems of TWIP steels are mainly related to decarburization and Mn depletion
producing a mixed +microstructure in the subsurface zone.
Carbon and manganese concentration profiles on TWIP steels show that both C and Mn are
depleted in the subsurface zone due to annealing treatment under decarburizing atmosphere. It
is worthy to note that the depth of Mn depleted zone (typically <30m) is significantly lower
than C decarburized layer.
All the TWIP samples annealed at 1000C and 1200C reveal in the subsurface zone a mixed
microstructure +' even without any deformation with a resultant magnetic behavior The
presence of '-martensite is due to the local lowering of SFE in the C and Mn depleted zone.
TWIP2,3,4,5 steels reveal a similar behavior that is in good agreement with the theory of
decarburization in austenitic phase (Birks-J ackson model) strictly related to bulk carbon
diffusion. The decarburization depth is more sensitive to annealing temperature (exponential
dependence) with respect to soaking time (t
1/2
dependence).
The decarburization depth of TWIP steels is larger than carbon steel probably because for
austenitic steels the carbon is in solid solution and is ready to react with oxygen. The kinetics of
decarburization of a medium carbon steel (C45) on relatively short time is decreased by phase
transformation +pearlite . During this transient the formation of a ferrite layer on the strip
surface could slow down the steel decarburization kinetics.
In terms of decarburization the final annealing process (after cold rolling) could be critical. For
this treatment a controlled annealing furnace atmosphere have to be considered in order to
avoid the occurrence of decarburization and so the formation in the subsurface zone of a mixed
+ microstructure.
Tensile tests (=10
-2
s
-1
) carried out on samples with different hydrogen content show similar
tensile properties. The elongation to rupture of hydrogen charged specimen is markedly higher
than the strip sample with a surface decarburized layer (impaired by presence of martensite in
the microstructure).
The high desorption temperatures indicate that the hydrogen is trapped by high energy bonding.
This result would suggest that the diffusible hydrogen can be considered negligible. Therefore,
under plastic deformation the hydrogen absorbed cannot move so easily to reach dislocation
and/or crack tip, creating favourable condition to brittle fracture.

Task 3.1.2
The stress ratios (the yield stress to the tensile strength) of TWIP steels are much lower than those of
the low C cold drawing steels under quasi-static conditions. This means TWIP steels promoted higher
strain hardening potential. Under dynamic tensile conditions, stress ratios of TWIP steels increased as a
result of increasing yield strength, but they are still lower than those of the low C cold drawing steels.
Furthermore, the n-values of TWIP steels from dynamic tensile tests are much higher than those of
conventional automotive steels.
The enhancing of the ductility, strength and strain hardening of material is advantageous for crash
energy absorbing characteristics.
TWIP steels promoted higher ductility and higher strain hardening with high strength, and therefore
TWIP steels have higher crash energy absorption and consequently higher crash safety than steels
TRIP700, DP600 and H340LAD.

Task 3.1.3
The hot torsion results show a strong temperature effect in the strength level and an important effect of
strain rate in the ductility. The trend of the behaviour is common for the four steels investigated



10

(TWIP2,3,4,5), although TWIP3 is clearly more ductile that the other three compositions. A change in
the behaviour from cold-work to warm/hot-work occurs at about 250C. At the highest strain rate and at
low temperature, the initial strain hardening rate is much higher than its static counterpart, a fact that
could be linked to an enhancement of the twinning activity at high strain rates. However, only TWIP2
and TWIP3 below 250C clearly behave as expected from TWIP steels, with the typical hardening stage
associated to profuse deformation twinning. In all other cases the work hardening is an approximately
linearly decreasing function of the flow stress soon after the yield stress, a behaviour characteristic of
dislocation-mediated plasticity controlled by dynamic recovery.

Task 3.1.4
The hot ductility curves of the TWIP steel variants show quite good high temperature performances.
The hot ductility in some cases, such as for TWIP 3 and TWIP2 (RA>60% between 700-1200C), is
higher than that of the austenitic AISI 304.

Task 3.1.5
The yield stress for 0.2% plastic elongation clearly shows a grain size dependence. The Hall-Petch
constant found for TWIP2 steel grade is =
HP
K 356.5 MPa m
1/2
.
The results of this task allowed to achieve a better description of the grain growth kinetics of the
TWIP2 steel. It is worthy to note that for fine grain size (<10m) the twin boundary fraction is
significantly lower than for larger grain size. This means that the TWIP effect is dependent on grain
size and the best performances are relevant to a grain size in the range 15-30m.

Task 3.2
The fatigue behavior of three high-Mn TWIP steels, with slightly different Mn contents (between 16
and 22 wt.%) and Nb or Al alloying were investigated using reversed bending loading and examining
the cyclic damage features on surfaces. The main conclusions can be drawn as follows:
Fatigue behavior of three TWIP steels is quite identical. Fatigue stress limit (the cyclic life
beyond 2x10
6
cycles) is well above their yield strength values. The ratio of fatigue limit/tensile
strength is 0.42-0.48 that is quite a similar value as commonly observed for various carbon
steels and for Types 301LN and 316L austenitic stainless steels.
During cyclic loading, planar slip bands are formed in an early stage of fatigue life consisting of
extrusions and intrusions. With continuing cycling, the slip bands intersect with grain
boundaries as well as annealing twin boundaries producing local strain concentrations that
induce microcracks at these boundaries.
Fatigue crack embryos nucleate at an early stage of fatigue life (25%) at sites of intersections
of slip bands and grain boundaries as well as annealing twin boundaries.
Crack propagation takes place along slip lines, grain and twin boundaries but the overall path is
mainly transgranular in its character. In this stage, ductile striations are formed on fracture
surfaces.
Microcracks link and propagate readily along grain boundaries indicating some degree of
inherent grain boundary weakness, as suggested in the literature for austenitic high-Mn steels.
Neither mechanical twins nor -martensite are formed during cyclic loading in the investigated
TWIP steels, so that the TRIP or TWIP effects seem to play no role in the course of high-cycle
fatigue.
The degree of cyclic hardening revealed by hardness is strongly dependent on the grain size
decreasing with refined grain size.
Refinement of the grain size improves significantly the fatigue strength of the 0.6C-22Mn
TWIP steel.




11

Task 3.3
Comparing the Charpy values of TWIP variants arise that TWIP1 reveals the best results at all tested
temperature. TWIP2 and TWIP3 are slightly better than TWIP4 and TWIP5. Qualitatively the Charpy
energy behavior of TWIP steels as a function of the temperature is quite similar to stainless steels such
as AISI304. In fact the Charpy energy remains of the same order from +150C down to -50C, with a
slight increase from RT down to -50C.

Task 3.4
The work hardening of TWIP2,3,4,5 steels is significantly higher than stainless steels; at a true strain of
0.5 the difference in terms of stress is about 38%. The above result implies difficulties in cold rolling in
terms of loads, number of passes or reduction ratio at each stage.
Depending on the hot strip thickness, an intermediate annealing treatment (two step cold rolling
process) could be necessary for obtaining the aimed final cold strip thickness (<2.0 mm).


WP 4: Basic characterisation of application properties: formability, weldability and coatability

Task 4.1
It can be seen that variation among the steels is quite small. Generally, the Erichsen Index (IE) is higher
if the elongation is higher, and the best values are obtained for TWIP2. However, better IE values were
obtained at high-speed Erichsen testing.
This can be attributed to the adiabatic heating of the sample during the tensile test increasing the SFE
and resulting in decreasing density of mechanical twins. However, with increasing the strain rate up to
1000 s
-1
, the total elongation increases again reaching values above that in tensile testing at the strain
rate of 0.1 s
-1
,
It is possible to make comparison between the elongation in dynamic tensile tests ( 1000 & s
-1
) using
the Hopkinson split bar method and that in quasi-static tensile tests. Then, for example, for TWIP2 the
total elongation is 83% under quasi-static tension and 80% under high-speed tensile testing, i.e. the total
elongation in these two cases is almost equal.
In the conventional Erichsen testing according to the DIN 50101, the typical strain rate can be estimated
to be order of 0.01 s
-1
. (For instance, no 0.4 cylinder speed is 0.56 mm/s). In high-speed Erichsen
testing, where the speed of impact front is about 200 m/s, the strain rate can be order of 5 s
-1
(dome
height 10 mm; at 200m/s it takes 0.05 s. Strain is 0.26, hence, the strain rate =0.26/0.05s =5/s), i.e.
about 500 times higher.

Task 4.2
The visual control of galvanized samples surfaces revealed a general uniformity of the coating layer.
Coating adhesion test was made and as a results all the tests were acceptable according to the standard
since no detachment of any small square was verified. No noticeable differences were detected between
the two pre-treatments in the galvanized adhesion layer test. All the samples after the galvanization
process revealed the typical galvanization structure. The batch hot-dip galvanized coating consists of a
series of zinc-iron alloy layers with a surface layer of almost pure zinc. The alloy layer is as much as
50% of the total thickness and it consists of two or more distinct zinc/iron layers. Each layer has a
specific amount of iron and zinc.

Task 4.3
To assess the weldability as well as its main influencing factors, experimental laser welding analysis of
four TWIP has been performed.
The work allowed to conclude that the joining of TWIP steels is easily achievable by laser welding. The
factors that determine the good welding behaviour and quality of TWIP steels are intrinsically related to
the steel composition and austenitic structure.



12

Concerning the dissimilar steel welding all the weld and heat affected zones present acceptable
hardness values which indicates the mechanical properties of the base materials are matched or
improved after laser welding. This study permitted to prove the good potentialities of TWIP materials
on automotive applications where the welding ability is one the the main requirements.

WP 5: Industrial trial

Task 5.1
TWIP3 is the selected TWIP grade to be casted at Duferco steelworks. TWIP3 steel variant (chemical
composition reported in following table) is characterized by a markedly lower Mn content that is the
most expensive element in TWIP steels and, as well known, the element that could have unwished
impact on environment during steel making due to Mn evaporation. The properties revealed by this
steel if, in some instance, are below the TWIP2 are really promising and could be further improved by
means of a fine tuning of the alloy design and industrial processing conditions. Up to now no patent
application has been submitted.

Fe Mn C Si Nb
min bal 16.00 0.60 0.20 0.015
max bal 17.50 0.65 0.30 0.030
Table FS2: Range of elements of the TWIP steel selected for industrial trial (TWIP3).


Task 5.2
TWIP steel industrial heat was not performed due to the stronger than expected relevance of the
following issues:
Hydrogen embrittlement susceptibility of high Mn steel. To minimize this risk the heat was
postponed in order to wait for the installation of a VD facility at Duferco steelworks aiming to
achieve a significant reduction of hydrogen content in steel. Unfortunately several causes
determined a larger delay of the VD facility completion inclusive, of course, the recent steel
markets crisis that widened the time for VD installation and commissioning work.
Definition of the steelmaking route of high Mn steel using a direct current electric arc
furnace (DC-EAF). The feasibility of TWIP steel on a direct current arc furnace required a in
depth study of interactions between high Mn steel and furnace soils electrodes to avoid furnace
damagement. The conclusion of this study yielded to state the feasibility of a high Mn steel.
However some countermeasures were introduced in the steelmaking operating practice to
increase the EAF safety, among which, minimization of the Mn melting time and hence the
interaction time between Mn and EAF soil electrodes and, before the heat, assessment of the
consumption status of the soil electrodes.



13

Scientific and technical description of the results

WP1 Testing material supply and basic metallurgical characterisation of cast materials

Task 1.1 Definition of the TWIP steel compositions matrix to be investigated based on the
reference TWIP steel composition Fe-Mn-Al-Si and newer TWIP steel compositions (high C and
N).

Task 1.1.1 Selection of TWIP steels to be investigated
The first task of the project consisted in the definition of the TWIP steel compositions to be
investigated. After a in depth discussion between the partners it was decided to select 2 reference TWIP
steel chemical compositions on the basis of the literature survey. The reference TWIP steels were
selected for two order of reasons:
1. To investigate the basic metallurgical properties of TWIP steel according to the technical annex
and
2. To evaluate the effect of different alloying solutions on TWIP steel properties.

The reference TWIP steel selected were:
1. Fe-22Mn-3Al-3Si
2. Fe-22Mn-0.6C

In addition to the reference TWIP steel, further 3 TWIP variants were proposed. The scope of the
introduction of additional TWIP variants to be investigated was to investigate the effect of different Mn,
Al, Si, C, N content on:
metallurgical properties such as SFE, tensile properties, hot and cold deformation properties,
etc.
application properties: coating ability, welding ability;
manufacturing route: from hot rolling up to final cold processing route.

On the basis of the above considerations it was decided to investigate on TWIP steels variants with the
following alloying modifications:

a) Lower Mn content (16-18%) could be exploited in order to reduce the heat costs and the
enviromental problems related to high Mn evaporation during steelmaking process;

b) Al addition in order to stabilize with respect to phase.

c) Addition of C and N to achieve the optimal SFE value and austenite stability but avoiding
precipitation of carbide/nitride during heat treatments or high temperature treatments. The addition of
N, in partial substitution of C, will be tested also to verify the influence on the mechanical properties.
d) Nb addition: Nb is reported in literature to have a positive effect on SFE but the effectiveness is still
unclear.

Summarising the steels to be investigated are reported in the following table. The reference steel are
well defined in terms of composition while for the additional TWIP variant TWIP3-4-5 calculations of
the SFE, by means of thermodynamical models, are necessary.








14


TWIP
variant
Mn C N Al Si Nb
TWIP1
(ref.)
22 0.01 - 3.0 3.0 -
TWIP2
(ref.)
22 0.6 - - 0.2 -
TWIP3 18-22 0.6 - - 0.2 0.02
TWIP4 16-18 0.6 - 1.5 - -
TWIP5 18-22 0.2-0.3 0.2-0.3 - 0.2 -
Table 1.1.1.1 Selected TWIP steel compositions (Fe balance).


Task 1.1.2 Definition of the TWIP steels compositions matrix
Thermodynamic model for SFE
The SFE plays a strategic role on selection of the deformation mode and therefore on design of TWIP
composition.
A thermodynamical model for SFE calculation was developed mainly based on thermodynamic models
for the chemical driving force of the martensitic transformation. The SFE itself depends upon
two important metallurgical and thermodynamic parameters: the composition and the temperature.
Therefore, SFE can be modeled as a thermodynamic function, if each stacking fault is considered as a
double phase boundary between the -austenite (FCC) and the -martensite phase (HCP). SFE of in
the Fe-Mn base alloys has been calculated using the following equation proposed by Olsen and Cohen
[1]:



2 2 + = =

G SFE
fcc
(1)

is the planar packing density of a closed packed plane.

is the interfacial energy of a coherent boundary between the and phases. The established
values of

in transition metals are from 10 to 15 mJ /m
2
. In the present calculations, 15 mJ /m
2
was
used.
Based on the regular solution model, the free energy change for the phase transformation

G can be calculated as a function of temperature and composition, and then SFE can be estimated
based on the Olsen and Cohens model (Eq. 1).
Two ways were used to calculate

G .

Using the equations found in literature giving

Gi for each elements;
Using ThermoCalc to calculate the total free energy change for the phase transformation

G .

At moment of the present project start-up, two thermodynamical models for SFE calculations were
reported in literature: Grssel model [2] and Allain model [3]. In the table 1.1.2.1 are shown the
parameters for calculation of SFE for both models.
It can be noticed that using these equations somewhat different results for SFE would be obtained. It
can be seen that, while Allains equations give lower SFE for low C with low Mn, e.g. 0.1C with 15-
20Mn, Grssels equations seems to give more satisfying calculations of SFE at the interesting ranges



15

of C and Mn. Furthermore Allains model has no equations for including Al and Si, so that they cannot
be applied for Al or Si-bearing steels.
For this reason it was decided to adopt the Grssel model in order to define the steel chemical
composition to be investigated in the project.



Parameter Grssel et al. [2] Allain et al. [3]

Fe
G
2
00222 . 0 685 . 1 85 . 821 T T + +
-2243.38+4.309T

Mn
G
2
00455 . 0 7 . 2 0 . 3925 T T +
-1000.00+1.123T

C
G
12 . 24595 -22166

Al
G
5481.04-1.79912T

Si
G
T + 1800

FeMn

Mn
X 1 . 15282 5 . 9135 +
2180+532(X
Fe
-X
Mn
)

FeC

42500 42500

FeAl

3323

FeSi

1780
15 9
Table 1.1.2.1: Numerical values and functions used for the calculations of SFE in two models.



Definition of the steel chemical compositions to be cast
According with the Grssel equation, the calculated SFE values of reference steels (TWIP1) Fe-22Mn-
3Al-3Si and (TWIP2) Fe-22Mn-0.6C are respectively 26 and 42 mJ /m
2
.
On the basis of the Grssel model the effect of each element on SFE was evaluated and the three new
variants were selected as reported in the following table.


TWIP variant Steel composition Grssel et al
SFE (mJ m-2)
TWIP 1- ref. Fe-22Mn-3Al-3Si-0.01C

42
TWIP 2 ref. Fe-22Mn-0.6C-0.2Si

26
TWIP 3 Fe-18Mn-0.6C-0.2Si

23
TWIP 4 Fe-16Mn-1.5Al-0.2Si-0.3C

28
TWIP 5 Fe-21Mn-0.2Si-0.2C-0.2N

17
Table 1.1.2.2: Calculated SFE for TWIP steels at 298 K.


It is worthy to note that in Grssel model the nitrogen effect is not taken in consideration.




16

Task 1.2 Laboratory VIM ingot casting
Five heats were performed at CSM VIM facility with the following chemical compositions. The ingots
produced were about 80kg in weigth.


Table 1.2.1.1 Ingots chemical analysis.

The ingots were hot rolled and afterthat cold rolled in order to produce the strip samples needed for the
start up of the investigations.

Task 1.3 - Solidification structure characterisation

TWIP1 ingot sample
The ingot sample of TWIP1 shows a columnar macrostructure at the ingot surface, approx. 1.5 cm
thick, and a core region of equiaxed grains, fig. 1.3.1a). Its microstructure is a two-phase structure:
austenite matrix with an interdendritic ferrite phase that represents about 10% in volume, see fig.
1.3.1b) and fig.1.3.2.


a) b)
Fig. 1.3.1: Images of TWIP1 ingot. a) Macrostructure of the TWIP1 ingot sample, polished and Nital
2% etched b) SEM image of structure 2% Nital etch.


The sample is ferro-magnetic and this is in agreement with ferrite presence in the microstructure. The
solidification structure consists of austenite -fcc +ferrite -bcc (fig. 1.3.2).





17



a) b)
Fig. 1.3.2: a) Optical microstructures of TWIP1 in the cast state of lathy (black) and vermicular ferrite;
b) XRD of TWIP1 in the cast state showing the presence of duplex structure.

The ferrite phase appears both with lathy and vermicular morphology. XRD-analysis was performed to
confirm the presence of the austenite and ferrite phases and the diffractogram is shown in Fig. 1.3.2b).
Concentration profiles from the cast TWIP1 structure by SEM-EDS mapping indicate different contents
of the alloying elements of Mn and Al between the ferrite and austenite phases, as shown in fig. 1.3.3.
As seen in figs. 1.3.3.b-c, the ferrite phase is enriched in Al and depleted in Mn.


a) b) c)
Fig. 1.3.3: The element distribution (X-ray map) in the austenite and ferrite phases in cast TWIP1, (a)
SEM image, (b) Al distribution, and (c) Mn distribution.


Fig. 1.3.4: SEM-EDS analysis locations on the cast TWIP1.

The presence of ferrite should be related to the presence of both high Si content in connection with high
Al, which are strong ferrite formers. The C content in the steel is not enough to stabilize the austenite in
spite of the high Mn content. Figure 1.3.4 shows the dual-phase microstructure with five locations of



18

analysis. As shown, there is a significant difference in Al and Mn contents between the austenite and
ferrite phases. However, the difference in the Si content is low.
The partition ratio P
D
of Al, Mn and Si
,
defined as the ratio of the concentration of an element in ferrite
to that in the adjacent austenite, are given in table 1.3.1. The partition ratios of Al and Si are higher
than 1 and that of Mn is lower than 1. It is well known Al and Si are ferrite formers and Mn favours the
austenite in the Fe-Mn-Al system. The partition of Si is quite slight.

Element Al Mn Si

P
D
1.62 0.77 1.18
Table 1.3.1: Partition ratios P
D
of alloying elements between austenite and ferrite in TWIP1.


TWIP2
The microstructure of the cast TWIP2 (Fe-22Mn-0.6C) is fully austenitic with large elongated grains.
The microstructure displayed the dendritic structure, as shown in Fig. 1.3.5. The chemical etching
suggested clear composition variations in the structure which fact was confirmed by EPMA. A fine
criss-cross pattern of dendrites can be detected within each grain; dendrite cores being lower in Mn and
appear relatively bright. Between the dendrites (interdendritic regions) the Mn content is higher and
these regions are more heavily etched appearing darker in colour.


Fig.1.3.5: OM photo of the microstructure of the cast TWIP-2.

Electron probe microanalysis (EPMA; J eolJ XA 8200) with the pixel size of 0.2 m was applied to
investigate the microsegregation of the alloying elements. A Vickers hardness tester was used to mark
the start and end points of the line scan. Concentration profiles recorded from the dendritic cast
structure of TWIP2 show several maxima and minima. The minima of both Mn and C are located at the
dendrite cores. The segregation ratio (S), i.e. the ratio of an element concentration in the interdendritic
regions to that at the dendrite cores, was estimated after the quantitative calibration of EPMA. It was
found that S
Mn
and S
C
are 1.6 and 1.5 respectively.


TWIP3
The microstructure of TWIP3 (Fe-18Mn-0.6C-0.019Nb) steel, shown in fig. 1.3.6, revealed a austenitic
solidification with dendritic morphology.



19


Fig. 1.3.6: OM photo of the microstructure of the TWIP3 in the cast state.


The microsegregation of the steel was examined using the EPMA similarly as for TWIP2. C and Mn
have simultaneous segregation, peaks locating at the interdendritic regions, similarly as in the case of
TWIP2. The segregation ratio S
Mn
is equal to 1.5. The Nb content is so low that it could not be
recorded.
With careful focusing, the microstructure of TWIP3 revealed the presence of martensite phase with
the lath morphology, as shown in Fig. 1.3.7. Martensite plates extend across the whole austenite grains,
i.e. crossing several dendrites. It can been suggested that the low stacking fault energy of this steel
favours the formation of -martensite in the cast ingot, similarly as in TWIP 1.


Fig. 1.3.7: Presence of -martensite in the cast TWIP3.

The presence of martensite in TWIP3, as seen in Fig. 1.3.7, may be attributed to the segregation of
Mn. Martensite plates are always located in dendrite cores, where Mn has its minimum concentration.


TWIP4
The microstructure of the cast TWIP4 (Fe-16Mn-1.5Al-0.3C) displayed dendritic structure, as shown in
Fig. 1.3.8. The maximum distance between two dendrite cores is about 900 m. However, at high
magnifications, the presence of fine plate phase, i.e. -martensite, in the dendritic regions can be seen.
However, this phase is present in the dendritic core regions, as shown in Fig. 1.3.8.





20



Fig. 1.3.8: OM photo of TWIP-4 in the cast state. Fine plates of -martensite in dendrite cores (right).


It can be concluded that segregation of alloying elements plays a strong role on the generation of
preferential nucleation sites for the -martensite. From the elemental analysis, it is known that in the
dendrite core regions have lower Mn and C contents, i.e. the SFE is locally lower there. According to
Olson and Cohens thermodynamic model, the lower Mn content would decrease SFE in the dendrite
core regions to 24 mJ /m
2
, while the higher Mn content in the interdendritic regions would mean a SFE
of 45 mJ /m
2
. This explains the observation the -martensite can exist in the dendrite core.


TWIP-5
The cast microstructure of TWIP5 (Fe-22Mn-0.2C-0.2N) displays a dendritic segregation, as seen in
Fig. 1.3.9. At high magnifications, the fine plate-like phase of -martensite is present in the dendrite
cores and arms, but such a phase is not found in the interdendritic regions, as seen in Fig. 1.3.9(b). This
situation is exactly similar to that for TWIP4. However, the -martensite fraction in TWIP5 is much
higher.


a) b)
Fig. 1.3.9: OM photos of the microstructure of the cast TWIP5.




21

EPMA analysis was conducted to record the micro-segregation using a line crossing two dendrite cores,
with the length of 250 um.
The C and Mn concentration profiles begin at the peak followed by a minimum, thereafter there is
second maximum that corresponds to the interdendritic region (etched dark in the figure). However, no
variation of N can be revealed. The segregation ratio of Mn is equal to 1.5, similarly as for TWIP2 and
TWIP4.
To study further the short-range segregation, a distance between two secondary dendrite arms was
analysed using EPMA. As observed, the maxima of Mn and C correspond to the interdendritic region
between the two secondary arms. As the dendrite grows into the melt, and as secondary arms spread
from the main dendrite stem, while the solute Mn is rejected. In the N distribution, no segregation could
be detected.

Determination of the liquidus and solidus temperature of the TWIP steel variants
The evaluation of liquidus and solidus temperature are of paramount importance in order to define the
operating practice steelmaking and continuous casting process. On the basis of these critical
temperatures is calculated the liquid steel overheating (in tundish and mould). At the same way the
knowledge of solidification range is also important to define the optimal continuous casting process.
Differential thermal analysis (DTA) was carried out in order to evaluate the liquidus and solidus
temperature of TWIP2 steel. For other TWIP variants the critical temperature were qualitatively
evaluated by Thermocalc model. The results of measures and calculations are summarized in the table
1.3.2. Comparing the measured and calculated critical temperatures the following considerations can be
argued for TWIP 2 steel:
The measured liquidus temperature is quite close to calculated value (the difference is only
0.4%);
The calculated solidus temperature is underestimated of 30C (about 2%).


Steel grade T
solidus
(C) T
liquidus
(C)
TWIP 2 1322 (DTA measure) 1406 (DTA measure)
TWIP2 1292(calculated) 1400 (calculated)
TWIP 3 1312(calculated) 1420 (calculated)
TWIP4 1314(calculated) 1418(calculated)
C, Mn steel 1495(calculated) 1525 (calculated)
Table 1.3.2: T
solidus
and T
liquidus
of TWIP steel variants.



Conclusion of Task 1
Five TWIP steel variants were selected on the basis of stable austenitic phase and low SFE. The
variants were of two main types Fe-Mn-C-N and Fe-Mn-Al-Si-C.


Table 1.3.3 Ingots chemical analysis.




22

Of these five TWIP variants the first variant revealed a mixed primary solidification structure with
austenite +ferrite. The ferrite phase is stable also at RT.
The remaining 4 TWIP variants revealed a fully austenitic solidification. The austenitic phase is stable
down to RT. Microsegregation associated to dendritic solidification determine zone with lower local
SFE (low Mn and C). In these zones the presence of -martensite was detected.

















































23

WP2: Fundamental investigations on the physical metallurgy of TWIP steels

Task 2.1 Measure of SFE by means of Transmission Electron Microscopy observations of
extended nodes. Evaluation of Ms
>
temperature.

Task 2.1.1: Measure of SFE by means of TEM observation of extended nodes

Background
Mechanical twinning and -martensite formation are competitive deformation mechanisms that are very
similar from the morphology and origin point of view. Whelan first [1] and Brown later in 1964 [2]
showed that the dissociation of dislocation a/2 <110>into partials of burger vector a/6<112>lying on
{111} planes creates stacking fault on successive parallel {111} planes. The crystallographic structure
in the faulted region is still FCC but in a twin orientation compared to the matrix. Epsilon martensite
formation occurs when the same dislocations glide on every second {111} plane. In this case the
deformed region takes the form of a thin lamella or platelets with a close packed hexagonal structure.
Both mechanisms are strongly related to the SFE, which controls the energetic cost for creating such
defects.
The methodology adopted for the SFE measure is based on the work of Remy [3] and A. W. Ruff and
L.K. Ives [4] and consists in the measure of SFE by means of TEM measurement of extended nodes
size produced by interaction of extended dislocations.

Sample preparation methodology
The SFE measurement was carried out on a TWIP2 steel specimen. The selected strip sample was a
cold rolled strip annealed, in N
2
atmosphere, at 1000C for 5 min. (Fig. 2.1.1.1).


Fig 2.1.1.1: TWIP2 microstructure after annealing treatments at 1000Cx5 min (average grain size 32
m).
The samples were polished first mechanically up to a thickness of 200 m, then further thinning was
carried out electrolytically down to 80-100 m. After this step the specimen was deformed by means of
a double bending (to produce few dislocations). The final step consisted in the jet spray electrolytic
thinning to achieve the thin foil specimen suitable for TEM observation.

Results
Different thin foils were produced and observed by means of a STEM (J EOL -100KV). As a whole 10
nodes were selected during TEM examination and were judged suitable for SFE measurement. In fig



24

2.1.1.2 are shown some images of the extended nodes selected. In tab. 2.1.1.1 are reported the values of
the SFE obtained taking into consideration only the suitable extended nodes.





Node W (m)

mJ/m
2
A1 2.5E-08 19.8
A 2.0E-08 24.6
B 2.0E-08 24.6
C 2.7E-08 18.5
D 3.1E-08 15.8
E 2.4E-08 20.7
F 1.7E-08 28.7
H 2.8E-08 17.7
I 1.9E-08 25.7
L 2.7E-08 18.1
average 21.4
dev. Std. 4.2
std error 0.4
Fig. 2.1.1.2: Extended nodes detected on a TWIP2 sample. Table 2.1.1.1: SFE results achieved on
TWIP2.



The average value of SFE for TWIP 2 resulted in 21.4 mJ /m
2
. The standard deviation of SFE values is
consistent with other measurements reported in literature.

Comparison of TEM result with empirical models
The stacking fault energy (SFE) of high Mn TWIP steels was evaluated using thermodynamic models
due to Grssel and Allain. In addition ThermoCalc code was used to assess the SFE.
The analysis revealed that ThermoCalc and the model due to Grssel gave good agreement, whilst that
due to Allain et al. gave significant differences also because this model did not consider the influence of
Al and Si on stacking fault energy. However, recently the model of Allain et al has been extended to
consider Al and Si by the work of Dumay et al [5]. Thus, to assess the SFE of TWIP grades 1 to 5 the
new model will be used and compared to the results of the model due to Grssel. The new model due to
Dumay et al is reported in the table below.




25


Table 2.1.1.2: Model parameters for calculation of SFE in Dumay et al model [5].




Steel composition Dumay et al
SFE (mJ m-2)
Grassel et al
SFE (mJ m-2)
Fe-21.3Mn-3Al-3Si-0.01C
(TWIP 1)
11 42
Fe-22.3Mn-0.59C-0.22Si
(TWIP 2)
22 26
Fe-17.8Mn-0.6C-0.2Si-0.02Nb
(TWIP 3)
17 23
Fe-16.4Mn-1.54Al-0.21Si-0.29C
(TWIP 4)
10 28
Fe-21Mn-0.23C-0.2Si-0.2N
(TWIP 5)
7 17
Table 2.1.1.3: Calculated SFE for TWIP steels at 298 K.


Table 2.1.1.3 shows the calculated SFE from the Dumay model and that due to Grassel for TWIP
grades 1 to 5. Comparing the results in table 2.1.1.3 arises that the model of Dumay gives the best
correlation with the measured SFE for TWIP2.

Conclusions of task 2.1.1
The SFE of TWIP2 steel was measured by means of TEM adopting the extended nodes method. The
average SFE value for TWIP2 steel resulted of 21.4 mJ /m
2
. The standard deviation of SFE values is
consistent with other measurements reported in literature.
The comparison with thermodynamical model reveals that the Dumay model gives the best correlation
with the measured SFE for TWIP2. The model of Dumay predicts that the variants TWIP 1, 3, 4 and 5
should have SFE values below 18 mJ m
-2
. However the contribution of N and Nb is not taken into
account.




26

Task 2.1.2 Evaluation of the Md of TWIP steel variants
In low SFE austenitic steels the temperature Ms

indicates the temperature at which the austenite


phase is thermodinamically instable and hcp-martensite start to form. This temperature is of particular
importance because it is strictly related to SFE value and gives an indication of the stability of the
austenitic phase during deformation against the formation of hcp-martensite. The volume fraction
formed of hcp-martensite depends on the strain and on temperature through the SFE.
Generally for austenitic steels is more significant and easier to evaluate the temperature at which the
strain induced hcp-martensite achieves a threshold value. For austenitic stainless steel the martensite
transformation temperature M
d
30 is defined as the temperature at which 50% of martensite (+) is
formed after a straining of 0.3 true strain.
In order to define also for TWIP steel a similar parameter related to deformation induced martensite the
following activities were carried out :

Two series of TWIP samples were deformed at true strain 0.1 and 0.3 at temperatures in the
range 20C -180C using liquid nitrogen to cool down and control the sample temperature;
The presence of -martensite and -martensite as a function of the temperature was evaluated
metallographically by means of special color etching and measuring the magnetic behavior
(ferritoscope).
XRD pattern on deformed samples were also carried out but the low fractions of phases to be measured
and also the small difference between the different samples suggested to evaluate metallographically the
fraction of -martensite and -martensite as a function of the temperature by means of special color
etching and measuring the magnetic behavior by ferritoscope. On the basis of the results achieved and
reported in fig. 2.1.2.1 the martensite transformation temperature M
d

for TWIP steels was defined in


these terms:
M
d30

=the temperature at which the fraction of hcp-martensite achieve a fraction of 2% after a
deformation of 0.30.
Adopting this definition the value for the M
d30

of TWIP2, TWIP3 and TWIP5 was evaluated and
reported in the following table 2.1.2.1.


Fig. 2.1.2.1: Hcp-martensite fraction on sample deformed at 0.30 at low temperature.





27

TWIP variant M
d30

(C)
TWIP2 -170
TWIP3 -145
TWIP5 -72
Table 2.1.2.1: M
d30

evaluation from fig.2.1.2.1.




Conclusions of task 2.1.2
The temperature for deformation induced transformation M
d30

was evaluated for TWIP2, TWIP3


and TWIP5 and the values are respectively -170C, -145C and -72C. These results confirm, again,
that TWIP 2 and TWIP3 are the steel grades revealing the best microstructural stability and TWIP
effect during deformation even at quite low temperature.

Task 2.2: Characterization of recrystallization behaviour

Task 2.2.1 Critical strain for DRX initiation, flow stress, peak stress, maximum softening rate by
using a thermo-mechanical simulator (Gleeble) and Hot torsion tests at different temperature
(900-1100C) and strain rates.
To study the hot deformation characteristics of the steels, the flow resistance and softening behaviour,
the specimens were compression tested using a Gleeble 1500 thermo-mechanical simulator. In hot
compression tests, specimens were reheated at 1200 C for 2 min and then cooled to the test
temperature (between 900 C and 1100 C) at the cooling rate of 5 C/s. After 15 s of soaking at the test
temperature, the specimens were compressed in a single hit to the true strain of 0.8 at the constant true
strain rate 0.1 s
-1
.
The static recrystallization (SRX) kinetics of the steels was studied by employing the double-hit
compression test technique at temperatures between 900 C and 1100 C and at the constant strain rate
of 0.1 s
-1
. The applied strain was 0.2 and the holding times between the passes were 1 to 1000 s. The
typical test schedule is shown in Fig. 2.2.1.1. The 5% total strain reloading method was adopted in
determining the recrystallized fraction in order to exclude the effect of recovery from the softening data
[1,2]. As conventionally, the softening fraction, X, is calculated from the equation:
( )
( )
1 3
2 3

= X (1)

where
1
and
2
are the offset stresses due to the first and second hit, respectively, and
3
is the flow
stress of the work-hardened material.





28



Fig. 2.2.1.1: Schedule used in double-hit compression tests.


Hot deformation behavior: TWIP-2 (Fe-22Mn-0.6C)
The microstructure of TWIP2 (22Mn-0.6C), characterized using the SEM-EBSD technique, as heat-
treated at 1200C for 2 min on the Gleeble simulator and cooled very fast by water spray to room
temperature, is shown in fig. 2.2.1.2. The microstructure exhibits coarse austenite grains with the size
about 97 m.


Fig. 2.2.1.2: SEM-EBSD photo of TWIP-2 steel as heated at 1200C for 2 min and water quenched.
Red lines reveal high-angle (>15) grain boundaries.


Flow stress curves at high temperatures
Typical true stress-true strain curves of TWIP2, as compressed at 1100, 1000 and 900 C at the strain
rate of 0.1 s
-1
, are shown in fig. 2.2.1.3. For comparison, the flow strain curves of a low-carbon steel
(0.10C-0.45Mn) are displayed in the same figure.
It can be seen that the flow curves are featured by rapid work hardening at the initial strains and a broad
stress peak at all test temperatures revealing the occurrence of dynamic recrystallization (DRX). The
peak stress (
p
) and peak strain (
p
) depend on the temperature. For example, at 1100C, the peak stress
(112 MPa) is attained at the strain 0.26 and at 1000C, the peak (
p
=157 MPa) is at 0.38. The high-
Mn TWIP steels have much higher hot deformation resistance than that of low-C steel, as reported
previously [3], and also displayed in fig. 2.2.1.3 at all testing temperatures.



29


Fig. 2.2.1.3: Typical true stress-strain curves of TWIP-2 (Fe-22Mn-0.6C) steel at high temperatures and
constant strain rate of 0.1 s
-1
. Curves for the low-carbon steel are included for comparison.



The peak stresses and peak strains for the both steels are plotted as a function of the inverse temperature
in fig. 2.2.1.4. It is seen that the peak strain is higher for the high-Mn steel compared to that of the low-
C steel. Also the peak strain is lower for the low-C steel. For example, at 1100C, the peak strains are
0.16 and 0.26 for the low-C steel and TWIP-2, respectively, indicating a significant delaying effect of
high Mn content on DRX.
The peak strain
p
is an important variable. The critical strain (
c
)

at which dynamic recrystallization
starts can be approximately determined from
p
, for
P c
8 . 0

(1). The dependence of (
p
)

on the
Zener-Holloman parameter (Z) and initial grain size (d
0
)

has been found as the following:

p
=A
n
d
0
Z
m
(2)

p
=A
1
Z
m
(3)
Z = exp(Q
def
/RT) (4)


where the parameters A, n, m and A
1
depend on the alloy composition. Where is the strain rate, Q
def
is
the activation energy of hot deformation, R the gas constant and T the absolute temperature. In the
present work, the peak strain (
p
) was determined for all the flow curves where the peak stress (
p
) was
clearly discernable. The results were then fitted with Eq. (3), and shown Fig. 2.2.1.5. The activation
energy of deformation Q
def
for low-C and high-Mn TWIP steels have been determined in other works
[3-5] to be 315 kJ /mol and about 380 kJ /mol for low-C and 25Mn-Al type steels, respectively. It is seen
the slopes vary to some extent, so that the Zener-Hollomon exponents (m) values are 0.197 and 0.135
for low-C and 22Mn-0.6C steels, respectively. These values are in good agreement with the values
reported for C-steels in the range 0.12-0.22 [6]. Elwahabi et al. [7] measured the Zener-Hollomon
exponents for Type 304 austenitic stainless steel to be in the range 0.125-0.156.




30



Fig. 2.2.1.4: Dependence of peak stress (
p
) and peak
strain (
p
) on the inverse temperature at the strain rate
of 0.1 s
-1
for TWIP-2 and low-C steels.
Fig. 2.2.1.5: Plot of ln(
p
) vs ln Z for the low-C and
TWIP-2 (22Mn-0.6C) steels.




Recrystallization kinetics of TWIP2
A selection of interrupted double-hit compression stress-strain curves determined at 1000C, at the
constant true strain rate of 0.1 s
-1
, an applied strain 0.2 and interpass times of 3 to 50 s.
During the unloading time, static softening occurs by the static recovery at short times and mainly by
static recrystallization (SRX) at longer times.
The fractional SRX curves at three temperatures (900-1100C) as a function of holding time after
compression to the 0.2 strain at the strain rate of 0.1 s
-1
are plotted in fig. 2.2.1.6.




Fig. 2.2.1.6: SRX rates of TWIP-2 at constant strain rate of 0.1 s
-1
. Double-hit compression data and
fitted curves. Times for 50% recrystallization, t
50
, and the Avrami exponents are listed.


As seen in fig. 2.2.1.6, the data can be fitted well with the sigmoidal curves, corresponding to the
Avrami-type relationship [8], as follows:

( ) [ ]
n
t t X
50
693 . 0 exp 1 = (5)




31

where X is the recrystallized fraction, t time,
50
t time for the 50% recrystallization and n is the Avrami
exponent. It was found that the values for n of the TWIP-2 are quite low ( 0.8-1.2) compared with the
values 1.5-2 typical of the carbon steels [2].


TWIP-3 (Fe-18Mn-0.6C-0.02Nb)
Initial microstructure
The microstructure of TWIP3 sample, after soaking at 1200C for 2 min on the Gleeble simulator and
cooled very fast by water quenching to room temperature, was characterized using the SEM-EBSD
technique. The microstructure exhibits coarse austenite grains of the size of about 80 m.

Flow stress curves at high temperatures
Typical true stress-true strain curves of the present steel as compressed at 1100, 1000 and 900 C at the
strain rate of 0.1 s
-1
are shown in fig. 2.2.1.7. For comparison, the flow stress curve of Fe-26Mn-0.14C
at 1000C/0.1 s
-1
, tested in another study [9], is displayed in the same figure.
It is seen that TWIP3 steel exhibits hot deformation behaviour similar to that of TWIP2. For example, at
1100C, the flow stress curve has a peak at 0.26, which peak strain is identical for that of TWIP2. Also,
at 1000C, both steels exhibited the peak at the same strain of 0.36.
Comparison with the Fe-26Mn-0.14C steel shows that the both steels have the same behaviour and flow
resistance up to the peak strain of TWIP3 (
P
=0.36), but then the steel with the higher Mn level
delaying DRX so that the peak stress is at 0.46. Hence, as observed earlier by comparing 22Mn-0.6C
steel with the low-C steel (with 0.45Mn), it is seen that a higher Mn content in steels retards DRX
(assuming that C content has no influence). Comparing TWIP steels having equal peak strains, it can be
concluded that Nb of 0.022% retards DRX to the same amount than the difference in the Mn contents of
the steels (22 and 18%) enhances.



Fig. 2.2.1.7. Typical true stress-strain curves of TWIP-3 (Fe-18Mn-0.6C-0.02Nb) steel at high
temperatures and the constant strain rate of 0.1 s
-1
. A curve for Fe-26Mn-0.14C steel is included for
comparison.






32


Recrystallization kinetics of TWIP3
The softening kinetics of TWIP3 was investigated at three temperatures 900C, 1000C and 1100C
after compression to the 0.2 strain at a constant strain rate 0.1 s
-1
. The fractional SRX curves as a
function of holding time are plotted in fig. 2.2.1.8. For comparison, the softening of Fe-26Mn-0.14C
steel, investigated elsewhere [10], are included in the figure. Also the data are being fitted well with the
sigmoidal curves, corresponding to the Avrami-type relationship [8].



Fig. 2.2.1.8: SRX of TWIP-3 (0.2 strain at
constant strain rate 0.1 s
-1
). Double compression
data and fitted curves.
Fig. 2.2.1.9: SRX of TWIP-3 determined in a
relaxation test at 1000C/0.2/0.1 s
-1
.



It can be observed that the SRX kinetics of TWIP3 is high at 1000C and 1100C with Avrami
exponent n =1.1 and 1.2 and t
50
11 s and 4 s, respectively. However, at 900C SRX is very slow. SRX
kinetics of Fe-26Mn-0.14C is slightly slower than that of TWIP3. This can be attributed to the higher
Mn content of TWIP3, Mn retarding SRX [3,9].
Another hot deformation testing method, stress relaxation, was also employed to measure the SRX
kinetics of TWIP3. In the stress relaxation test, the displacement of the anvils is held constant after
deformation and the drop in the stress recorded as a function of time.
The SRX fraction from a stress relaxation test at 1000C is shown in fig. 2.2.1.9 with the Avrami-type
fitting. A good agreement between the double-hit compression data and the data from the stress
relaxation test are observed. Both methods displayed the same SRX kinetics with the Avrami exponent
of 1.2 and t
50
=11 s.


TWIP4 (Fe-16Mn-1.5Al-0.3C)
Flow stress curves
The flow stress curves of TWIP4 (Fe-16Mn-1.5Al-0.3C) at three temperatures and at the constant strain
rates of 0.1 s
-1
are shown in fig. 2.2.1.10.



33


Fig. 2.2.1.10: Typical true stress-strain curves of TWIP4 (Fe-16Mn-1.5Al-0.3C) at the constant strain
rate of 0.1 s
-1
. Flow stress curves for 25Mn1Al [9] steel are included for comparison.


It can be seen that the flow stress curves of TWIP4 display distinct peaks at 1100C and 1000C, but it
is difficult to discern any peak at 900C. The peak strains are quite equal.
For comparison, the flow stress curves for the 25Mn1Al steel are included in the same figure [9]. The
hot deformation resistance of TWIP4 is lower than that of the 25Mn1Al steel. This can be attributed to
the lower Mn content in TWIP4. From literature the strengthening effect of Mn is about 2 MPa/wt%
and that of Al about 12 MPa/wt%. Hence, the lower Mn content of 9% in TWIP4 would mean the stress
of 18 MPa lower and 0.5% higher Al, in turn, about 6 MPa higher stress level. As a result, the flow
stress could be 12 MPa lower for TWIP4 compared to that of 25Mn1Al. In fig. 2.2.1.10, the difference
seems to be about 20 MPa, i.e. somewhat more than predicted.


Recrystallization kinetics of TWIP4
The softening kinetics of TWIP4 was investigated at three temperatures 900C, 1000C and 1100C
after compression to the 0.2 strain at the constant strain rate of 0.1 s
-1
. The fractional SRX curves as a
function of holding time are plotted in fig. 2.2.1.11. Also, the data was fitted well with the sigmoidal
curves, corresponding to the Avrami-type relationship [8].
It can be observed that SRX of TWIP4 is fast at 1000C and 1100C with t
50
=8 s and 3 s, respectively.
However, at 900C SRX kinetics is slower with t
50
=55 s. 25Mn1Al has identical recrystallization
kinetics, with t
50
=8 s at 1000C and the Avrami exponent of 1.




34


Fig. 2.2.1.11: SRX rates of TWIP-4 at the constant strain rate of 0.1 s
-1
. Double-hit compression data
and fitted curves. Data for 25Mn1Al at 1000C from [9].


TWIP-5 (Fe-22Mn-0.2C-0.2N)
Fig.2.2.1.12 shows the flow stress curves of TWIP-5 at high temperatures (900-1100C) at the constant
strain rate of 0.1 s
-1
, compared with the flow stress of TWIP-2 (Fe-22Mn-0.6C). Both steels show the
same hot deformation behaviour, displaying the peak at the identical strains 0.27 and 0.35 at 1100C
and 1000C, respectively. However, TWIP-5 has lower deformation resistance (about 10 MPa) at
highest temperatures, but at 900C, TWIP-5 shows a higher flow stress.



Fig. 2.2.1.12: True stress-strain curves of TWIP-5 (Fe-22Mn-0.2C-0.2N) steel at high temperatures and
at the constant strain rate of 0.1 s
-1
. Curve for TWIP-2 (Fe-22Mn-0.6C) is included for comparison.


The results from the double-hit compression tests for TWIP-5 in fig. 2.2.1.13 show that TWIP-5 has the
slowest recrystallization kinetics among the tested TWIP steels, because t
50
at 1100C (7 s) 1000C (22



35

s) and 900C (110 s) are about two times longer than those of the other steels (about 3-4, 8-11 and 55-
75 s, respectively). Hence, N alloying seems to retard the softening kinetics. Also the Avrami exponents
are smaller than typical of the other steels.




Fig. 2.2.1.13: SRX of TWIP5 at the constant strain rate of 0.1 s
-1
. Double-hit compression data and
fitted curves.



Effect of C on high temperature deformation behavior
Typical true stress-true strain curves of TWIP steel, as compressed at 1100, 1000 and 900 C at the
strain rate of 0.1 s
-1
have been presented above. The flow stress curves of TWIP steels with different
alloying contents and a low-carbon steel (0.10C-0.45Mn) have been compared.
Complexively the steels considered are:

TWIP steels of Metaldesign project
Fe-22Mn-0.6C
Fe-18Mn-0.6C-0.02Nb
Fe-16Mn-1.5Al-0.3C
Fe-22Mn-0.2C-0.2N

TWIP steels from literature
Fe-25Mn-0.16C-1Al
Fe-26Mn-0.14C

Low C steel from literature
(0.10C-0.45Mn)

As can be realized, the C content ranges between 0.10% up to 0.6% and the Mn content range is
between 0.45% and 26%.




36

Qualitatively the value of peak stress at different temperatures can be considered as an indicator of the
hot deformation resistance behavior of the steel considered. In the following table, only for example,
the peak stress at 1000C of TWIP steels are listed together with the other literature data. On the basis
of these scarce data, a multiple correlation analysis between alloying contents (C, Mn, Al and N) and
peak stress at different temperatures (at 900, 1000 and 1100C) was carried out. Some conclusions can
be drawn and summarized in these terms:

The high-Mn TWIP steels have a much higher hot deformation resistance than that of low-C
steel. This difference seems to be mainly related to the higher Mn content in TWIP steels.
Considering only TWIP steels, the effect of alloying element contents (C, Mn, Al and N) on the
peak stress is not so distinct and this is confirmed by quite poor correlation factors found
(<0.7).


Steel Peak stress (MPa) at 1000C
Fe-22Mn-0.6C

148
Fe-18Mn-0.6C-0.02Nb

145
Fe-16Mn-1.5Al-0.3C

148
Fe-22Mn-0.2C-0.2N

140
Fe-25Mn-0.16C-1Al

162
Fe-26Mn-0.14C

148
C-Mn steel (0.10C-0.45Mn)

90
Table 2.2.1.1: Peak stress at 1000C of different TWIP steels.



Effect of C on recrystallization behaviour
On the basis of the results of double-hit compression tests carried out on the TWIP steel variants, a
qualitative study of the effect of alloying elements (C, Mn) was evaluated by means of multiple
correlation analysis between C and Mn content with t
50
values (time for 50% of recrystallization) at
different temperatures. In the following table, for example, the values of t
50
at 1000C and 1100C
relevant to TWIP steels variants are reported.

Steel t
50
at 1000C (s) t
50
at 1100C (s)
Fe-22Mn-0.6C

10 4
Fe-18Mn-0.6C-0.02Nb

11 4
Fe-16Mn-1.5Al-0.3C

8 3
Fe-22Mn-0.2C-0.2N

22 7
Table 2.2.1.2: Values of t
50
at 1000C and 1100C relevant to TWIP steels variants.
Some conclusions can be inferred and summarized in these terms:



37

No clear trend arises from the analysis of the effect of C content on rex kinetics. This is
confirmed by quite a poor correlation coefficient. This is consistent with C-steels, where,
according to literature, C has no influence on static recrystallization kinetics.
TWIP-5 revealed the slowest recrystallization kinetics among the tested TWIP steels. N
alloying seems to retard the softening kinetics.


Static recrystallization kinetics
The results shown above indicated that all the investigated high-Mn TWIP steels have almost equal
recrystallization kinetics that is identical to that of 25Mn1Al. Only the TWIP5 has a distinctly slower
softening behaviour. The steel 25Mn1Al has been used to investigate more extensively the power of
various variables on the SRX kinetics by applying double-hit compression technique. These results
have been published in [9] but briefly described here to complete the characterization of SRX behaviour
of high-Mn TWIP steels.


Temperature and alloying
SRX fractional softening curves after the deformation to the 0.2 strain (i.e. smaller than the peak strain)
at 0.1 s
-1
at five temperatures are plotted in fig. 2.2.1.14. As shown, sigmoidal Avrami-type curves can
be fitted with the experimental data. It is well established that the time for the 50% recrystallized
fraction t
50
can be described by the following empirical relation [16]:

t
50
=A
p

q
d
s
exp(Q
app
/RT) (6)

where A is a constant, the strain,

strain rate, d the grain size, Q


app
the apparent activation energy of
recrystallisation, R the universal gas constant and T the absolute temperature. Material constants p, q
and s are the strain, strain rate and grain size exponents, respectively.


Fig. 2.2.1.14: SRX rates (strain 0.2, strain rate 0.1 s
-1
) for the 25Mn1Al steel. Double-hit compression
data and fitted curves.




38

The recrystallization kinetics of low-C (0.09C-0.45Mn) and Nb-microalloyed (C-Mn-0.03Nb) steels as
well as one austenitic stainless steel (Type 304) has been investigated previously, e.g. [11,12,17]. Some
new tests were performed for low-C and austenitic stainless steels, and these data at 1050C are plotted
in fig. 2.2.1.15 for comparison. For the Nb-steel, SRX data obtained by the double-hit and stress
relaxation methods at 1050C/0.1s
-1
was taken from a paper of Perttula and Karjalainen [2], suggesting
the t
50
time of 7 s. However, the grain size of this steel was 60 m. The grain size difference can be
accounted by using the power of grain size s =2.13*d
-0.105
[18,19]. The predicted data and the curve are
plotted in fig. 2.2.1.15. It is seen that the 25Mn1Al steel exhibits faster SRX kinetics than the austenitic
stainless or Nb-bearing steels but slower than that of low-C steel.
The t
50
times are 1, 4, 16 and 15 seconds for low-C, 25Mn1Al, Nb and Type 304 steels, respectively.
For high Mn-Al steels, the Avrami exponent seems to decrease with decreasing temperature. For the
Avrami curves the exponents are 1.2, 1.1, 0.8, 0.7 and 0.7 at 1100, 1050, 1000, 950 and 900C,
respectively. These values are quite low compared with the commonly reported values for C-Mn steels
(between 1-2) [13]. It is known that recovery tends to decrease the value. Hence, it can be concluded
that there might still be some contribution of recovery, even though the 5% total strain method was
adopted. It was realized that in high-Mn steels, dynamic recovery is very intense; particularly in steels
with high Al levels that have higher stacking fault energy [5].


Fig. 2.2.1.15: Comparison of SRX kinetics of 25Mn1Al to low-carbon, Nb and Type 304 steels. Data
for the Nb-steel from [2].


Effect of strain and strain rate on SRX
The effects of strain and strain rate on t
50
times for the 25Mn1Al steel are shown in figs. 2.2.16 and
2.2.17. From the slopes of the lines, values of -2.7 and -0.3 are obtained for the strain and strain rate
exponents, respectively. The strain exponent for C-Mn steels has been reported to be in the range -2.5
to -4 at the strain range of 0.1-0.2 [18,20-22]. Values between -2 and -3 have been measured by the
stress relaxation technique for some microalloyed steels [23]. Somani et al. [18,19] used values of -2.8
for C/C-Mn/Nb/Ti/Nb-Ti steels and -2.5 for Mn-V/other steels in developing a regression model based
on chemical composition for predicting SRX kinetics of a large variety of steels. Koskiniemi et al. [12]
determined values of -3 and -1.5 for Type 304 and a 12Cr stainless steels, respectively. Barraclough and
Sellars [24] found a strain exponent of -4 at small strains, but the value decreased as the strain



39

approached the critical strain for the onset of DRX. Most of these strain exponent values are of the same
order, and hence, a strain exponent of -2.7 can be considered reasonable for the 25Mn1Al steel as well
as for other TWIP steels, owing to the low effect of Al on the SRX characteristics and kinetics.
As compared to strain, the effect of strain rate is relatively small at small strains, and the computed
exponent from the experimental data for 25Mn1Al and some limited data for the 25Mn, 25Mn3Al and
25Mn6Al steels is about -0.3. In comparison, Koskiniemi et al. [12] obtained the strain rate exponents
for Type 304 and 12Cr stainless steels as -0.30 and -0.33, respectively. Strain rate exponents equal to -
0.38 are commonly reported for Type 304 and Type 316 steels in the literature, too (e.g. [25-27]). All
these values are relatively high compared to the values obtained for C and C-Mn steels (-0.11), medium
carbon steels (-0.13) and also Ti-steels (-0.12) [28]. In between the two, the strain rate exponents for Nb
and Nb-Ti and Mo-steels are measured to be about -0.23 [13,19], which value has also been used in the
development of regression models for kinetics and activation energy of SRX, essentially based on
chemical composition [18,19]. All these values indicate the dependence of strain rate effect on the
extent and type of alloying. Thus, the exponent of -0.3, experimentally measured for the 25Mn1Al steel,
can be considered reasonable for the all TWIP steels, being closely equal to that of Type 304 stainless
steel, as mentioned earlier [12].



Fig. 2.2.1.16: Plot of t
50
vs strain to calculate Fig. 2.2.1.17: Plot of t
50
vs strain to calculate the
power of strain for 25Mn1Al. the power
of strain rate.



Activation energy of SRX
The temperature dependence of SRX kinetics for the 25Mn1Al steel is shown in fig. 2.2.18, where t
50

times are plotted against the inverse absolute temperature. The apparent activation energy of SRX
(excluding data above 1075C) deduced from the data is about 257 kJ /mol, which is lower than that
reported for Type 304 (285 kJ /mol) and close to that of the 12Cr stainless steel (265 kJ /mol) [12].




40


Fig. 2.2.1.18: Time t
50
of SRX for 25Mn1Al vs the inverse absolute temperature.


The activation energy of hot deformation Q
def
for the 25Mn and 25Mn3Al steels has earlier been
determined to be 380-405 kJ /mol [3], so that Q
def
of 385 kJ /mol can be assumed for 25Mn1Al. Then,
Q
rex
for this steel can be computed to be about 373 kJ /mol. In comparison, Koskiniemi et al. [12]
reported equal Q
rex
values of 400 kJ /mol for both Type 304 and 12Cr stainless steels. In the literature,
largely varying values for Q
rex
have been reported for Type 304 steel, e.g. in the lists of Barbosa [29]
(360-460 kJ /mol) and Ryan and McQueen [27,30] (334-550 kJ /mol). Anyhow, all these values are of
the same order, so that Q
rex
of 373 kJ /mol computed for the 25Mn1Al steel can be considered to be
reasonable also for the other TWIP steels, even though a small effect of Al on Q
def
cannot be ignored.
This level of Q
rex
is comparable to those obtained for Ti-steels (255-275 kJ /mol) and Nb-steels (345-400
kJ /mol) [18,19] but it is substantially higher than the ordinary C/C-Mn and medium-C steels (200-240
kJ /mol).
With the powers of strain (-2.7) and strain rate (-0.3) and the apparent activation energy of SRX (257
kJ /mol), the following fractional softening equation for SRX has been determined:

t
50
=3.2*10
-15

-2.7
'
-0.3
d
s
exp(257000/RT) (7)

where the power of grain size, taken from [18,19], is assumed to be

s =2.13 d
-0.105
(8)


Grain size evolution in SRX
Several equations given in the literature for predicting the statically recrystallized grain size in carbon
and austenitic steels were tried to apply. It was found that some common equations developed for C-Mn
steels give quite reasonable predictions, particularly those in refs. [21,32]. One of these equations is as
follows:

d
rex
=0.35
-1

67 . 0
0
d (9)

where d
o
is the austenitic grain size before hot deformation.



41

Conclusions of Task 2.2.1
The main results and conclusions from the work carried out regarding flow stress and SRX behaviour
are as follows:
Hot deformation resistance of high-Mn TWIP steels is dependent on Mn content (strengthening about 2
MPa/wt%) and increases with increasing Al alloying up to 6% (strengthening about 12 MPa/wt%). Nb
and N in the contents used here in steels have a minor influence. The austenitic high-Mn TWIP steels
exhibit higher deformation resistance than those of low-C, C-Mn-Nb and austenitic stainless steels.Flow
stress curves exhibit broad stress peaks at quite low strains. However, the completion of DRX occurs
slowly. Very fine grain size is obtained as a result of DRX. SRX kinetics of TWIP steels is faster than
that of Type 304 and C-Mn-Nb steels and slower than that of low-C steels. Mn is the main element
retarding the rate of SRX and Al has only a minor contribution. The regression equation for the static
recrystallization kinetics for TWIP steels can be used to predict the SRX rate under given conditions.
Grain size will be refined effectively by SRX, and certain equations published for C-Mn steels can be
used to predict the grain size.


Task 2.2.2 Recrystallization kinetics under different cold rolling schedule
Introduction
The investigation on recrystallization behavior of TWIP steels has been focused on a thorough
characterization of the isothermal annealing behaviour of cold rolled TWIP2 steel (22% Mn, 0.6% C,
hot rolled band, 40% to 70% cold rolling reductions) in the temperature range 450-1100 C . The
assessment of the annealing effects has been made by following the Vickers macro-hardness, structure
(recrystallized fraction, grain size, proportion of twin boundaries) and texture evolution (microtexture).

Material and annealing treatments
Hot rolled TWIP2 samples (5.4 mm thick) were reduced by cold rolling at a CSM laboratory mill to
different thicknesses: 3.24 mm (R =40 %), 2.7 mm (R =50 %), 2.16 mm (R =60%) and 1.6 mm (R =
70%).
An OIM of the hot rolled structure of the starting material is shown in fig. 2.2.2.1. A non-equilibrium
grain structure typical of high temperature deformation with some residual deformed intra-grain
structure (subgrains) is evidenced by this OIM image. The grain size (mean linear intercept) is 23.3 m
(an upper bound, as twin boundaries were not counted). The structure of the cold rolled samples is too
distorted for being completely resolved by OIM. The micro-texture of the resolvable regions is a typical
FCC rolling texture. Practically it contains only the Brass orientation, {110}<112>, plus very weak
Goss {110}<001>and S {123}<634>components.
The cold rolled samples subjected to the annealing treatments summarized in Table 2.2.2.1.
The 450 C T 900 C treatments were performed in a salt bath furnace and were interrupted by
water quenching after different annealing times. The heating time was controlled by treating dummy
samples with inserted thermocouples. Heating time was always a small fraction of the time spent at
each treating temperature but for the nominal t 12 s ones.





42


Fig. 2.2.2.1: OIM image of hot rolled TWIP2 sample (inverse pole figure and grain maps, rolling plane
normal.


Treatments at 1000 C and 1100 C were performed in a resistance furnace under Ar protective
atmosphere and were followed by water quenching.
The fraction recrystallized for each annealing time, temperature and prior cold rolling reduction has
been deduced from hardness measurements complemented with metallographic and micro-texture
observations.


T (C) Time of annealing (minutes) at target T before water quench
450 0.02 (1 s) 0.2 (12 s) 0.5 (30 s) 1 3 9 27 81 243 729
600 0.02 (1 s) 0.2 (12 s) 0.5 (30 s) 1 3 9 27 81 243 729
700 0.02 (1 s) 0.2 (12 s) 0.5 (30 s) 1 3 9 27 81 243 729
800 0.02 (1 s) 0.2 (12 s) 0.5 (30 s) 1 3 9 27 81 243
850 0.02 (1 s) 0.2 (12 s) 0.5 (30 s) 1 3 9 27 81
In a salt bath
furnace
900 0.2 (12 s) 0.5 (30 s) 1 3 9 27
1000 3 9 27 In a mufla
furnace (Only for
R =60 %)
1100 3 9 27
Table 2.2.2.1. Annealing treatments


Recristallization kinetics
The evolution of static recrystallization fraction at two temperatures, 600 C, 650C and 700 C for 60%
cold rolling reduction is plotted in fig. 2.2.2.2 in order to check their agreement with an Avrami
behaviour.
For 600 C, recrystallization has not ended for the maximum time tested and the fraction recrystallized
being known from the metallographic observations, ( ) [ ] % 7 . 86 15 . 12
600

C rex
o h X . In fig. 2.2.2.3 is
shown the recrystallization kinetics at 700C for different cold rolling reductions. As can be noted at
700 C, recrystallization ends after 3 minutes, data for longer times are for grain growth.
Final grain size is very small: many nucleation sites are available because of the tremendous number of
twin intersections after 60% cold rolling deformation. Same observations have been made for
recrystallized grain sizes of austenitic stainless steel (metastable austenite) and TWIP steels [16].





43

0
0.2
0.4
0.6
0.8
1
1.2
0.00001 0.01 10 10000 1000000
t (s)
X
s
o
f
60 % REDUCTION
700 C
650 C
600 C

0
0.2
0.4
0.6
0.8
1
1.2
0.001 0.1 10 1000 100000
t (s)
X
s
o
f
t
40%
50%
60%
70%
700 C

Figure 2.2.2.2: Recrystallization kinetics for 60%
reduction derived from the softening by annealing
temperature of 600C, 650C and
700C as function of time. TWIP 2 steel with
composition 22% Mn- 0.6% C
Figure 2.2.2.3: Recrystallization kinetics for all
reductions derived from the softening by annealing
temperature of 700C as function of time. TWIP 2 steel
with composition 22% Mn- 0.6% C


Table 2.2.2.2 shows the individual values of ksoft and B (constants of the Avrami equation). The values
of the exponent are of the typical order of magnitude reported for other alloys. No intent of a refined
characterization of the kinetic equation of recrystallization has been pursued because the recrystallised
grain size is so small (less than 2 in all cases) and the time for complete recrystallization so small,
above 650C, that a finer analysis does not seem relevant for practical purposes.


Table 2.2.2.2. Values of ksoft and B (constants of the Avrami equation) obtained from Avrami fittings
to the recrystallization results.


With all the observations carried out, it is possible to draw an annealing map (table 2.2.2.3) in the
explored T-t sub-space that summarizes the different processes at work. A small region of static ageing
(hardening) is observed at low annealing temperatures and times. Other authors have observed dynamic
strain ageing from room temperature to 300C [11, 12]. No structural changes are detected at 450C; a
weak softening (weak recovery) takes place for long annealing times beyond the ageing region.




44

1100
1000
900
850
800
700
650
600
450
T [C] vs. t [s] 1 12 30 60 180 540 1620 4860 14580 43740
Recr ystall izati on. Negli gi bl e gr ain growth
Static agei ng by sol id solution segregation to disl ocati ons
Recovery. No r ecrystal li zation
Grai n gr owth. Recrystal li zation is completed

Table 2.2.2.3. Annealing processes map of TWIP steel in T-t space. Not explored regions in blank.


Grain growth kinetics
According to the measurements of grain sizes performed by EBSD-OIM, grain growth rate at 700 C is
very low. Recrystallized grain size is 1.5 m and recrystallization is reached after nine minutes of
annealing but grain size is only 2.27 m after twelve hours. It is still rather low, 4.2 m, after 27
minutes at 900 C. Only above 1000 C grain growth rate increases enough for reaching grain sizes
larger than 20 m in 27 minutes of annealing. From isochronal plots, it is possible to estimate the
activation energy for the grain growth processes QGG. Combining the data from annealing at 900 C,
1000 C, 1100 C, and assuming as activation energy the value QGG =363 60 kJ /mol calculated from
the isochronal plots, a good fitting of all the grain growth data is obtained with an exponent n
GG
3.5,
fig. 2.2.2.4.

y = 3.5407x - 38.315
R
2
= 0.8867
-40
-35
-30
-25
-20
-15
0 1 2 3 4 5
Ln (D*)
l
n
[
e
x
p
(
-
Q
G
G
/
R
T
)
t
]
Q
GG
= 363 60 kJ/mol

Fig. 2.2.2.4: Grain growth equation. D* is calculated from mean linear intercept method, twin
boundaries not counted as grain boundaries. TWIP2 steel with composition 22% Mn- 0.6% C.

Texture changes
The texture after cold rolling is the typical brass texture {011}<211>. The recrystallization texture
(without perceptible grain growth, grain size D <2 m) is rather similar to the rolling one, with a strong
brass component, plus a weaker {011}<100>component. After grain growth these texture components
remain but the texture intensity is even weaker, with intensity maxima smaller than 1.5. Fig. 2.2.2.5
shows the pole figures corresponding to the 60% cold rolled sample.




45




Fig. 2.2.2.5 Macro-textures, pole figures: a) TWIP steel 60% cold rolled with the typical brass-type
texture {011}<211>; b) Recrystallization texture, D 2 m; c) Grain growth texture with D 9 m.


Conclusions task 2.2.2
Recrystallized grain sizes of TWIP steel of 22% Mn - 0.6% C (in mass-%) cold rolled in the range
of 40%-70% reductions and isothermally annealed in the temperature range 600 C T 900 C are
very small, D 2 m.
At 450C the effect of annealing is very weak. After some seconds there is some hardening (static
ageing by solid solution segregation to dislocations) and a very weak softening thereafter,
attributable to recovery, without any noticeable metallographic changes.
Above 700 C, recrystallization is complete in less than nine minutes and takes less than ten
seconds above 800 C. At 900 C T 1100 C, the kinetics observed only corresponds to grain
growth.
Recrystallization and grain growth textures are very weak. Consequently, the elastic and plastic
anisotropies of annealed TWIP sheets will be negligible.
Although there is no apparent texture change from recrystallization to grain growth, there is a
strong change in the grain boundary composition. The fraction of 3 twin boundaries increases
suddenly from 14% to 40% when grain growth starts and it remains constant thereafter
independently of the grain size reached.
An empirical equation of grain growth for this steel has been obtained with an apparent activation
energy QGG =363 60 kJ /mol and an exponent nGG 3.9.



Task 2.2.3 Modelling of recrystallization behaviour of TWIP steels by modifying the available
mathematical models for austenitic steels and the relevant constitutive equations
Introduction
In modelling static recrystallization of cold deformed austenite three different approaches due to Zurob
and co-workers has been used [1-3]. Assuming that the grain boundaries interact with Mn atoms in this



46

TWIP steel, the velocity of the grain boundaries v
g
during recrystallization, can be related to the driving
force F, using Cahns theory of solute drag, quoted in [3].
In the following section, models for the fraction recrystallized evolution are described which all
consider the interaction of manganese solute atoms with grain boundaries. The three models have been
initially tuned using the experimental fraction softened curve of previous section. Next the best model
is then applied to a range of experimental fraction softened curves for various cold rolling reductions
and the results discussed. The models considered were:
1. Model n.1: Constant grain boundary velocity with site saturated nucleation.
The equation for the fraction recrystallized X
v
as a function of time t is the following
( )
3 3
exp 1 t fNv X
g v
= ,
where f is a shape factor (=4/3 for spheres), v
g
grain boundary velocity, N is the recrystallized nuclei
density.

2. Model n.2: Constant grain boundary velocity with a decreasing nucleation rate.
The equation for the fraction recrystallized X
v
as a function of time t is the following

( )
3
exp 1
g v
dgfv X = ,

Where g is a constant of the nucleation rate equation
Bt
g
N
r
+
=
1
,
f is a shape factor and d is given by:

( ) ( ) ( )
4
6
1 ln 6 2 3 6
B
Bt Bt Bt Bt
d
+ + +
=

3. Model n.3: Decreasing boundary velocity with site saturated nucleation.
The static recovery model used, is that due to Verdier et al [12] later expanded by Zurob.
In the model the stress due to dislocations
d
is related to time through [2]:

t
T k
Gb M k
RT
Q
G M
B
d
t d d

+ =
=
3
1 0
2 3
0 ,
sinh exp
3
4 1 1


,

where
d,t=0
is the initial stress,
d
is the Debye frequency (=1 X 10
13
s
-1
), Q
0
is the activation energy
for bulk self diffusion in austenite (=270 kJ /mol [13] ), k
B
is Boltzmanns constant and k
1
is a constant
less than unity.
Finally from [7] the fraction recrystallized is given by:

=

3
0
exp 1
t
g v
dt v fN X


Comparison of models with experimental results
As can be seen from figures 2.2.3.1-2-3, the model n.3, i.e. that in which the boundary velocity
decreases with time due to recovery, gives the best agreement with experimental data. Thus the
modelling of experimental data only model 3 will be used.



47

Model n.3 is applied to experimental data for different cold reductions with the annealing temperature
kept constant at 600C. The results are shown in fig. 2.2.3.4.

0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d


0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
ti me (s)
F
r
a
c
t
i
o
n

r
e
x
e
d
Figure 2.2.3.1: Comparison of model 1 (black line)
with experimental data for a cold reduction of 60%
with an annealing temperature of 600C.
Figure 2.2.3.2: Comparison of model 2 (red
line) with (corrected) experimental data for a
cold reduction of 60% with an annealing
temperature of 600C.

0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d


Figure 2.2.3.3: Comparison of model 3 (blue line) with (corrected) experimental data for a cold
reduction of 60% with an annealing temperature of 600C.



As can be seen from fig. 2.2.3.4 generally good agreement between model and experiment is obtained
for different cold reductions with N as the only free model parameter. The agreement for the cold
reduction of 40% is less good than for the other reductions however.
Comparison with the average N (N as 7.23 X 10
17
m-3) shows good agreement for reductions of 60%
and 70% but not for the intermediate reductions.
Applying the model n.3 with an average N (with A as 0.657 and k
1
as 0.0685) still gives acceptable
overall agreement with the experimental data. The fact that the model gives acceptable agreement for a
single value of N seems to suggest that the recrystallized grain size does not change significantly in the
range of reductions investigated.






48

0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d
0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d
A) B)
0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d
0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
1 10 100 1000 10000 100000
time (s)
F
r
a
c
t
i
o
n

r
e
x
e
d
C) D)
Fig. 2.2.3.4: Comparison of model 3 with a range of experimental data, for a constant annealing
temperature of 600C. A) 40% reduction B) 50% reduction C) 60% reduction and D) 70% reduction.

Conclusions task 2.2.3
Physically based recrystallization models have been applied to the experimental data for cold rolled and
annealed TWIP steel. Several models were considered with different assumptions for the nucleation
behaviour and boundary velocity behaviour. All models assumed that grain boundary mobility was
controlled by interaction with manganese solute atoms. The possible influence of twins on the
recrystallization process was not considered. From the modelling results the following conclusions can
be drawn:

The model which best described the experimental data was the model n.3 in which nucleation
was site saturated and the grain boundary velocity decreased with time due to static recovery.
Comparison of this model with more experimental data revealed good agreement when the
nucleation density was a free model parameter.
Imposing an average nucleation density and recalculating recrystallization curves still gave
reasonable agreement with experimental results.


Task 2.3 Study of the precipitation at equilibrium by means isothermal treatments. Precipitates
analysis by means of electron microscopy techniques (SEM-EDX, extraction replica for TEM).

The aim of this task is to study the precipitation behaviour of TWIP steel at different temperatures
(from 500C to 1000C) at long soaking time (approaching equilibrium conditions). The results will be
used to design the hot rolling processing conditions (coiling, annealing). The hot rolled strip samples
used for this activity are in the solution treated condition (1200C x 1h). In table 2.3.1 are reported the
annealing treatments carried out for all the TWIP variants.






49

Soaking
Temperature
(C)
Soaking time
(h)
500 10h
600 10h
700 10h
800 10h
900 1h
Table 2.3.1: thermal treatments for precipitation study.


The isothermal section of Fe-Mn-C [1] system in the range of 800C - 900C does not reveal the
precipitation of carbides. At temperature below 700C the -phase became more restricted and the
reduction of C solubility coincides with the occurrence of a complex series of equilibria between -
phase and Fe-Mn carbides. At temperature below 700C and for Mn content in the range 16-22%wt and
C =0.4-0.6%wt the most stable carbide is M
3
C cementite type (with C content about 7%wt). The
isothermal section of Fe-Mn-C and Fe-Mn-Al systems [1] highlights that at temperature lower than
600C, and in correspondence of segregated zone with lower Mn content (dendrite centre), the
austenite can be thermodynamically unstable and the formation of pearlitic phases containing cementite
and ferrite can occur [2]. This phenomena should occur on very long time (>10h) and is more
pronounced during massive carbide precipitation due to local lowering of the C in solid solution.



Precipitation analysis at scanning electron microscope
A first screening of the precipitation behaviour of the TWIP variants was carried out by means of LOM
and SEM aiming to evaluate the occurrence of carbide precipitation at temperature below 900C and the
differences in relation with the TWIP steel chemical composition. The aim of this qualitative analysis is
first of all to define the range in which the carbide precipitation has a massive aspect. The occurrence of
so huge precipitation must be absolutely avoided, in any step of the production route, because the
tensile properties of TWIP steel could be significantly affected. The results of the SEM-EDS analysis
carried out are summarised as follows.

Precipitation after 10h of soaking at T=800-900C
In fig. 2.3.1 are shown the typical microstructures found for each TWIP variant after soaking at 800C
for 10h. As can be noted no precipitation was observed by OM and SEM analysis. Only oxide particles
and MnS were detected. Tha same situation was found in the samples heated at 900C for 1h.






50


TWIP 1 TWIP2

TWIP3 TWIP4

TWIP5
Fig.2.3.1: Microstructures of the TWIP variants after soaking at 800C for 10h.



Temperature range 500-700C
Carbides precipitation is detected in the range 500-700C but with remarkable differences between the
TWIP variants. In the following sections are summarised the results for each variant.

TWIP 1 steel
TWIP 1 grade is characterised by the lowest C content (0.01wt%) and by a significant second phase
ferrite content (about 6%). This characteristic suggests a lower austenitic stability with respect the other
TWIP variants. Very long permanence (10h) at 700C resulted in additional ferrite formation. The
ferrite particles reveal a higher Al and Si content and lower Mn content with respect to austenitic matrix
(fig. 2.3.2). The formation of ferrite was also confirmed by ferritoscope measurement.



51


Fig. 2.3.2: TWIP1 - 700Cx10h.


TWIP2 - TWIP3 steels
TWIP2 and TWIP3 are characterised by a Mn content in the range 18-22wt% and C content 0.6wt%.
Carbides precipitation in these steel variants is quite abundant in the temperature range 500-600C. In
the fig. 2.3.3 is shown a SEM image of carbides precipitated on the austenitic grain boundaries of
TWIP2 after a soaking at 700C for 10h. The semi-quantitative analysis gave a C content of about
7%wt consistent with carbide of cementite type. In fig.2.3.4 is shown a SEM image of carbides
precipitated on the austenitic grain boundaries of TWIP3 after a soaking at 700C for 10h. In fig.2.3.5-6
is shown carbide precipitated on austenitic grain boundaries at 600Cx10h on both TWIP2 and TWIP3.




Fig. 2.3.3: SEM image of the TWIP2 sample after soaking at 700C for 10h.



Fig. 2.3.4: SEM image of the TWIP3 sample after soaking at 700C for 10h.




52



Fig. 2.3.5: SEM image of the TWIP2 sample after soaking at 600C for 10h.


Fig. 2.3.6: TWIP3: SEM +EDS image of the cementite precipitated on the austenitic grain boundaries
after a soaking at 600C for 10h.


TWIP4
TWIP4 grade is characterised by a Mn, Al and C content respectively of 16%, 1.5% and 0.4%. In the
temperature range of 500-700C TWIP4 grade revealed a formation of ferrite and precipitation of
carbide. In fig 2.3.7 is shown the microstructure of TWIP4 after 10h soaking at 700C in which can be
noted the ferrite formed. The carbides were not resolved probably due to fine dimensions but the
presence of a higher carbon content with respect to matrix suggests that the phase formed are
ferrite+carbides. In the fig. 2.3.8-9 is shown the microstructure of TWIP4 after 10h soaking at 500-
600C in which can be noted the ferrite formed.

Fig. 2.3.7: TWIP4 at 700C: within some grains is detected the precipitation of ferrite +carbides.






53



matrix particle
Wt% Wt%
C - K 0.5 2.9
Al - K 1.4 1.7
Si - K 0.3 0.8
Mn- K 18.2 15.4
Fe- K 77.2 78.4
Fig. 2.3.8: SEM +EDS image of the TWIP 4 samples after a soaking at 600C for 10h.




Fig. 2.3.9: SEM +EDS image of the TWIP 4 samples after a soaking at 500C for 10h.


TWIP 5 steel
TWIP5 is characterised by a Mn content of 22wt% and a C content of 0.2wt% and Nitrogen of 0.2wt%.
The precipitation behaviour of TWIP5 is quite different with respect to previous variants. SEM analysis
carried out on the sample annealed at 700C and 600C for 10h did not reveal any presence of carbides
even at quite high magnification. A fine precipitation of carbide particles (fig.2.3.10) was detected after
soaking at 500C for 10h. Also in this case the small carbides were recognized as cementite because the
(Fe, Mn)/C ratio is consistent with cementite carbides (C content about 7%wt).







54


Fig. 2.3.10: TWIP 5 specimen after soaking for 10h at 500C.


Extraction replica analysis by transmission electron microscopy
Single stage carbon extraction replicas were prepared using the conventional method starting from a
surfaces prepared as for optical microscopy and using a selective electrolytic dissolution method to
remove the matrix around the carbides. The extracted carbon replicas were examined using a J eol J EM
200CX (STEM) electron microscope operated at 200kV. The replica extraction was carried out on
TWIP samples soaked for 10h at 600C and 700C. The results of the replica analysis are detailed as
follows.

TWIP 1
TEM extraction replica on TWIP1 steel confirmed the presence of ferrite+carbides. In fig.2.3.11 can be
noted rows of particles extracted from larger island in which can be recognized particles of ferrite with
a typical higher content of Al and Si and lower content of Mn with respect to matrix (Mn is about 22%).
Carbides detected are of cementite type (FeMn)
3
C (fig. 2.3.12) and are characterized by finer size with
respect to ferrite particles. The STEM-EDS analysis of ferrite and carbide particles are reported in
fig.2.3.11.


Fig.2.3.11: TWIP1-700C: Low magnification image.



55




Fig.2.3.12: TWIP1-700C: Carbide of cementite type (FeMn)
3
C, the analysis is reported in fig. 2.3.11.


TWIP2
The precipitation features of TWIP2 at 600C and 700C, in terms of type and chemical composition,
are the same. The remarkable difference is in terms of amount of precipitates: at 700C the number of
precipitates is significantly lower than at 600C.
Two type of precipitates were found:
1. (Fe, Mn)
3
C cementite
2. Vanadium carbonitrides characterized by fine size ( <50nm).
The presence of Vanadium carbonitrides is due to unwished presence of V in ferroalloy during ingot
casting. In fig.2.3.13-14 are reported the picture of the two carbide types with the relevant diffraction
pattern.



Fig. 2.3.13: (Fe,Mn)
3
C carbide image with relevant diffraction


In the fig. 2.3.14 is reported the image of the Vanadium carbo-nitride precipitate type.




56



Fig.2.3.14: Vanadium carbo-nitride image with relevant diffraction.


TWIP3
TWIP3 steel is characterized in terms of chemical composition by Nb addition. As expected the
precipitation of carbo-nitride is strongly affected by this micro addition. In fig. 2.3.15 is shown the
difference in terms of number of Nb carbo-nitrides between 600C and 700C (the total number of
precipitates analysed is 50). As can be noted the amount of NbCN at 700C is significantly higher and
even the particle size are bigger. This means that at relatively low temperature (below 600C) the
precipitation of Nb carbo-nitrides is strongly reduced. In addition to NbCN, carbides of cementite type
(Fe, Mn)
3
C were detected. The latter are predominant at 600C as can be noted in the fig.2.3.16.



TWIP3-600C TWIP3-700C
Fig.2.3.15: Nb content of the precipitates selected on extraction replica.





57


Fig.2.3.16: TWIP3 600C: (Fe,Mn)
3
C carbide image.


TWIP5
STEM-EDS analysis was carried out on TWIP 5 sample soaked at 700C for 10h. A quite low fraction
of fine (Ti, Al) carbo-nitrides (size less than 150nm) was detected. The presence of Ti and Al is due to
unwished residual presence in ferroalloy during ingot casting. In fig. 2.3.17 is shown the image of a
typical (Ti, Al) carbo-nitride.

Fig. 2.3.17: TWIP5 at 700Cx10h - (Ti, Al) carbo-nitride.





58

Conclusions of task 2.3
The precipitation behavior of TWIP steel depends on one side on the C, N, and elements carbide-nitride
formers (Ti, Al, Nb, V) content, but on the other side is strongly affected by thermodynamical stability
of austenite in the range 500-700C; Infact the ternary system Fe-Mn-C under defined conditions of
temperature and chemical composition shows that the austenite could partially transform in
ferrite+carbides (pearlite like structure).
The study carried out on TWIP steels by SEM-EDS and STEM-EDS allows to state the following
conclusions:
Both TWIP1 and TWIP4 revealed, at temperature below 700C the tendency of austenite to
destabilize and to forme ferrite+carbide structures. These observation is in agreement with other
results achieved on TWIP1-4 and confirm that the austenite stability of these steel grades is
lower with respect to reference grade TWIP2 (Fe-22Mn-0.6C);
TWIP2 and TWIP3 show a similar behavior. Both steel grades revealed in the range 500-700C
a massive carbide precipitation of cementite type (Fe, Mn)
3
C. No ferrite phase was detected in
the range 500-700C.
TWIP5 grade revealed a very stable structure: no massive carbide precipitation was detected in
the range 500-700C. The precipitated particle are constituted of cementite carbides and fine
(Ti,Al) carbo-nitrides. No ferrite phase was detected even after long soaking time in the range
500-700C.

Task 2.4 Industrial feasibility of hot and cold processing route of TWIP steels

Introduction
The design of the hot and cold strip processing route of TWIP steel consisted in the definition of the
operating practice of the following steel manufacturing steps:

1. Hot rolling process
Slab reheating process: the goals of the study are the definition of the slab
discharging temperatures, evaluation of impact on usual C-steel production,
and minimization of fuel consumption.

Thermo-mechanical treatment:
-design of hot rolling schedule;
-cooling pattern on ROT;
-coiling temperature;
Hot rolled strip annealing conditions (if necessary);

2. Pickling process conditions

4. Cold rolling process (plain strain compression tests task 3.4)

5. Cold rolled strip annealing conditions.


The definition of the industrial operating practice have adopted, on one side, the results arising from the
basic investigations and, on the other side, additional activities were carried out as for basic creep
strength evaluation, hot and cold deformation strength evaluation, characterization of pickling behavior.
In the following are detailed the results find out.



59


Slab reheating process

Qualitative creep strength evaluation
One important aspect in the design of the manufacturing cycle consists in the definition of the optimal
slab reheating temperature. The need of high finishing rolling temperature (900C) impose as a
consequence to choose a high entry temperature for roughing mill (1180-1200C) and entry finishing
mill (1100-1150C). This means that the TWIP slabs must be reheated at a temperature very close to
usual carbon steel slab reheating temperature, that is 1200-1250 C.
From CSM laboratory results and from thermo-dynamical calculations TWIP steels are expected to be
characterized by a lower T
solidus
(ranging 1320-1350C) with respect to a conventional C-Mn steel
(Tsol=1490-1500C) selected as a reference. This means that the feasibility of slab reheating in the
range 1220-1250C has to be carefully verified in order to avoid problems in the reheating furnace
(walking beam) and in following hot rolling process.
To evaluate qualitatively the creep resistance behavior at high temperature (1200C) a test based on the
sag test specification was carried out.
This test consisted in measuring the bending occurred after a 3h soaking at 1200C of TWIP steel
specimens with same geometry (200mm length, 20mm width, 2.0 mm thickness). For reference the tests
was carried out also for a conventional carbon steel (C,Mn steel grade). The tests was carried out
adopting a laboratory resistance furnace with a controlled oxygen atmosphere (O
2
about 5%). The
bending measured after treatment is strongly dependent on the sample geometry and of course the
thinner is the specimen the higher is the bending. In the following are presented the results achieved
adopting specimens with 2mm thickness.
The results in terms of max bending in the centre of specimen are reported in table 2.4.1. As can be
noted the creep resistance of TWIP2 at 1200C is significantly lower than the reference C, Mn steel
samples.



Sample size
NIM length (mm) thickness[mm]
Average bending
[mm]
TWIP 2 200 2.00 22
TWIP 3 200 2.00 15
TWIP4 200 2.00 16
C, Mn steel 200 2.00 12
Table 2.4.1: Bending after a sag test with 3h soaking at 1200C.


TWIP3 as well as TWIP4 steel variants show an intermediate creep strength with respect to
conventional C, Mn steel and TWIP2. The difference between TWIP2 and TWIP3/TWIP4 could be
ascribable to the different T
solidus
as reported in the table 5.1.2.
The results of this qualitative tests indicate that the TWIP slabs could show, during the reheating
process in walking beam, a slightly larger bending at high temperature and this suggests, for safety of
the plants, to adopt slabs with maximum feasible thickness (250mm) and reduced slab length (5m
instead of usual 10m) in order to control the maximum bending of slabs in furnace.
Due to their austenitic structure the expected thermal conductivity of TWIP steels, below about 800C,
should be significantly lower than ferritic steels. In order to avoid too long reheating time, loss of
productivity and to minimize the fuel consumption, the slab hot charging at a temperature higher than
600C is recommended.



60

For this scope hot charging tests were carried out in order to verify the industrial feasibility at the
Duferco-La Louviere plant and hence to define the best practice. In parallel calculations were carried
out in order to evaluate the effectiveness of hot charging in terms of productivity and to evaluate the
impact for insertion of mini-program inside usual rolling schedule taking into consideration the
expected total reheating time.
In fig 2.4.1 is shown the typical temperature evolution of the conventional route. The slab from oxy-
cutting, down the casting machine, until the piling up in the storage area. As can be noted the slab
temperature decreases quite fast in the first part but after pile up the cooling rate is slower (about
20C/h).
The average time to achieve 500C is, adopting the conventional route, about 14 h.
An insulated box suitable for hot charging was realized setting-up a device already existing in steel
works. To increase the thermal insulation a special attention was devoted to control the air circulation
within the box.
The slab temperature evolution adopting a hot charging route gave the following results. In fig.2.4.2 is
shown the slab temperature evolution from the oxy-cutting until the storage within the insulated box.
The slab monitored was the second as stacking order in the box. It can be noted that, a part the initial
drop due to air cooling during transfer, the slab temperature drop (in the range 600-400C) is strongly
reduced (7C/h) in the case of slab stored in box to be compared with 18C/h for conventional slab
piling up.



.

Fig.2.4.1 Typical slab temperature in conventional route.

Piling up



61


Fig.2.4.2 Typical slab cooling evolution adopting the hot charge route (piling up in a box).


Hot rolling schedule design
The hot rolling schedule design consisted in the following main activities:
1. Evaluation of the high temperature mean flow stress of TWIP steels from hot compression tests;
2. Calculation of hot rolling schedule by means of CSM model taking into account the technical
specification of the DLL hot rolling mill;
3. Definition of the strip cooling pattern on run out table and coiling temperature.
Evaluation of mean flow stress from hot compression test results
Calculation of the TWIP steel flow stress on the basis of flow stress measurements carried out by means
of compression tests with a strain rate of 0.1s-1. Assuming that the maximum flow stress curve is an
estimation of the mean flow stress it was applied the Ford-Alexander equation to calculate the rolling
forces. This assumption is considered reasonable even if the measurements were made at strain rate
significantly lower than the strain rate experimented in industrial hot rolling conditions.


Piling up in box



62


Fig. 2.4.3: Comparison of the MFS of TWIP2 and a conventional low-C steel (strain rate 0.1s-
1
).



In fig 2.4.3 is shown the mean flow stress of TWIP2 steel. In the same plot is reported also the mean
flow stress of a reference low C-Mn steel. As can be noted from the comparison results that TWIP2
steel has a significantly higher (70%) flow stress compared with a conventional low-C steel.

Calculation of HRM schedules
In the following the results of rolling schedules calculations of TWIP steel (Fe-22Mn-0.6C) on both
roughing and finishing mill at the DLL Hot Strip Mill are reported.
The following conditions have been taken into account:
Discharging slab temperature: 1200 C
Tranfer time on the run-out table from reheating furnace to roughing mill stand: 35 sec.
Fe-22Mn-0.6C TWIP steel.
Initial slab thickness: 250 mm
Initial slab length: 5000 mm
Rolling schedules are calculated for the bar head threading in all the passes

The dimensions considered in the calculations are reported in the next tables.


**************************************************************************************
** Rever si ng Roughi ng Hot St r i p Mi l l Pr eset - Cal cul at ed r ol l i ng schedul e **
**************************************************************************************

St r i p wi dt h [ mm] : 1000
Pass r educt i on [ %] : 13. 52 19. 06 23. 43 25. 15 29. 21 34. 51 39. 78
Bar t hi ckness [ mm] : 250.00 216.20 175.00 134.00 100.30 71.00 46.50 28.00
Sur f ace bar r ol l i ng t emper at ur e [ C] : 1137 1097 1087 1068 1069 1063 1068 1066
Bar st r ai n [ - ] : 0. 145 0. 211 0. 267 0. 290 0. 345 0. 423 0. 507
Bar st r ai n r at e [ 1/ sec] : 1. 4 1. 9 2. 5 3. 0 3. 7 4. 8 6. 1
Bar yi el d st r ess [ N/ mm2] : 130. 0 136. 1 141. 4 145. 1 151. 1 159. 9 169. 4
Rol l i ng For ce [ kN] : 18064 21745 23528 22779 23567 24992 26056
Bar t hr eadi ng speed [ m/ sec] : 1. 25 1. 35 1. 40 1. 40 1. 40 1. 40 1. 35
Hi gh r ol l i ng speed [ m/ sec] : 1. 25 1. 35 1. 80 2. 80 3. 30 4. 20 4. 50
For war d sl i p [ - ] : 0. 020 0. 025 0. 033 0. 042 0. 057 0. 081 0. 116
Rol l i ng t or que [ kNm] : 1544 2052 2216 1947 1881 1828 1663
Mot or power [ kW] : 4934 7042 7827 6818 6495 6174 5244
**************************************************************************************

Table 2.4.2: HRM Rolling schedule - TWIP 22Mn 0.6C steel- slab format 1000x250x28 mm.



63


Table 2.4.3: Calculated TWIP steel finishing rolling schedule for strip format: 1000x28x4. mm.


Discussion of results
The calculated MFS (Fig. 2.4.3) reaveals that TWIP2 steel is characterised by significantly larger flow
stress than the MFS of conventional low C-Mn steel.
The conclusions of the hot rolling schedule calculations can be summarised as follows:

Final rolling temperature should be greater than 900 C to avoid excessive rolling loads and
torques;
Incoming bar temperature at the finishing mill entry should be as higher as possible(>1040C)
to decrease the motor current;
Hot rolling of TWIP steel strips seems to be feasible, in terms of rolling loads and torques, till
to 1000 mm width and final thickness down to 4 mm.


ROT cooling pattern and coiling temperature
TWIP steels are characterised by a stable austenitic structure in the whole temperature range. This
means that the strip cooling pattern after hot rolling does not play any metallurgical role. Nevertheless
after hot rolling, even if, no phase transformation occurs the following topics have to be considered:
Permanence in the temperature range 600-900C could provoke strip surface oxidation (scale
growth, decarburization, intergranular oxidation);
Huge carbide precipitation occurs during slow coil cooling in the range 500-600C;

Coiling at high temperature (700-750C) could favour a partial recrystallization without the need of
additional continuous or batch annealing cycle. Nevertheless the risk of carbide precipitation during coil
cooling has to be considered. Infact under the typical coil cooling rate conditions the time to cross the
range 500-600C can reach few hours. So the best strip cooling conditions on the run-out-table are:

ROT cooling pattern: continuous cooling pattern from finishing rolling temperature (900C)
down to coiling temperature (CT) using the water curtains cooling system on the run out table.
Coiling temperature: coiling in the range 450- 500C.




64

Hot rolled strip annealing conditions
The hot rolled strip microstructure can be strongly affected by:

Hot rolling schedule: a proper choice of the hot rolling schedule allows to activate the dynamic
recrystallization.
Run-out table strip cooling pattern and coiling temperature: High coiling temperature could
activate static recrystallization.

This means that if dynamic recrystallization is activated or high coiling temperature (>700C) is
adopted, to promote static recrystallization, a recrystallized (even partially) structure can be achieved
and the annealing treatment of hot rolled strip can be avoided.
Conversely if during hot rolling the dynamic recrystallization is not enough and/or the coiling
temperature is too low to promote static recrystallization, in this case for the follow up of the industrial
manufacturing route (cold rolling) a annealing cycle is necessary.
In the latter case on the basis of the results of task 2.2.2, the annealing conditions could be defined as
follows: soaking temperature at 1000C for a soaking time of 30 s (continuous annealing line).

Pickling ability characterization
The pickling behavior of TWIP steels was evaluated on strip samples having a scale that could be
considered as close as possible to the industrial hot band. The strip samples used for the
experimentation were obtained through the following steps:

1. Hot rolled strips (TWIP and reference low carbon steels) were mechanically polished in order
to remove completely the scale and simulate the steel condition at the entry finishing mill (after
descaler);
2. The samples were heated in inert atmosphere (N
2
);
After about 2 min for temperature homogenization was introduced air in the furnace in order to form the
scale layer on the samples. To simulate the coiling, the samples were cooled down slowly in a furnace
from a temperature of 700C down to RT.


TWIP steel scale characterization by SEM
In the following sections are reported the results of scale analysis by means of SEM-EDS.

TWIP1 and TWIP4 (Fe-Mn-Al-Si-C)
Both TWIP1 and TWIP4, in terms of chemical composition, are characterized by a significant Al
content. This common aspect determines a similar scale structure and composition. The results can be
summarised as follows:

Outer scale layer: the outer layer is constituted of a matrix of Fe-Mn oxide (Fe is the main
constituent). Dispersed in the matrix were detected a second phase of spinel particles
(Al
2
O
3
)(Fe,Mn)O.
Internal oxidation layer (interface with steel):
For TWIP1 sample the base steel, at interface scale-steel, is Fe-enriched and a fine
precipitation of small Fe-Mn oxide particles is detected.
For TWIP4 sample the base steel, at interface scale-steel, is Fe-enriched and a fine
precipitation of small Fe-Mn oxide particles together with rod-like spinel phase
particles is detected.

In fig. 2.4.4-5 are reported the scale structure and main phases compositions detected on TWIP1 and
TWIP4 steel variant.



65





Fig 2.4.4: TWIP1 scale analysis. Fig 2.4.5: TWIP4 scale analysis.


TWIP2-TWIP3-TWIP5 (Fe-Mn-C-N)
The scale characteristics of TWIP2, TWIP3 and TWIP5 are quite similar. The results of SEM-EDS
analysis can be summarised as follows:

Visual aspect : brittle and porous;
Outer scale layer: the outer scale layer is constituted of a matrix of Fe-Mn oxide. In terms of
second phase some difference are found:
For TWIP2 sample the second phase is constituted of Fe-Mn-Si oxide particles (Mn is
the main constituent).
For TWIP3 and TWIP5 the second phase is constituted of metallic Fe-rich particles;

Internal oxidation layer (interface with steel): at the interface scale-steel the base steel is Fe-
enriched and a fine precipitation of small Fe-Mn oxide particles is present.


In fig. 2.4.6 is reported the scale microstructure and main phases detected on TWIP2 and TWIP3 steel
samples.





66


a) TWIP 2 scale. b)TWIP3 scale.
Fig.2.4.6: Scale microstructure and main phases detected on: a) TWIP2 and; b) TWIP3 steel samples.





TWIP 5 scale analysis.
Fig. 2.4.7: Scale microstructure and main phases detected on TWIP5.






67

Summary of results
All TWIP variants are characterized by a outer scale layer constituted of a Fe-Mn oxide matrix
in which are embedded second phases particles. The chemical composition of these particles
depends on specific steel chemical composition and in particular on the presence of Al.
Therefore in presence of Al (TWIP1 &TWIP4) the second phase particles are spinel oxide
particles (Al
2
O
3
)(Fe,Mn)O. In TWIP2-3-5 variants (no Al) the second phase are constituted of
metallic particles (Fe-rich).
The internal oxidation layer, at the interface scale-steel, is constituted of Fe-enriched metallic
matrix in which are precipitated Fe-Mn oxide particles. This layer plays an important role in
pickling ability and for this reason the pickling ability of TWIP steels is expected to be
generally good due to presence of metallic Fe-enriched layer together with an overall brittle
aspect.


Pickling tests
The aim of this activity is to evaluate the pickling ability of TWIP steels using as reference a
commercial low C-Mn steel. The procedure adopted for pickling tests can be described, for each TWIP
variant, in the following steps:

Preparation of a temperature controlled tank (66C) with a water solution of 140 g/l HCl and
5g/l Fe
2+
and 1ml/l inhibitor Leuzolit extra 284M.
Measure of weight and dimensions of samples;
Immersion in the pickling bath for a fixed timet
i
;
Washing, cleaning and weighting of samples;
If after t
i
the sample did not reveal a good pickled surface the procedure was repeated for a
longer time t
i
+ t
i
.

The results of the tests carried out in terms of average scale loss per second are reported in the table
2.4.5.


Table 2.4.5: Results of the pickling tests.


Further tests would be required for scaling up to industrial size as the mechanical conditioning of scale
was not carried out before pickling (to get a cracked scale that favours the acid percolation and reduce
the pickling time). Summarising the results yield to the following conclusions:

The steel TWIP1, TWIP2 and TWIP3 reveal a good pickling ability (in HCl) in terms of
soundness of pickled strip surface, even if in comparison with the reference low carbon steel
the pickling kinetics is slightly slower.
The steel TWIP4 reveals zone with residual scale even at longer immersion time in the pickling
solution.



68

The steel TWIP5 requires longer pickling time with respect to reference and also with respect to
the other TWIP1,2,3 steels.


Conclusion of task 2.4
The task 2.4 was incentrated on demonstrating the feasibility of TWIP steel production at Duferco La
Louviere steel works and to define the industrial conditions for TWIP steel processing. The attention, of
course, was focused mainly on the hot rolling process because it is well recognized that TWIP steel are
characterized by a quite high flow stress at high temperature. The results of the study allows to
conclude that TWIP steel hot rolling is feasible at Duferco La Louviere plant, provided that a dedicated
operating practice, quite different from conventional low C-Mn steel, is adopted. This is the result from
the point of view of plant capability.
Slab hot charging at a temperature higher than 600C is recommended to avoid too long reheating time,
loss of productivity and to minimize the walking beam fuel consumption.
Summarising the operating practice for hot rolling process of TWIP steel production are:

Slab dimensions: thickness 250mm, width 1000mm, length 5000mm;
Slab hot charging;
Slab discharging temperature range: 1180-1220C;
Entry finishing temperature range: >1040C;
Finishing rolling temperature: 900-920C;
Hot band thickness achievable >4.0 mm;
Coiling temperature: 450-500C.
Hot rolled strip pickling: conventional pickling process as adopted for C-Mn steel (HCl acid).






























69

WP3 Study of the deformation mechanisms and strain hardening behaviour

Task 3.1 Characterization of mechanical properties in relation with the microstructure,
dominating deformation mechanism, strain rate and temperature.
The activities of task 3.1 are articled in 5 subtasks. The results are reported in the following sections.


Task 3.1.1 Static uniaxial tensile tests to investigate the deformation mechanisms transition
(deformation twinning --> dislocation glide) and strain hardening behaviour
The activities of the subtask 3.1.1. revealed a more than expected complexity mainly due to necessity
of a in-depth investigation on the effect of hydrogen and decarburization on embrittlement of TWIP
steel. For this reason the activities were organized in further three subtasks as reported below.


Task 3.1.1.1 Quasi static tensile tests and strain hardening behaviour analysis
Quasi static tensile tests for a qualitative study of the effect of strain rate and temperature
on tensile behaviour and strain hardening analysis.


Task 3.1.1.2 Characterization of austenite phase stability and microstructural evolution in
TWIP grades during deformation at different temperature
Investigation on deformation mechanism transition at high temperature (deformation
twinning dislocation glide);
Characterization of austenite phase stability and microstructural evolution in TWIP grades
during deformation in the temperature range -180C350C (LOM, XRD);


Task 3.1.1.3 Investigation on TWIP steel embrittlement
Due to anomalies detected during test performance and unexpected results on tensile tests (poor
elongation) it was decided to carry out a in depth investigation on the causes of the large
scattering of tensile properties revealed by TWIP steel. This subtask was not included in the
technical annex of the project. The activities carried out were:
Metallographic examination of selected tensile specimens in order to characterize the strip
microstructure, presence of defects and analysis of surface oxidation and decarburization;
Low strain rate tensile tests on H-charged samples and internal hydrogen behavior (TDA).


Task 3.1.1.1 Quasi static tensile tests and strain hardening behaviour analysis
Tensile tests, at room temperature, were carried out on all the TWIP variants and the results are reported
in the table 3.1.1.1. The tensile specimens are in the state of cold rolled and annealed at 1000Cx5min
under N
2
atmosphere. The following features can be highlighted. TWIP2 steel is characterized by an
excellent elongation 82-88%. However also the other steel are characterized by quite high elongation to
rupture (A80%) around 60-65%. These quite high elongations are due to large strain hardening
coefficient n ranging between 0.55-0.58. TWIP5 steel is the exception because the coefficient n is
significanly lower (0.4). In terms of yield stress and tensile strength some considerations can be
underlined: TWIP steels are characterized by relatively low yield stress (240-280Mpa) and quite high
tensile strength (820-930Mpa). TWIP5 steel has a different behaviour because yield stress is higher and
a tensile strength is lower than TWIP1-2-3-4 grades.





70


Table 3.1.1.1: Tensile test at 20C results (cold rolled and annealed at 1000Cx5min).


Tensile properties: effect of temperature
The tensile properties of TWIP variants (TWIP2-3-4-5) were characterized at different temperature 20-
350C and strain rate. The occurrence of anomalies of tensile tests performance, mainly in terms of
scattering of elongation, was highlighted. The tensile tests were repeated with a different preparation of
the specimens, i.e. the samples after annealing were mechanically polished in order to remove a surface
layer of about 0.5 mm (table 3.1.1.2). The comparison of the tensile tests results with and without
surface polishing is shown in fig. 3.1.1.1.


Table 3.1.1.2: Tensile test results at different temperature with mechanically polished surface.



71

As can be noted the elongations of polished tensile specimens are less scattered and typically are
located at the upper bound of scattering band.
As can be noted the temperature influence on tensile properties of the five TWIP grades is very similar
with only some quantitative differences. The yield stress is slightly affected by temperature while the
tensile strength is significantly influenced by temperature. This means that at higher temperature the
Rp
0.2
/UTS ratio tend to increase due to progressive change of the deformation mechanism
(twinningdislocation glide) and a consequent reduction of the strain hardening ability and elongation
is detected (figure 3.1.1.1a-b).


a) b)
Fig. 3.1.1.1: a) tensile tests results carried out at room temperature and higher temperature 150-350C;
b) tensile tests results carried out at room temperature and higher temperatures 150-350C.


Tensile properties: Strain rate sensitivity
The strain rate sensitivity of the five TWIP steel grades was evaluated collecting all the data available,
torsion tests, tensile tests and Hopkinson bar tests as well. All the mechanical tests were carried out at
room temperature and the grain size of the specimens were in the range of 10m<D<19 m taking into
account twin boundaries as a grain boundaries. Merging all the data obtained in this project in a single
figure (tension and torsion, Von Mises equivalencies, no distinction between steels, 8 orders of
magnitude of equivalent strain rate), figure 3.1.1.2 is obtained. In fig 3.1.1.2a is shown the yield stress
behaviour as a function of strain rate. As can be noted, the behaviour of the five TWIP grades is very
similar but with only some quantitative differences.
The yield stress is substantially unaffected by strain rate up to 10
2
s
-1
. This means YS is almost constant,
i.e. sensitivity is about zero, over the strain rate range from 0.001 up to 100 s
-1
.
Only at very high strain rates ( 200 >
&
s
-1
) there is a strain rate induced increment of the flow stress.
This results is confirmed even at higher deformation up to 0.25 equivalent plastic strain.
At higher equivalent plastic strain the behaviour of TWIP steels appears different (fig 3.1.1.2b). In this
case a negative strain rate sensitivity can be detected in the strain rate range from 10
-3
up to 10
-1
s
-1
.
Taking into account the negligible strain rate sensitivity of Ys appear reasonable to ascribe this behavior
to adiabatic heating of specimen. Infact for yield strain (almost) no work has been done yet, so no
adiabatic heating can be expected.
As it is well known the adiabatic heating is related to heat production during the work done during the
deformation process of a specimen. However, at low strain rate, part of heat will disappear during slow
straining, so that temperature increment remains lower (zero at strain rate below 0.0001 /s). At strain
rates, high enough, the heat loss will remain insignificant, so that temperature increase is about
independent of strain rate. This limit seems to be about 0.01 /s. Hence, at higher strain rates than this,
temperature rise is constant (50C after 0.4 strain and about 100 C after 0.9 strain).



72

In fig 3.1.1.2b the flow stress at 40% as a function of strain rate is shown. It can be noted that at strain
rates 0.01 /s and above, the stress slightly decrease (from 1300 to 1100 MPa). This shows that
something is causing negative strain rate dependence/sensitivity. This could be the evidence of an
intrinsic characteristic as reported in literature in TWIP steels but, in this case, it appears as a result of
adiabatic heating of the specimens.


a) b)
Fig. 3.1.1.2 The strain rate sensitivity of the five TWIP steel grades was evaluated collecting all the
data, torsion, tensile tests and Hopkinson bar tests as well.



Tensile properties: Strain hardening behavior

Case 1: room temperature
The work hardening rates for each TWIP steel is reproduced in figure 3.1.1.3. This analysis of the work
hardening behaviour was obtained by plotting the work hardening rate (

d
d
) against strain. To obtain
meaningful plots the experimental data was first smoothed by calculating a moving average of stress
and strain values. A 6 order polynomial law was then fitted to each curve (plastic region only) and the
work hardening rate obtained as a function of strain from the fitted polynomial.


Fig. 3.1.1.3: Calculated work hardening curves for each TWIP grade.




73

From figure 3.1.1.3 it can be seen that the work hardening curves can be divided qualitatively into 3
stages.The first stage (decreasing hardening rate) is attributed to dynamic recovery. The change in
hardening rate at the onset of stage 2 has been found to be due to the start of twinning. The new twins
act as barriers to dislocation motion, and lead to an increase in strain hardening rate. Depending on the
extent of twinning, these leads to the observed overall hardening rate to decrease at a lower rate, remain
constant or for extensive twin formation to actually increase [4,5]. The third stage (decreasing
hardening rate), has been interpreted as a region where further twin formation becomes difficult i.e. a
region where the rate of twin formation decreases [4].
What it seems really peculiar of TWIP2 and TWIP3 steel is the second stage in which the strain
hardening increase with strain. This should be related to the effect of deformation induced twinning
occurring after the first stage predominated by dislocation glide.
The comparison of the stress-strain curves for TWIP 2 and TWIP3 led to the conclusion that the larger
work hardening rate in TWIP 2 could be a consequence of a greater degree of twinning compared to
TWIP 3. From table 3.1.1.1-2 it can be seen that the UTS and elongation are significantly larger for
TWIP 2 compared to TWIP 3, again consistent with a greater degree of twinning in TWIP 2. For the
TWIP4 grade on the basis of the previous results it is possible to argue that the increase of work
hardening in the second stage is a mixed contribution of strain induced alpha and/or epsilon martensite
together with twinning. The balance of these mechanisms is responsible for the different behavior.


Modelling the work hardening
This analysis was carried out on TWIP grades 2 and 3 in which can be assumed that during deformation
no strain induced phases are produced. Thus for these steels the stress-strain curves can be analysed
further by applying a physical model for deformation of TWIP steels due to Bouaziz et al. [7].
The model fitting parameters are
0
(yield stress), m (parameter related to SFE), k (dislocation forest
hardening coefficient) and a (coefficient related to dynamic recovery). The values of the other model
parameters used are shown in table 3.1.1.3 below:

Parameter Value Reference
M 3 [7]

1
0.35 [9]
G 72 GPa [7]
b 0.26 nm [10]
e 1 m [7]
Table 3.1.1.3: Values of physical parameters used in modelling

In addition to the above parameters the initial grain size of each TWIP grade is needed by the model.
From optical microscopy results for TWIP 2 and 3, the average austenite grain sizes have been
determined to be 32 and 25 m respectively. The initial dislocation density, for both TWIP grades, was
taken on reference [10] equal to 10
12
m
-2
.
A good agreement is obtained between model and experiment for both steel grades. The model fitting
parameters obtained for each grade are shown in table 3.1.1.4.


Steel grade
0
(MPa) k a M
TWIP 2 213 0.017 0.041 2.27
TWIP 3 235 0.009 0.040 2.06
Table 3.1.1.4: Obtained model fitting parameters

As can be seen from table 3.1.1.4, the fitted yield stress is similar for both TWIP grades. Table 3.1.1.4
also shows the contributions of dislocation-forest hardening, dynamic recovery and twinning, through



74

the parameters k, a and m respectively. As can be seen the dislocation forest hardening is significantly
larger for the TWIP 2 grade. Furthermore TWIP 2 displays a slightly larger m value. In general a
higher m (parameter related to SFE) value indicates a greater twin fraction for a particular strain. This
analysis allows to conclude that TWIP2 steel developes a slightly larger amount of deformation induced
twinning with respect to TWIP3.


Case 2: Strain hardening at elevated temperature



a) True stress-true strain curves for TWIP
3.
b) True stress-true strain curves for TWIP
4.
Fig. 3.1.1.4: True stress-true strain curves for TWIP3-4.


The interesting features of high temperature strain hardening behavior are:
The appearance of a sharp yield point and the presence of serrations. Figure 3.1.1.4 shows the
stress-strain behaviour of TWIP 3 and TWIP4 at 3 different temperatures. The occurrence of
serrations is related to dynamic strain ageing via carbon locking of dislocations. This
phenomenon is observed at room temperature but it is more pronounced at 250C and almost
absent at 350C. This result is consistent with reference [7] discussed above, where in Fe-
30Mn-1C alloy serrations were observed even at at room temperature.
The work hardening is more extensive at room temperature. This is a consequence of the fact
that the stacking fault energy increases with temperature. This leads in turn to a change in
deformation mechanism depending on the SFE value. As temperature increases the tendency
for twinning reduces and dislocation glide is preferred and became the main deformation
mechanism.


Conclusions task 3.1.1.1
All the TWIP steel grades investigated revealed excellent tensile properties. However significant
differences are present in terms of deformation mechanisms and microstructural evolution during
deformation. The tensile properties resulted to be quite sensitive to the specimen surface preparation but
the investigation of this phenomena is remainded in the task 3.1.1.3.
Temperature effect
The tensile properties of TWIP steel grades show a quite similar behaviour at increasing temperature
with only some quantitative differences. The yield stress is slightly affected by temperature while the
tensile strength is significantly influenced by temperature. This means that at higher temperature the
Rp
0.2
/UTS ratio tends to increase due to progressive change of the deformation mechanism
(twinningdislocation glide) and a consequent reduction of the strain hardening ability and elongation
is detected.
Strain rate effect



75

For equivalent plastic strain below 0.25, the behaviour of TWIP steels is very similar at room
temperature and the strain rate influence on the strength is very weak. Only at very high strain rates
( 200 >
&
s
-1
) there is a small strain rate induced increment of the flow stress.


Strain hardening ability
The main characteristic of a true TWIP steel (TWIP2 and TWIP3) is the presence of a intermediate
stage in the strain hardening curve the instantaneous coefficient n increase with strain. This should be
related to the effect of deformation induced twinning occurring after the first stage of the curve
predominated by dislocation glide. The new twins act as barriers to dislocation motion, and lead to an
increase in strain hardening rate. Depending on the extent of twinning, these leads to the observed
overall hardening rate.
The other TWIP grades (TWIP1,4,5) are characterised by a lower austenite stability and this is
demonstrated by the occurrence of martensite ( or ) during deformation or presence of ferrite also at
zero strain as for TWIP1.
The strain hardening of TWIP 1,4,5 grades shows a sligth different behaviour as a function of strain,
due to the complex combination of deformation mechanisms (twinning+dislocations) and deformation
induced phases (-martensite and -martensite).


Task 3.1.1.2 Characterization of austenite phase stability and microstructural evolution in TWIP
grades during deformation at different temperature
It is well understood that TWIP steel tensile properties are strictly related to SFE and therefore to
temperature. The present task was focused on the study of the deformation mechanisms and austenite
stability of TWIP variants in a broad range of temperature from -180C up to 350C.

Case 1: Room temperature microstructure evolution during straining
For each TWIP grade extra tensile tests were performed for true strains of 0.1, 0.2 and 0.4. Samples for
optical microscopy were then taken from each tensile specimen in both the head region (non-
deformed) and the centre region (deformed). The samples were cut and sectioned to view the
microstructure in the longitudinal direction i.e. parallel to the deformation axis. The microstructures
were revealed with two etching techniques. The first (etchant I) involved a pre-etch with 2 % nital
solution followed by etching with a solution of 20g sodium metabisulphite dissolved in 100ml of water.
This etchant revealed the grain contrast. The second (etchant II), involves etching in a solution of 50ml
saturated aqueous sodium thiosulphate and 5g of potassium metabisulphite. This reagent (also known as
Klemms II reagent), gives a colour etch, with austenite grains yellow to brown or light to dark blue,
whilst -martensite is shown as dark brown and finally -martensite is revealed as white [1]. Figures
3.1.1.5-3.1.1.8 shows a summary of the microstructures obtained. Note that for clarity only the
micrographs for 2 levels of strain are shown i.e. 0 (head region) and 0.4.
TWIP1 microstructure in undeformed state is constituted of austenite +ferrite (6%). The deformed
samples reveal flattened grains in which can be detected intersecting shear bands. In some regions dark
plate like structures are visible. From their colour (brown) these plate structures are suggested to be -
martensite.
From figure 3.1.1.5 a) TWIP 2 displays a equiaxed austenitic structure with a larger grain size
compared to TWIP 1. The microstructure appears to be completely austenitic. The deformed structure
(figure 3.1.1.5b) reveals intersecting shear bands in some grains.





76

a) b)
Fig. 3.1.1.5: TWIP 2 x500 a) head region etchant I, b) strain =0.4, etchant I.

The microstructure of TWIP 3 in the undeformed state is shown by figures 3.1.1.6 a). The structure is
completely austenitic with equiaxed grains showing some shear banding and annealing twins as for
TWIP 2 in the same condition. The grain size appears to be smaller than for TWIP 2. In the deformed
state figures 3.1.1.6b) shows intersecting shear bands, as for TWIP 2.

a) b)
Fig. 3.1.1.6: TWIP 3 x500 a) head region etchant I, b) strain =0.4, etchant I.


Figure 3.1.1.7 a) shows the TWIP4 structure constituted of equiaxed grain structure with some
annealing twins, as for the previous grades in the undeformed state. In addition the grain size appears to
be similar to that for TWIP 2. After a strain of 0.4 it can be seen from figure 3.1.1.7b) that most grains
contain shear bands which are mostly obscured by a darker constituent which seems to be present as
thin parallel plates in some grains. The brown plate like features are observed. From their colour this
constituent seems to be -martensite. This result is confirmed by ferritoscope measurements.




77

a) b)
Fig. 3.1.1.7: TWIP 4 x500 a) head region (strain=0) etchant I, b) strain =0.4 etchant II.


The undeformed microstructure of TWIP 5 is shown in figure 3.1.1.8 a). In the deformed state the
microstructure as revealed by figures 3.1.1.8 b) shows some intersecting shear bands. In addition as for
the deformed TWIP 1 and 4 grades, some brown plate like features are visible i.e. -martensite.



a) b)
Fig. 3.1.1.8: TWIP 5 x500 a) head region etchant I, b) strain =0.4 etchant II.


XRD analysis
X-ray Diffraction Analysis (XRD) was carried out on TWIP2, TWIP3, TWIP4, TWIP5, strip samples
before and after interrupted tensile test at 10%, 20% and 40% of elongation (always at 1/4 strip
thickness).
X-Ray diffraction experiments were performed with Mo-k

radiation, the volume fraction of phases


and constituents were quantified by the Rietveld method (spectrum fitting in the range 18-35 2).
From XRD diffraction spectra 4 constituents were identified with varying intensities: austenite, ferrite
(only for TWIP1), -martensite and -martensite.
10 m



78

Although the accuracy of the calculated volume fractions is low (high background noise level), the
results obtained can be used as an indication of the microstructural evolution during tensile straining,
and the differences in behaviour observed between the TWIP grades are expected to be still significant.
Figure 3.1.1.9 shows the results obtained.



A) B)

C) D)

E)
Fig.3.1.1.9: Calculated volume fractions of constituents in TWIP steels during tensile straining. A)
TWIP 1, B) TWIP 2, C) TWIP 3, D) TWIP 4 and E) TWIP 5.


From figure 3.1.1.9A it can be seen that for the TWIP 1 steel, a significant amount of epsilon martensite
forms during straining (compared to TWIP 2, 3 and 4). In addition the amount of alpha increases
significantly during straining i.e. strain-induced alpha martensite has formed in addition to the ferrite
content present at at zero strain.
Figures 3.1.1.9B and 3.1.1.9C (TWIP 2 and TWIP3) show similar behaviour i.e. very low levels of
epsilon martensite and alpha which remain approximately constant with increasing strain.
For TWIP 4, figure 3.1.1.9D shows that a negligible amount of epsilon martensite is formed during
straining, whilst the fraction of alpha i.e. alpha-martensite, increases with strain.
0
5
10
15
20
25
30
35
0 0.1 0.2 0.3 0.4
True strain
Fraction (%)
alpha
epsilon martensite
0
5
10
15
20
0 0.1 0.2 0.3 0.4
True strain
Fraction (%)
alpha
epsilon martensite
0
5
10
15
20
0 0.1 0.2 0.3 0.4
True strain
Fraction (%)
alpha
epsilon martensite
0
5
10
15
20
0 0.1 0.2 0.3 0.4
True strain
Fraction
(%)
alpha
epsilon martensite
0
5
10
15
20
0 0.1 0.2 0.3 0.4
True strain
Fraction (%)
alpha
epsilon martensite



79

Finally for TWIP 5, it can be seen from figure 3.1.1.9E that there is a low level of alpha that remains
approximately constant with increasing strain. On the other hand the fraction of epsilon martensite
appears to increase, before reaching a constant level at a strain of 0.2.

Discussion of results
TWIP 1 shows presence of both strain induced epsilon and alpha martensite. Since the fraction of
epsilon martensite increases continuously with strain, it is suggested that alpha martensite forms
directly from austenite i.e. different from the two-step transformation where epsilon martensite is the
intermediate phase. This direct transformation from austenite to alpha martensite has previously been
observed in another high manganese steel [1].

For TWIP grades 2 and 3, the X-Ray diffraction results suggest that the microstructure for both steels is
almost entirely austenite during straining. This is consistent with conclusion that both steels deform via
twinning.

For TWIP4 grade, the X-Ray diffraction results indicate that strain induced alpha martensite forms.
Since the fraction of epsilon martensite remains very low, the transformation proceeds directly from
austenite as for TWIP 1.

Finally for TWIP 5, a small amount of alpha phase is present during straining as indicated via X-Ray
diffraction. From the previous optical microscopy results this phase is suggested to be alpha-martensite.
Since the epsilon martensite fraction is shown to increase as strain proceeds (figure 3.1.1.9E), this
would indicate that the alpha martensite forms directly from austenite as for TWIP 1 and 4.
From the above results the microstructural evolution during room temperature deformation of these
steels can be summarised in the following table:


Steel composition Undeformed
microstructure
Deformed microstructure
(strain = 0.4)
Fe-21Mn-3Al-3Si
(TWIP 1)
. ferr
BCC FCC
+
Ms
HCP
Ms
BCC
ferr
BCC FCC
+ + +
.

Fe-22Mn-0.6C-0.2Si
(TWIP 2)
FCC

FCC

Fe-18Mn-0.6C-0.2Si-
0.02Nb (TWIP 3)
FCC

FCC

Fe-16Mn-1.5Al-0.2Si-0.3C
(TWIP 4)
FCC

Ms
BCC FCC
+
Fe-21Mn-0.2C-0.2Si-0.2N
(TWIP 5)
FCC

Ms
HCP
Ms
BCC FCC
+ +
Note that in above table Ms =martensite and ferr. =ferrite.
Table 3.1.1.5: Microstructural constituents/phases before and after testing of TWIP steels at room
temperature.


Case 2: Low temperature range (0-180C)
The characterization of the microstructure evolution during deformation at low temperature was carried
out on specimens deformed (strain =10% and 30%) at different temperature ranging between 0C down
to -180C. The microstructure was examined by means of selective color etching typically used for high
Mn steel (known as Klemms II). This reagent gives a color etch, with austenite grains yellow to brown
or light to dark blue, while -martensite is shown as dark brown and finally -martensite is revealed as
white.



80

The fraction of the ferro-magnetic
bcc
(bcc-martensite), as a function of the temperature, was measured
also by means of a ferritoscope. The results are shown in the following figure 3.1.1.10-11. On the basis
of the selective metallographic etching the fraction of hcp-martensite was measured by means of LOM
image analysis. The results of the measurements as a function of temperature are plotted in fig. 3.1.1.10.
As can be noted the second phases ( and ) produced during deformation are below 3% for all TWIP
variants. These circumstances together with low resolution related with deformed specimens does not
allow the use of XRD or EBSD techniques to evaluate quantitatively the phases formed after straining.



Fig. 3.1.1.10: Ferritoscope measurements of
bcc
martensite on strained TWIP steels samples
(deformation 10%).
Fig. 3.1.1.11: Ferritoscope measurements of
bcc
martensite on strained TWIP steels samples
(deformation 30%).


The results can be summarized as follows:

TWIP2: This variant revealed a quite stable austenitic structure in the range 20C -180C. In the
whole temperature range tested only very low magnetic phase ('-martensite) was detected. For what
concern the hcp-martensite low amount (2%) was detected only after high deformation (30%) in the
temperature range -150C-180C.

TWIP3: The behavior of this variant is quite similar to previous steel (TWIP2). TWIP3 steel revealed a
quite stable austenitic structure even at very low temperature. It is worthy to note that at a temperature
below -120C, increasing deformation from 10% to 30% the fraction of both '-martensite and hcp-
martensite phase increase even if the volume fraction remains quite low (<3%).

TWIP4: The behavior of the steel TWIP4 is quite different from the other TWIP steels. The austenite
phase of TWIP4 steel is markedly less stable even at room temperature due to higher formation rate of
-

martensite during deformation.
As can be noted from comparison of fig. 3.1.1.10-11, on decreasing the test temperature the fraction of
-martensite increases quickly while the fraction of -martensite decrease. This can be ascribed to
temperature dependence of SFE and hence at lower temperature (lower SFE) -martensite is favored.

TWIP5: in the temperature range 20C 0C the austenite phase is stable and only a low amount of
hcp-martensite can be detected (<1%) even after straining at 30% . Some presence of -martensite is
detected but the percentage remains very low even at the lowest temperature tested. At temperatures
below -50C the occurrence of hcp-martensite increases markedly with respect to the other TWIP
variants. Nevertheless even at the lowest temperature (-180C) the amount of second phase is below 5%
(after deformation at 30%).




81


Case 3: High temperature microstructure evolution during straining
(RT350C)
The study of deformation mechanisms operating during deformation at temperature in the range 250C-
350C was carried out by means of tensile specimens interrupted after a true strain =0.3 (strain rate
0.01 s
-1
).
In the fig. 3.1.1.12-15 are shown the microstructure of TWIP1,3,4,5 deformed at high temperature.



Fig. 3.1.1.12: TWIP1: deformed at 250C (strain 0.3 - strain rate =0.01 s
-1
).




a) 250C b) 350C
Fig.3.1.1.13: TWIP3: microstructure deformed at: a) 250C; and b) 350C (strain 0.3 - strain rate =
0.01 s
-1
).




82


a) 250C b) 350C
Fig.3.1.1.14: TWIP4: deformed structure at: a) 250C; b) 350C (strain 0.3 - strain rate =0.01s
-1
).




Fig. 3.1.1.15: TWIP5: deformed at 250C (strain 0.3 - strain rate =0.01 s
-1
).
The effect of temperature on deformation induced twins is quite evident. The results can be summarized
in the following table in terms of occurrence of deformation induced twins.




Table 3.1.1.6: Mechanical twins occurrence during deformation at high temperature (strain rate 0.01s
-1
).


Conclusions of task 3.1.1.2
The results of this task can be summarized in the following topics:



83

TWIP2 and TWIP3 are characterized by largest stability of austenite phase under deformation
from 250C down to -180C. Within this temperature range the deformation induced twinning
represent the main deformation mechanism. At temperature of 350C both steels do not reveal
deformation induced twinning.
TWIP1, TWIP4 and TWIP5 XRD pattern analysis revealed the occurrence during deformation
at room temperature in addition of deformation induced twinning (TWIP effect) even formation
of second martensitic phases ( and ). This tendency became stronger at low temperature due
to decrease of SFE. Since the fraction of epsilon martensite increases continuously with strain,
it is suggested that alpha martensite forms directly from austenite and not through the two-step
transformation where epsilon martensite is the intermediate phase. The occurrence of
deformation induced twinning disappears before 250C.


Task 3.1.1.3 Investigation on TWIP steel embrittlement
The activities carried out in this subtask are:

Metallographic examination of selected tensile specimens in order to characterize the strip
microstructure, presence of defects and analysis of surface oxidation and decarburization;
Low strain rate tensile tests on H-charged samples and internal hydrogen behavior and
consequences on TWIP tensile properties.


3.1.1.3.1 Metallographic examination of selected tensile specimens in order to characterize the
strip microstructure, surface decarburization and oxidation
The microstructure of tensile specimens revealing low tensile properties was fully characterized. In fig
3.1.1.3.1 a) is shown the cross section of a tensile specimen of TWIP3 steel. The annealing treatments
were carried out under N
2
fluxing (O
2
=4-5% and dew point 0C). As can be noted the strip surface
shows a lot of cracks with a penetration up to a depth of about 200 m. Fig 3.1.3.1.1b) shows a close up
of the microstructure in correspondence of the strip surface. As can be noted a huge presence of
martensite can be detected in the microstructure. This is also confirmed by magnetic behavior revealed
by means of a ferritoscope.

Fig. 3.1.1.3.1 a) Longitudinal cross section of a
TWIP3 tensile specimen close the fracture surface.
Fig.3.1.1.3.1b): Subsurface microstructure
after tensile test (TWIP3) Klem II etching.



3.1.1.3.2 Study of TWIP steels decarburization during high temperature annealing
The effect of surface decarburization on TWIP steel performances was studied through a series of
annealing tests reported in the table 3.1.1.3.1.



84


Samples Temperature Soaking time
TWIP 2,3,4,5 1000C, 1200C 300s, 1100s
C45 (reference) 1000C, 1200C 300s, 1100s
Table 3.1.1.3.1: Annealing tests carried out to study the strip surface decarburization.

The annealing treatments were carried out in a muffle furnace with air (dew point 10C) in order to
study the effect of decarburizing conditions on TWIP steel. A conventional C45 steel sample was used,
as a reference, to compare the decarburization behavior of TWIP (austenitic steel) at two high
temperatures (1000C and 1200C).
All the strip samples (hot rolled state) were mechanically polished (about 1mm was removed for each
surface) in order to remove completely the scale layer and also the previous decarburized layer. On
selected samples (TWIP2 and TWIP3) were carried out GDOES analysis in order to study
quantitatively the carbon and manganese concentration profiles. Micro-hardness profiles were carried
out on all samples in order to evaluate the evolution of the local tensile strength as a function of the
depth from the surface. A ferritoscope was used in order to detect the presence of martensite in the
microstructure close the strip surface. All the TWIP samples annealed at 1000C and 1200C revealed
in the subsurface zone a ferro-magnetic behavior. This confirms that the austenitic phase in the
decarburized zone is destabilized and the microstructure is a mixture of +' even without any
deformation. The presence of '-martensite is due to the local lowering of SFE in the C and Mn
depleted zone.
In the following fig. 3.1.1.3.2-3 are shown the microstructure of the TWIP2 samples after annealing
treatment at 1000 and 1200C. The effect of decarburization is quite clear and typically can be noted in
all TWIP samples two different zones moving from surface towards the bulk (different etching
behavior): the outer zone is characterized by higher amount of martensite (low C and Mn content).
Below, towards the bulk, the presence of martensite is lower (Mn approach bulk content) but the local
SFE value could be lower than bulk material and additional martensite can be formed during
deformation.


Fig. 3.1.1.3.2: TWIP2 microstructure after
annealing at 1000C x 300s.
Fig. 3.1.1.3.3: TWIP2 microstructure after
annealing at 1200C x 1100s.

As can be noted from the values reported in the table 3.1.1.3.2, for TWIP steels, the zone with mixed
microstructure reveals a quite high hardness with respect to bulk values. The huge difference in terms of
hardness between bulk and surface highlights also that the ductility of the subsurface zone is quite low.
On contrary it is worthy to note that, for conventional C45 steel, the decarburized zone is softer as
revealed by lower hardness with respect to bulk.




85

1000C 1200C
Bulk() subsurfacezone(+') Bulk() subsurfacezone(+')
TWIP2 178 265 189 320
TWIP3 181 300 187 330
TWIP4 190 240 210 260
TWIP5 182 274 180 292
C45 270 190 275 180
Table 3.1.1.3.2: Comparison of Vickers hardness (HV200g) average values on bulk and decarburized
zone.

In the following fig. 3.1.1.3.4 the depth of decarburized layer (measured as depth of subsurface zone
with microstructure (+) are plotted together with the Birks-J ackson model. As can be noted the
agreement is quite good considering the half of depth arising from model calculations. In the same
figure the decarburization behavior of TWIP steels is compared with the C45 medium carbon steel. As
can be noted, in the range of soaking time explored 300-1100s, the decarburization depth of TWIP
steels is larger than carbon steel. This difference could be originated by a different behavior of these
steels in the temperature range below 910C. In fact for the austenitic TWIP steels the carbon is in solid
solution and is ready to react with oxygen even at relatively lower temperatures. For a medium carbon
steel (C45) the amount of decarburization at lower temperatures (during heating) is low due to phase
transformation +pearlite . During this transient the formation of a ferrite layer (low C solubility) on
the strip surface could slow down the steel decarburization kinetics.



Fig. 3.1.1.3.4: Comparison of the decarburization depth of different TWIP steel variants (TWIP2,3,4,5)
and C45 steels at 1000C and 1200C.


3.1.1.3.3 Decarburized layer analysis by means of GDOES
In fig. 3.1.1.3.5 is shown the carbon and manganese concentration profiles on TWIP2,3,4 samples in the
annealed state. As can be noted the both C and Mn are depleted in the subsurface zone due to annealing



86

treatments. The depth of Mn depleted zone (<30m) is significantly lower than C decarburized layer.
The decarburized layer is quite independent from TWIP variant and is typically in the range 120-150m
for annealing at 1000C and 300-350m for annealing at 1200C.


TWIP 2: decarburization after annealing at 1200C x
300s.
TWIP 2: Mn concentration profile after annealing at
1200C x 300s.

TWIP3: decarburization after annealing at 1000Cx
300s.
TWIP3: Mn concentration profile after annealing at
1000C x 300s


TWIP4 - decarburization in the final state: (final
annealing at 1000Cx300s).
TWIP4 - Mn concentration profile in the final state
(annealing at 1000Cx300s).
Fig. 3.1.1.3.5: GDOES Carbon and manganese concentration profiles on TWIP2,3,4.





87



3.1.1.3.4 Study of the effect of hydrogen pre-charging on low strain rate tensile tests
The characterization of TWIP steels susceptibility to hydrogen embrittlement represent a huge work and
require a dedicated project of investigations and tests. Nevertheless, even if in the present project this
topic was not foreseen in the technical annex, selected tests were planned and carried out. In the
following the activities carried out are detailed:

1. Hydrogen charging of tensile specimens;
2. Low strain rate tensile tests on hydrogen charged TWIP specimens (charged at 900C) in
which the decarburized layer was mechanically removed.
3. Hydrogen thermal desorption analysis (TDA) was carried out in order to investigate on the
hydrogen trapping sites in TWIP steel in the temperature range 400-1100C.

Hydrogen charging of tensile specimens
Tensile specimens of TWIP3 steel were hydrogen charged at 900C using a suitable furnace working
under a pure hydrogen flux (10 l/h). After soaking the samples were quenched and the final hydrogen
content was evaluated and the results are reported in the following table 3.1.1.3.3.

Sample condition Hydrogen content (ppm)
Mechanically polished (reference) 1.3
Mechanically polished and
Hydrogen charged at 900C
4.5
Table 3.1.1.3.3: Hydrogen content of the reference and charged TWIP3 samples.



1. Tensile tests on hydrogen charged TWIP3 specimens
Tensile tests (strain rate=10
-2
s
-1
) on reference sample and hydrogen charged TWIP3 specimen, with the
decarburized layer mechanically removed, were carried out in order to evaluate the effect of high
hydrogen content on TWIP3 tensile properties (fig. 3.1.1.3.6).

Fig. 3.1.1.3.6: Tensile test curve of hydrogen charged TWIP3 sample.





88


Table 3.1.1.3.4: Tensile tests reference and hydrogen charged TWIP3 sample.


As can be noted (fig. 3.1.1.3.7) the tensile properties of hydrogen charged sample and reference blank
sample show similar tensile properties. The strip sample with the decarburized layer shows a
significantly lower elongation to rupture.



Fig. 3.1.1.3.7: Results of tensile tests carried out on sample with different hydrogen content.



3.1.1.3.5 Thermal desorption analysis (TDA) on TWIP steel
Hydrogen determination by LECO RC-412
Hydrogen content of metallic materials is measured at CSM by thermal desorption technique, using the
LECO RC-412 instrument.
Such instrument is basically made up by a resistance heated, temperature-controlled furnace, a thermal
conductivity detector and several filters to separate hydrogen from other emitted gases.
Instrument operation can be summarized as follows:
- Specimen heating in the furnace, under constant nitrogen flow;
- Hydrogen and other adsorbed gas (H
2
O, CO
2
, etc.) evolution;
- Emitted gas transport by nitrogen flow (carrier gas);
- Gas filtration to separate hydrogen from other emitted gases;
- Determination of metal hydrogen content by means of the thermal conductivity detector.
LECO RC-412 main features are presented in table:







89


Furnace temperature range 80 1200 C
Powder 0,25 grams
Sample size
Strip or tubular samples up to 25,4 mm x 101,6 mm
Analysis time 2400 seconds maximum
Heating rate 15 200 C/minute
Number of selectable phase steps 10
Maximum time for each phase 600 seconds
Accuracy 0,1 ppm
Instrument range 0,1 -1000 ppm
Table 3.1.1.3.5: LECO RC-412 main features.


The hydrogen determination is made setting the starting temperature to 400C (hold for 100 s), the
ending temperature to 1000C (hold for 300 s) using a heating rate of 120C/minute. This procedure
provides the operator with a graphic plot, hydrogen signal vs. analysis time. In this plot one or more
peaks will appear and their area can be related to metal hydrogen content. For example, analysing
austenitic steels or nickel super alloys three different peaks can be found, one at about 400 C, a second
between 500 - 600 C and a third above 800 C. The position and the height of each peak indicates
that the relative amount of hydrogen in each different trapping site is different.
According instrument features, a different procedure can be proposed in order to identify dominant
types of trapping sites and their relative hydrogen content. A proper sample preparation could, also,
permit an estimation of the amount of diffusible hydrogen.
A slow heating rate should be used (verified minimum rate 15C/minute) and the start temperature
should be set to about 100C (verified minimum temperature 80C), this type of analysis will show the
operator the differing types of hydrogen effusing the sample. The point is to design a temperature
profile based on slow rate, broad temperature range and on instrument time constraints. For example,
using a constant heating rate of 15 C/min, can be investigated just a 700C range, i.e. if the starting
temperature is set to 80C is not possible to overcome 700C in one sweep. Optimization of these
testing parameters would allow to understand different trapping site behaviour. To implement hydrogen
differentiation, the temperature profile is programmable into 10 different phase. The operator enters
start temperature, end temperature, heating rate, and amount of time to hold at the ending temperature
for each phase selected. The results of thermal desorption analysis (TDA) of blank sample and
hydrogen charged sample are shown in the following fig. 3.1.1.3.8. The characteristic main peaks,
partially overlapping, of the reference sample are located at 800C and 1000C. The hydrogen charged
sample is characterized by a main broad peak ranging between 800-1100C. These high de-sorption
temperatures indicate that the hydrogen is trapped into the metal structure by high energy bonding. The
temperature profile indicates, also, that the diffusible hydrogen is practically absent. Therefore, under
plastic deformation the hydrogen absorbed cannot move so easily to reach dislocation and/or crack tip,
creating favourable condition to fragile fracture. These observations are confirmed by the mechanical
testing results, where the specimen with about 5 ppm of hydrogen behaved in the same way of that
having 1 ppm. Therefore, the conclusion is that the hydrogen absorbed into the TWIP alloy did not
determined any embrittlement and/or loss in ductility.





90


Fig. 3.1.1.3.8: DTA plot on blank and hydrogen pre-charged sample.



Conclusions Task 3.1.1.3
The results achieved can be summarized in the following points:

1. The results of the investigations carried out in the present task 3.1.1.3 allow to argue that the
embrittlement problems of TWIP steels are mainly related to decarburization and Mn depletion
producing a mixed +microstructure in the subsurface zone.
2. Carbon and manganese concentration profiles on TWIP steels show that both C and Mn are
depleted in the subsurface zone due to annealing treatment under decarburizing atmosphere. It is
worthy to note that the depth of Mn depleted zone (typically <30m) is significantly lower than C
decarburized layer.
3. All the TWIP samples annealed at 1000C and 1200C reveal in the subsurface zone a mixed
microstructure +' even without any deformation with a resultant ferro-magnetic behavior. The
presence of '-martensite is due to the local lowering of SFE in the C and Mn depleted zone.
4. TWIP2,3,4,5 steels reveal a similar behavior that is in good agreement with the theory of
decarburization in austenitic phase (Birks-J ackson model) strictly related to bulk carbon diffusion.
The decarburization depth is more sensitive to annealing temperature (exponential dependence)
with respect to soaking time (t
1/2
dependence).
5. The decarburization depth of TWIP steels is larger than carbon steel probably because for austenitic
steels the carbon is in solid solution and is ready to react with oxygen. The kinetics of
decarburization of a medium carbon steel (C45) on relatively short time is decreased by phase
transformation +pearlite . During this transient the formation of a ferrite layer on the strip
surface could slow down the steel decarburization kinetics.
6. In terms of decarburization the final annealing process (after cold rolling) could be critical. For this
treatment a controlled annealing furnace atmosphere has to be considered in order to avoid the
occurrence of decarburization and so the formation in the subsurface zone of a mixed +
microstructure.
7. Tensile tests (=10
-2
s
-1
) carried out on sample with different hydrogen contents shown similar
tensile properties. The elongation to rupture of hydrogen charged specimen is markedly higher than
the strip sample with a surface decarburized layer.
8. The high desorption temperatures indicate that the hydrogen is trapped into the metal structure by
high energy bonding. This result would suggest that the diffusible hydrogen can be considered
negligible. Therefore, under plastic deformation the hydrogen absorbed cannot move so easily to
reach dislocation and/or crack tip, creating favourable condition to fragile fracture.



91


Task 3.1.2 Dynamic Tensile Properties
High strain rate deformation of TWIP steels were carried out on cold rolled sheets of high-Mn TWIP
steels with 1.5-2 mm thickness using a tensile split-Hopkinson bar method.
Dynamic tensile testing of sheet steels is becoming more important due to the need for more optimized
vehicle crashworthiness analysis in the automotive industry. The deformation characteristics of sheet
steels can be measured precisely to an order of 1000 s
-1
. Positive strain rate sensitivity, i.e. the strength
increases with strain rate, offers a potential for improved energy absorption during a crash event.
Specimens of varying thickness 1.5 <t <2 mm were cut longitudinally to the rolling direction of the
annealed strips. All tests were carried out at room temperature with two different strain rates 855 and
1250 s
-1
.

Results and Discussion
In the fig. 3.1.2.1a) the quasi-static tensile properties of TWIP1-5 grades are compared with the typical
tensile properties of TRIP700, DP600, H340LAD.
Dynamic tensile mechanical properties, shown in Fig. 3.1.2.1b), showed raising yield strength for all
steels, for instance for TWIP2, R
p0.2
increased from 250 MPa for quasi-static to 560 MPa at high strain
rates. This positive strain rate sensitivity revealed by TWIP is also detected in other steels nevertheless
must be stressed that the elongation of TWIP steels is still much higher than those of the other three
automotive steels (TRIP, DP600 and H340LAD).
Fig. 3.1.2.2 shows the ratio of the yield stress to the tensile strength in quasi-static and dynamic tensile
tests for TWIP steels and the automotive steels. In addition, the plot includes strain hardening
coefficient n-value for full curve in dynamic tensile tests.




Fig. 3.1.2.1 a): Comparison between the quasi-static
mechanical properties, yield strength R
p0.2
, tensile
strength R
m
, and fracture elongation A of the present
TWIP steels [15] and those of TRIP700, DP600 and
H340LAD [17] at RT (the strain rate 10
-3
s
-1
).

Fig. 3.1.2.1 b): Comparison between the
dynamic mechanical properties, yield strength
R
p0.2
, tensile strength R
m
, and fracture
elongation A of the present TWIP steels and
those of TRIP700, DP600 and H340LAD [17] at
RT (the strain rate of order of 10
3
s
-1
).






92


Fig. 3.1.2.2: Comparison between the stress ratio in quasi-static and dynamic tensile tests of the present
TWIP steels and those of TRIP700, DP600 and H340LAD [17].


In the following sections the details of the behaviour of each TWIP variant are reported.

TWIP2 (reference steel)
The strain rate dependence of the stress-strain behaviour at 870 s
-1
and 1210 s
-1
appears similar. The
yield strengths at dynamic strain rates are almost identical 550 and 562 MPa, respectively. However,
the yield strength of that steel under quasi-static tensile tests at RT is much lower (273-280
MPa).TWIP2 steel exhibited higher uniform elongation (68%) than the other steels in SHB tests. These
results are consistent with the results obtained under quasi-static tensile tests, while TWIP2 showed
highest elongation to rupture (A =80%). Fig. 3.1.2.3 shows the work hardening coefficient (n-values)
of TWIP2 as tested at 1210 s
-1
. It can be seen that the n-value increases continuously with increasing
strain and reaches maximum values about 0.6 at the uniform elongation.


Fig. 3.1.2.3: Strain-hardening coefficient (n-value) from the Hollomon equation vs. True
plastic strain for TWIP2 tested at 1210 s
-1
and RT.



93


The fracture surface of TWIP2 after SHB test at 1210 s
-1
was examined using SEM. The fracture
surface shows a clear ductile morphology.

TWIP1
The dynamic tensile true stress-true strain curves at 855 s
-1
and 1250 s
-1
reveal that the strain rate has
small effect on the dynamic flow curves. The yield strengths are 504 MPa and 575 MPa at 855 s
-1
and
1250 s
-1
, respectively. However, the yield strength of that steel under quasi-static tensile tests at RT is
much lower (245-260 MPa).
For both dynamic and quasi-static tensile tests, it is observed that after yielding, the flow stress
increases gradually with further straining and it reaches almost the same ultimate (engineering) tensile
strength of 780 MPa and uniform elongation (48-50%). Thus the tensile strength and failure strains are
independent of strain rate.
The n-values (strain hardening coefficients) of TWIP1 while tested at the highest strain rate of 1250 s
-1

increases continuously with increasing strain and reaches the maximum value higher than 0.45 at true
strain of 0.4.

TWIP3
Dynamic tensile flow curves of TWIP3 at two strain rates show similar behaviour with small effect of
the strain rate. For example, yield strengths are 480 and 510 MPa and ultimate tensile strengths are 835
and 900 MPa at 830 and 1280 s
-1
, respectively. However, the yield strength and tensile strength of that
steel are 280 and 850 MPa, respectively, under quasi-static tensile tests at RT.
The work hardening coefficient, n-values, of TWIP3 tested at 1280 s
-1
shows that the steel exhibits a
similar behaviour for the other investigated steels. While strain hardening increases with strain and
reaches maximum n-value 0.55 at high uniform elongation.

TWIP4
TWIP4 exhibited the lower yield strength (420 MPa) than TWIP2 and TWIP3 steels. This behaviour
was similar also on quasi-static tensile tests with a yield strength of 240 MPa. It can be attributed to its
lowest Mn content.
Microstructure examination of TWIP4 after dynamic tensile tests at 1260 s
-1
displays highly distorted
grains with very high density of mechanical twins.
The work hardening coefficient of TWIP4 tested at 1260 s
-1
shows that the steel exhibits a similar
behaviour as for the other investigated steels. The strain hardening increases with strain and reaches the
same maximum n-value of 0.55 as in the case of TWIP3.

TWIP5
The steel exhibited high dynamic tensile mechanical properties with yield strength 510 MPa and high
uniform elongation 52%.

Conclusion of task 3.1.2
The stress ratios (the yield stress to the tensile strength) of TWIP steels are much lower than those of
the automotive steels under quasi-static conditions. This means TWIP steels promoted higher strain
hardening potential. Under dynamic tensile conditions, stress ratios of TWIP steels increased as a result
of increasing yield strength, but they are still lower than those of the three automotive steels.
Furthermore, the n-values of TWIP steels from dynamic tensile tests are much higher than those of the
automotive steels.
The enhancing of the ductility, strength and strain hardening of material is advantageous for crash
energy absorbing characteristics.



94

TWIP steels promoted higher ductility and higher strain hardening with high strength, and therefore
TWIP steels have higher crash energy absorption and consequently higher crash safety than steels
TRIP700, DP600 and H340LAD.


Task 3.1.3. Torsion tests in the 20C-450C temperature range: stress-strain behaviour at large
strains
The behaviour of four TWIP steels (TWIP steels 2, 3, 4 and 5) up to large plastic strains has been
studied by performing torsion tests at five temperatures in the 20C-450C range and at three tensile
equivalent strain rates ranging from 1.410
-3
s
-1
to 3.73 s
-1
. The stress-strain curves were calculated from
the torque-twist curves using the method of Fields and Backofen. The initial structure was the structure
after hot rolling. Figures 3.1.3.1 to 5 present the torsion shear stress vs. plastic shear strain curves for
the four steels. As no extensometer was used in the torsion tests, the small strain range of the results
(e.g., the yield stress) is not reliable.
The results show a strong temperature effect in the strength level and an important effect of strain rate
in the ductility. Also, the apparent strain rate effect has a superposed adiabatic heating effect at the two
highest strain rates used. The trend of the behaviour is common for the four steels, although TWIP3 is
clearly more ductile than the other three compositions. A change in the behaviour from cold-work to
warm/hot-work occurs at about 250C. At the highest strain rate and at low temperature, the initial
strain hardening rate is much higher than its static counterpart, a fact that could be linked to an
enhancement of the twinning activity at high strain rates. However, only TWIP2 and TWIP3 below
250C clearly behave as expected from TWIP steels, with the typical hardening stage associated to
profuse deformation twinning. In all other cases the work hardening is an approximately linearly
decreasing function of the flow stress soon after the yield stress, a behaviour characteristic of
dislocation-mediated plasticity controlled by dynamic recovery. At the higher temperatures and smaller
strain rates tested, the stress-strain curves show a maximum (and even oscillations) that could be due to
dynamic recrystallization, but the confirmation or rejection of this question by microstructural study is
still pending. At room temperature, the strain rate dependence observed in torsion agrees very well with
the equivalent values obtained in tension up to high strain rates.
In fig. 3.1.3.6 the maximum shear stress in torsion as a function of temperature for different strain rates
are shown. In fig. 3.1.3.7 the torsion shear failure strain of the four TWIP steels are shown as a function
of temperature and strain rate.






















95


0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT (1) RT (2) 150C (1) 150C (2)
250C 350C 450C
(a)
TWIP 2

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT 150C 250C 350C 450C
TWIP 3
(b)

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT 150C 250C 350C 450C
TWIP 4
(c)

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT 150C 250C 350C 450C
TWIP 5
(d)

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT (1) RT (2)
150C (1) 150C (2)
250C 350C
450C
(a)
TWIP 2

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(b)
TWIP 3

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
TWIP 4
(c)

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
TWIP 5
(d)
Fig. 3.1.3.1: Torsion shear stress-plastic shear strain curves at = 1.410
-3
s
-1
and corresponding
Kocks-Mecking plots (strain rate vs. flow stress).







96


0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT (1)
RT (2)
150C
250C
350C
450C
TWIP 2
(a)

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(b)
TWIP 3

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(c)
TWIP 4

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(d)
TWIP 5

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT (1) RT (2)
150C 250C
350C 450C
TWIP 2
(a)

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(b)
TWIP 3

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(c)
TWIP 4

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(d)
TWIP 5
Fig. 3.1.3.2: Torsion shear stress-plastic shear strain curves at = 0.113 s
-1
and corresponding Kocks-
Mecking plots (strain rate vs. flow stress).






97


0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(a)
TWIP 2

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(b)
TWIP 3


0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(c)
TWIP 4

0
200
400
600
800
1000
0 1 2 3 4 5 6 7 8


(
M
P
a
)
RT
150C
250C
350C
450C
(d)
TWIP 5
0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(a)
TWIP 2

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(b)
TWIP 3


0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(c)
TWIP 4

0
400
800
1200
1600
2000
100 300 500 700 900
(MPa)
d

/
d

p

(
M
P
a
)
RT 150C
250C 350C
450C
(d)
TWIP 5
Fig. 3.1.3.3: Torsion shear stress-plastic shear strain curves at = 3.73 s
-1
and corresponding Kocks-
Mecking plots (strain rate vs. flow stress).




98

0
200
400
600
800
1000
0 100 200 300 400 500
T (C)


(
M
P
a
)

6.5 s
-1
1.2 s
-1
0.0024 s
-1

0.520

0.173
TWIP2

1.040
(a)

0
200
400
600
800
1000
0 100 200 300 400 500
T (C)


(
M
P
a
)

(b)
6.5 s
-1
1.2 s
-1
0.0024 s
-1

0.520

0.173
TWIP3

1.040




Fig. 3.1.3.4: Torsion shear stress for three shear strain levels, 0.173, 0.520 and 1.040, as a function of
temperature, for the three strain rates tested (TWIP2, TWIP3).



99

0
200
400
600
800
1000
0 100 200 300 400 500
T (C)


(
M
P
a
)

(c)
6.5 s
-1
1.2 s
-1
0.0024 s
-1

0.520

0.173
TWIP4

1.040

0
200
400
600
800
1000
0 100 200 300 400 500
T (C)


(
M
P
a
)

(d)
6.5 s
-1
1.2 s
-1
0.0024 s
-1

0.520

0.173
TWIP5

1.040

Fig. 3.1.3.5. Torsion shear stress for three shear strain levels, 0.173, 0.520 and 1.040, as a function of
temperature, for the three strain rates tested (TWIP4, TWIP5).















100

TWIP 2
0
200
400
600
800
1000
1200
0 100 200 300 400 500
T (C)

M

(
M
P
a
)
0.0024 s-1
0.196 s-1
6.46 s-1
(a)

TWIP 3
0
200
400
600
800
1000
1200
0 100 200 300 400 500
T (C)

M

(
M
P
a
)
0.0024 s-1
0.196 s-1
6.46 s-1
(b)
TWIP 4
0
200
400
600
800
1000
1200
0 100 200 300 400 500
T (C)

M

(
M
P
a
)
0.0024 s-1
0.196 s-1
6.46 s-1
(c)
TWIP 5
0
200
400
600
800
1000
1200
0 100 200 300 400 500
T (C)

M

(
M
P
a
)
0.0024 s-1
0.196 s-1
6.46 s-1
(d)
Fig. 3.1.3.6: TWIP steels, maximum shear stress in torsion as a function of temperature for different
strain rates.

TWIP 2
0
1
2
3
4
5
6
7
8
0 100 200 300 400 500
T (C)

F

0.0024 s-1
0.196 s-1
6.46 s-1
(a)

TWIP 3
0
1
2
3
4
5
6
7
8
0 100 200 300 400 500
T (C)

F

0.0024 s-1
0.196 s-1
6.46 s-1
(b)

TWIP 4
0
1
2
3
4
5
6
7
8
0 100 200 300 400 500
T (C)

F
0.0024 s-1
0.196 s-1
6.46 s-1
(c)

TWIP 5
0
1
2
3
4
5
6
7
8
0 100 200 300 400 500
T (C)

F

0.0024 s-1
0.196 s-1
6.46 s-1
(d)

Fig. 3.1.3.7: Torsion shear failure strain of the four TWIP steels as a function of temperature and strain
rate.



101


Conclusion Task 3.1.3
The hot torsion results show a strong temperature effect in the strength level and an important effect of
strain rate in the ductility. The trend of the behaviour is common for the four steels, although TWIP3 is
clearly more ductile than the other three compositions. A change in the behaviour from cold-work to
warm/hot-work occurs at about 250C. At the highest strain rate and at low temperature, the initial
strain hardening rate is much higher than its static counterpart, a fact that could be linked to an
enhancement of the twinning activity at high strain rates. However, only TWIP2 and TWIP3 below
250C clearly behave as expected from TWIP steels, with the typical hardening stage associated to
profuse deformation twinning. In all other cases the work hardening is an approximately linearly
decreasing function of the flow stress soon after the yield stress, a behaviour characteristic of
dislocation-mediated plasticity controlled by dynamic recovery.


Task 3.1.4 Hot ductility curves in the temperature range 700 1300 C by means of a Gleeble
simulator

Experimental
Hot ductility of TWIP steels was carried out at a constant strain rate 1 s
-1
on a Gleeble 1500 thermo-
mechanical simulator. The diameter of tensile rod was 7 mm and the length 120 mm. In the middle
there is a thinned gauge length zone with 8 mm in length and 6 mm in diameter.
In hot ductility tests, specimens were reheated in vacuum at the rate of 20C/s to 1150C-1250C for 2
min, to dissolve any precipitates present, and then cooled to the test temperature (between 700 and
1100C) at the cooling rate of 5C/s. After 30 s of soaking at the test temperature, long enough to
stabilize the temperature field, the specimens were tensile strained until fracture at the constant true
strain rate of 1 s
1
. At the testing temperatures higher than the reheating temperatures, the specimens
were heated directly to the test temperature and held for 60 s before tensile straining.


Results and Discussion

TWIP1 (Fe-22Mn-3Al-3Si)

The dependence of the reduction of area (RA) on the deformation temperature, i.e. a hot ductility curve
for TWIP_1 is shown in Fig. 3.1.4.1.


Fig. 3.1.4.1: Hot ductility curve for TWIP_1 (Fe-22Mn-3Al-3Si).




102



In the temperatures range 700-900C, RA increases with decreasing temperature and the ductility has
the lowest value of 28% at 900C. In the temperature range 1000-1100C, the RA increases with
increasing temperature and it shows the highest RA of 80% at 1100C. In the temperature range 1200-
1300C, the ductility decreases with increasing temperature and reaches zero at 1300C.


TWIP2 (Fe-22Mn-0.6C)
The effect of deformation temperature on tensile behaviour of TWIP_2 is displayed that the strength
decreases as temperature increases. However, tensile elongation to fracture decreases as temperature
increases up to 900C. Further increase in temperature results in increased elongation up to 1200C.
Hot ductility curve of TWIP_2 is shown in Fig. 3.1.4.2. In addition to the influence of deformation
temperature, the effect of reheating temperature on the hot ductility was investigated. In most tests, the
reheating temperature of 1250C/2 min was used, but in addition two tests were carried out with the
reheating temperature of 1150C/2 min. Hot ductility curve for Type 304 austenitic stainless steel has
been taken from Ref. [5] and included in Fig. 3.1.4.2 for comparison.


Fig. 3.1.4.2: Hot ductility curve of TWIP-2. Curve of AISI 304 is included for comparison.


Hot ductility curve of TWIP2 shows slight decrease of RA from 68% to 60% with increasing
temperature from 700 to 900C. This is similarly as the case for TWIP1 and is typical to the existence
of ductility trough for C-Mn and microalloyed steels [6,7]. However, the minimum RA is quite high,
about double compared to that of TWIP1, indicating excellent ductility even at 900C. Further increase
in temperature results in improvement of RA to 87% at 1200C. At 1300C, ductility decreased to the
lowest value 44% in hot ductility curve. The differential thermal analysis of TWIP2 exhibits that the
solidus temperature lies between 1320C and 1340C and the melting point is 1378C. Thus the
occurrence of local melting leads to decrease in hot ductility at 1300C.
As seen from the hot ductility curves in Fig. 3.1.4.2, the TWIP2 steel has even better ductility than that
of the austenitic AISI 304. It can be attributed to more delayed dynamic recrystallization of AISI 304,
occurring at higher temperatures than that of high-Mn TWIP steels [9].

TWIP3 (Fe-18Mn-0.6C-0.02Nb)



103

Hot ductility curve of TWIP_3 is shown in fig. 3.1.4.3. All hot ductility tests were carried out with the
reheating temperature of 1150C for 2 min. For comparison hot ductility curve of TWIP2 is included in
the same plot. However, hot ductility tests of TWIP2 have been carried out with reheating temperature
1250C for 2 min. The former RH provided austenitic structure with about 80 m grain size and the
latter 120 m.
It can be observed that both steels show similar behaviour with shifting curve of TWIP3 to higher RA
values. TWIP3 displayed its highest RA value (98%) at 1100C, while TWIP2 showed its highest RA
value (87%) at 1200C. It seems that finer grain size of TWIP3 promoted excellent hot ductility by
enhancing dynamic recrystallization isolating micro-voids and consequently hindering the micro-voids
coalescence and propagation.




Fig. 3.1.4.3: Hot ductility curve of TWIP3. Curve of TWIP2 is included for comparison.


TWIP4 (Fe-16Mn-1.5Al-0.3C)
The hot ductility curve for TWIP4 is shown in fig. 3.1.4.4. For comparison, the hot ductility curve of
TWIP2 is included. It is seen that both steels have almost same RA values up to 1000C, regardless
slightly lower ductility of TWIP4 at 800C. Above 1000C, TWIP4 exhibits excellent hot ductility up
to 1300C, with better values than those of TWIP2.




104


Fig. 3.1.4.4: Hot ductility curve of TWIP4. Curve of TWIP2 is included for comparison.


TWIP5 (Fe-22Mn-0.2C-0.2N)
The hot ductility curves of TWIP5 and TWIP2 are shown in fig. 3.1.4.5. It can be seen that hot ductility
behaviour of both steels is almost identical with minor differences in RA values. In TWIP5, RA
decreases from 64% to 60% with increasing temperature from 700C to 900C, respectively. However,
with further increasing temperature, hot ductility increases to the maximum value (95%) at 1200C. At
1300C, hot ductility has dropped to the minimum value 52%. In comparison with TWIP2, the hot
ductility value of TWIP5 is slightly higher (RA =95%) than that of TWIP2 (RA =87%) at 1200C.
This may be attributed to the strengthening effect of nitrogen alloying.
The influence of reheating temperature in TWIP5 is identical to that in TWIP2. With decreasing
reheating temperature from 1250C to 1150C, the hot ductility increased from 82% to 98% at 1100C.



Fig. 3.1.4.5: Hot ductility curve of TWIP5. Curve of TWIP2 is included for comparison.



105

Conclusions Task 3.1.4
The hot ductility curves of the TWIP steel variants show quite good high temperature performances.
The hot ductility in some cases, such as for TWIP 3 and TWIP2 (RA>60% between 700-1200C), is
higher than that of the austenitic AISI 304.


Task 3.1.5. Study of the influence of grain size in the tensile stress-strain behaviour of TWIP
steels (Hall-Petch behaviour)
The influence of grain size in the room-temperature tensile stress-strain behaviour of TWIP steels,
TWIP1 and TWIP2 has been studied for two of the chemical compositions of the project at a strain rate
of 10
-3
s
-1
. TWIP1 is a 22% Mn, 3% Al, 3% Si, 0.01% C steel with a Duplex structure (less than 10% of
ferritic phase). Its austenite partially transforms to -martensite upon plastic deformation (instead of
deforming by twinning), because of its very low SFE. TWIP2 is a fully austenitic steel of composition
22% Mn, 0.06% C, that twins upon deformation. A Hall-Petch relationship has been found for the yield
and flow stresses of both steels, with almost the same Hall-Petch slopes.
The influence of strain rate on the Hall-Petch behaviour has been studied for steel TWIP2 by
performing room temperature tensile tests at three strain rates, 10
-3
s
-1
,

9.4 s
-1
and265 s
-1
.
The yield stress or the flow stresses for a fixed tensile plastic strain obey Hall-Petch relationships.
Surprisingly, the slopes are almost the same for both steels despite the strain-induced transformation
occurring in TWIP1 steel or the twinning occurring in TWIP2 steel, as figure 3.1.5.1 shows for the yield
stress. For true plastic strains <0.005 the lamellae are practically absent from both steels, i.e., the
yield stress should correspond to slip by dislocation glide.



y = 356.53x + 157.16
R
2
= 0.992
y = 320.16x + 176.82
R
2
= 0.9967
0
100
200
300
400
500
600
700
800
900
1000
0 0.2 0.4 0.6 0.8 1 1.2 1.4
[D (m)]
-0.5

y

(
M
P
a
)
TWIP 1
TWIP 2
(a)
10
-3
s
-1
y = 356.53x + 157.16
R
2
= 0.992
y = 320.16x + 176.82
R
2
= 0.9967
0
100
200
300
400
500
600
700
800
900
1000
0 0.2 0.4 0.6 0.8 1 1.2 1.4
[D (m)]
-0.5

y

(
M
P
a
)
TWIP 1
TWIP 2
(a)
10
-3
s
-1

Fig. 3.1.5.1: Hall-Petch plot of the tensile yield stress at 10
-3
s
-1
(flow stress for 0.002 tensile plastic
strain) of steel TWIP1 and TWIP2.










106


0
100
200
300
400
500
600
0 0.03 0.06 0.09 0.12 0.15 0.1

p
K
H
P

(
M
P
a

m
1
/
2
)
TWIP 1
TWIP 2
10
-3
s
-1
K
HP
(b)

0
100
200
300
400
500
600
0 0.03 0.06 0.09 0.12 0.15 0.1

p
K
H
P

(
M
P
a

m
1
/
2
)
TWIP 1
TWIP 2
10
-3
s
-1
K
HP
(b)

0
100
200
300
400
500
600
700
0 0.1 0.2 0.3 0.4 0.5 0

p
K
H
P

(
M
P
a

m
1
/
2
)
0.001 s-1
9.4 s-1
265 s-1
Fig. 3.1.5.2: Hall-Petch slopes for the flow stress
at fixed true plastic tensile strain values, steels
TWIP1 and TWIP2 as a function of plastic true
tensile strain, up to =0.15.
Fig. 3.1.5.3: Hall-Petch slopes of steel TWIP2 at
room temperature and three tensile strain rates, as
a function of tensile plastic strain.


The influence of strain and strain rate on the Hall-Petch slopes is presented in figure 3.1.5.2-3. The
great similitude of the Hall-Petch slopes of the two steels is evident. The Hall-Petch slope increases as
strain increases, although the strain hardening of TWIP2 is larger than the hardening of TWIP1. The
change observed is compatible with an effect of increasing heating of the samples during the tests at
high strain rates. Such change is better seen in figure 3.1.5.3, showing the Hall-Petch slopes as a
function of strain and strain rate. Numerical data corresponding to the tensile tests of TWIP2 are
gathered in table 3.1.5.



d/dt [s
-1
]
D (m)
y
(Pa)
u
(Pa)
u

0.1
(MPa) A%
1.5 445 1624 0.42 3327 50
1.5 456 1586 0.37 3324 50.8
6.2 303 1481 0.44 2727 56.66
6.2 311 1377 0.38 2745 46.83
12.2 260 1502 0.52 2400 73.3
12.2 254 1409 0.46 2394 66.7
19 250 1431 0.5 2340 69.2
19 225 1379 0.49 2368 66
40.7 213 1234 0.42 2732 56.6
40.7 209 1170 0.4 2651 52.66
1.5 407 1189 0.29 2757 40.3
1.5 407 1145 0.26 2760 35.33
12.2 325 1032 0.31 2467 47.5
40.7 270 1021 0.39 2198 52.5
40.7 260 979 0.36 2337 51.66
1.5 530 1234 0.27 2413 45.2
12.2 365 1148 0.32 2555 53.33
12.2 356 1120 0.32 2703 56.66
40.7 300 1076 0.37 2078 62.5
9.4 s
-1
265 s
-1
10
-3
s
-1

Table 3.1.5: TWIP2, numerical results of tensile tests. The columns are: strain rate, grain size, yield
stress, flow stress for maximum uniform strain, maximum uniform plastic strain, strain hardening rate at
a strain of 0.1 and area total elongation.


Influence of grain size on work hardening rate and ductility.
For the TWIP steels the transition from the elastic domain to the near-linear plastic behaviour occurs
very abruptly. The initial branch of the curves where the hardening rate decreases rapidly and makes a



107

knee is not a stage III (as it has been often quoted in the literature for twinning-deforming materials)
but, merely the elasto-plastic transition in the polycrystal.
The linear stage occupies almost all the uniform strain of the room temperature tensile tests and there is
some influence of the grain size on its slope (fig. 3.1.5.4), being larger for smaller grain sizes. The slope
ranges from 2250 MPa to 3200 MPa. After about 30% plastic elongation the hardening rate decreases,
an indication that dynamic recovery is taking increasing importance and, consequently, an indication
that the predominance of the twinning deformation that induces the dynamic Hall-Petch effect
responsible of the TWIP initial linear stage is becoming less important.

1000
1500
2000
2500
3000
3500
4000
200 400 600 800 1000 1200 1400 1600
(MPa)
d

/
d


(
M
P
a
)
12.2 m
40.7 m
1.5 m
19 m
6.2 m

Fig. 3.1.5.4: Work hardening rate vs. true flow stress of the TWIP 2 steel with composition 22% Mn-
0.6% C. Tensile tests at room temperature and 10
-3
s
-1
for a equiaxed grain size in the range 1.5 m <D
<50 m.


Annealing treatments. Grain growth kinetics
Grain growth kinetics equation
For studying the grain size dependence, the range of thermal treatments has been expanded with respect
to the range covered for studying the annealing kinetics. The new results have allowed for a better
description of the grain growth kinetics of the steel. The annealing treatments have covered a wide
range from 10 min at 700C to 12.5 h at 1100C, all of them implying some grain growth after complete
recrystallyzation of cold rolled structures (recrystallization is complete after 9 min at 700C). All the
data are plotted in figs. 3.1.5.5a and 3.1.5.5b assuming an apparent activation energy of 363 kJ mol
-1
. A
reasonable fitting valid for the range covered by the experimental measurements (1.5 m <D <50 m)
is obtained:
( ) ( )
( )


=
RT
mol kJ
s t D
/ 363
exp 10 2516 . 2 m
16 8894 . 3





108

y = 3.5407x - 38.315
R
2
= 0.8867
-40
-35
-30
-25
-20
0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5
ln (D*)
l
n
[
e
x
p
(
-
Q
g
g
/
R
T
)
t
]
y = 3,8894x - 37,653
R
2
= 0,9023
-40
-35
-30
-25
-20
0 0,5 1 1,5 2 2,5 3 3,5 4 4,5 5
ln D
l
n
[
e
x
p
(
-
Q
G
G
/
R
T
)

t
]
Fig. 3.1.5.5a: D
*
grain size (mean linear intercept)
without considering twin boundaries, after annealing
time t (s) .
Fig. 3.1.5.5b: D id., with twin boundaries counted
as grain boundaries.



Grain boundary analysis of annealed samples (EBSP-OIM)
The new data available the twin boundary fraction of high angle boundaries can be added to the graph
of twin boundary fraction vs. grain size, fig. 3.1.5.6. After an initial very rapid growth, the twin
boundary fraction increases slowly as the grain size increases above 10m.

Twin Boundary Fraction vs Grain Size D* (twin boundaries not counted)
0
0,05
0,1
0,15
0,2
0,25
0,3
0,35
0,4
0,45
0,00 10,00 20,00 30,00 40,00 50,00 60,00 70,00 80,00
Grain size D* (m)
T
w
i
n

b
o
u
n
d
a
r
y

f
r
a
c
t
i
o
n

Fig. 3.1.5.6: Twin Boundary Fraction vs. Grain size D
*
(twin boundaries not counted).

Conclusions of task 3.1.5
The yield stress for 0.2% plastic elongation clearly shows a grain size dependence. The Hall-Petch
constants found for TWIP2 steel grade is =
HP
K 356.5 MPa m
1/2
.
The results of this task allowed to achieve a better description of the grain growth kinetics of the
TWIP2 steel. It is worthy to note that for fine grain size (<10m) the twin boundary fraction is



109

significantly lower than for larger grain size. This means that the TWIP effect is dependent on grain
size and the best performances are relevant to a grain size in the range 15-30m.
Task 3.2 Bending fatigue tests to determine the fatigue strength and cyclic softening/hardening
behaviour and to analyse the crack initiation/propagation stages

Experimental
Cold rolled samples were annealed at different conditions to produce specimens with different grain
sizes respectively of 4.5 m, 13 m, 32 m and 55 m.
Fatigue tests were carried out at room temperature under normal atmospheric condition using a Schenk
flexural bending fatigue machine driven at a frequency of 23 Hz with a zero mean stress. The standard
hourglass-shape of flat fatigue specimens with a thickness of 2 mm were used in all tests.
In order to verify the properties of the surface features of the fatigued steels, cyclic damage and crack
formation were examined using three techniques: an optical microscope and a field emission gun
scanning electron microscope FEG-SEM (Carl Zeiss Ultra plus) applying either a electron channeling
contrast (SEM-ECC) imaging or SEM-EBSD.

Results
Fig. 3.2.1 shows the experimental fatigue data in the form of stress amplitude - number of cycles to
failure plot (S-N curve). From the data, the fatigue limit of all investigated TWIP steels, corresponding
no failure in 2*10
6
cycles, is about 400 MPa. For comparison, the S-N curves of two commercial
austenitic stainless steels, Type 301LN and 316L, taken from Ref. [1] and a high-strength (Rm =821
MPa) TRIP steel, taken from Ref. [2], are also inserted. The fatigue limits of 301LN, 316L and TRIP
steels, determined in reversed plane bending, are about 350, 300 MPa and 400 MPa, respectively.
Hence, in absolute values the fatigue limit of the TWIP steels are considerably higher than those of
annealed austenitic stainless steels and equal to that of the 780-grade TRIP steel.
It is known that the fatigue limit of steel is roughly related to its tensile strength, so that the ratio fatigue
limit/tensile strength (FL/TS) is between 0.4-0.6, see e.g. [3]. It was seen that the ratio FL/TS of the
TWIP steels varies between 0.42 and 0.48 (for AISI 304 is typically 0.42).


Fig. 3.2.1: S-N curves of the investigated TWIP steels and those of 301LN and 316L and high-strength
TRIP steel are included for comparison [1,2].






110

Crack nucleation and propagation
A few specimens were examined after the 25, 50 and 100 percents of the expected fatigue life to follow
the fatigue crack initiation and propagation.
It was seen that many cracks emerge from the ordinary grain boundaries (intergranular cracking) as well
as from annealing twin boundaries (twin cracking).
To investigate the type of crack propagation in relation to the grain structure, a fatigued sample was
cycled at the stress level of 500 MPa until failure. A high density of intense slip bands in the region near
the main fatigue fracture was observed, as shown in Fig. 3.2.2. In addition, high densities of
intergranular cracks and annealing twin boundary cracks could be observed.


Fig. 3.2.2: The final fatigued structure of TWIP (Fe-22Mn-0.6C) steel after failure.


Based on the microscopy observations on tensile strained TWIP steels, mechanical twinning is an active
deformation mechanism under monotonic loading. By SEM-EBSD technique, mechanical twins can be
identified based on their orientation difference in relation to the surrounding matrix. The SEM-EBSD
samples analysis indicates that no mechanical twinning takes place in fatigue of TWIP steels, but only
intense slip bands are formed as a result of cyclic stressing. This means that the TWIP effect has no
essential role in cyclic deformation of these steels.

Influence of grain size
The results of flexural bending fatigue tests at the stress amplitude level of 500 MPa are shown in Fig.
3.2.3. The figure indicates that a significant beneficial effect on the fatigue life is obtained by refining
the grain size. Moreover, it can be seen that the fatigue limit of the structure with the smallest grain size
of 4.5 m equals or is higher than 500 MPa, because no failure occurred within 2.2 million cycles.




111


Fig. 3.2.3: Effect of the grain size on the fatigue life of the TWIP2 steel (Fe-22Mn-0.6C). All tests were
carried out at the amplitude of 500 MPa.


Conclusions task 3.2
The fatigue behavior of three high-Mn TWIP steels, with slightly different Mn contents (between 16
and 22 wt.%) and Nb or Al alloying were investigated using reversed bending loading and examining
the cyclic damage features on surfaces. The main conclusions can be drawn as follows:

(1) Fatigue behavior of three TWIP steels is quite identical. Fatigue stress limit (the cyclic life beyond
2x10
6
cycles) is well above their yield strength values. The ratio of fatigue limit/tensile strength is 0.42-
0.48 that is quite a similar value as commonly observed for various carbon steels and for Types 301LN
and 316L austenitic stainless steels.
(2) During cyclic loading, planar slip bands are formed in an early stage of fatigue life consisting of
extrusions and intrusions. With continuing cycling, the slip bands intersect with grain boundaries as
well as annealing twin boundaries producing local strain concentrations that induce microcracks at these
boundaries.
(3) Fatigue crack embryos nucleate at an early stage of fatigue life (25%) at sites of intersections of
slip bands and grain boundaries as well as annealing twin boundaries.
(4) Crack propagation takes place along slip lines, grain and twin boundaries but the overall path is
mainly transgranular in its character. In this stage, ductile striations are formed on fracture surfaces.
(5) Microcracks link and propagate readily along grain boundaries indicating some degree of inherent
grain boundary weakness, as suggested in the literature for austenitic high-Mn steels.
(6) Neither mechanical twins nor -martensite are formed during cyclic loading in the investigated
TWIP steels, so that the TRIP or TWIP effects seem to play no role in the course of high-cycle fatigue.
(7) The degree of cyclic hardening revealed by hardness is strongly dependent on the grain size
decreasing with refined grain size.
(8) Refinement of the grain size improves significantly the fatigue strength of the 0.6C-22Mn TWIP
steel.


Task 3.3 Evaluation of impact strength by means of Charpy tests at different temperature
In this task 3 the absorbed energy of the five compositions being studied was determined by charpy
tests in four different temperatures. The impact tests were performed according to the test standard NP
EN 10045-1, three specimens were taken from each material.
It is possible to see the results in table 3.3.1 and the graphic on figure 3.3.1.





112

Material Temperature [C] Absorbed energy[Joules/cm
2
] Average Absorbed energy[Joules/cm
2
]
-50 150.00
-50 175.00
-50 150.00

158.33
0 166.67
0 133.33
0 141.67

147.22
20 108.33
20 100.00
20 100.00

102.78
150 125.00
150 125.00





TWIP 1
150 141.67

130.56
-50 115.38
-50 115.38
-50 141.03

123.93
0 102.56
0 89.74
0 89.74

94.02
20 102.56
20 76.92
20 89.74

89.74
150 115.38
150 115.38





TWIP 2
150 96.15

108.97
-50 116.67
-50 138.89
-50 111.11

122.22
0 106.38
0 127.66
0 111.70

115.25
20 72.22
20 72.22
20 83.33

75.93
150 111.11
150 127.78





TWIP 3
150 100.00

112.96
-50 86.21
-50 68.97
-50 68.97

74.71
0 77.59
0 77.59
0 77.59

77.59
20 51.72
20 51.72
20 51.72

51.72
150 51.72
150 60.34





TWIP 4
150 60.34

57.47
-50 75.76
-50 83.33
-50 90.91

83.33
0 75.76
0 83.33
0 83.33

80.81
20 60.61
20 60.61
20 68.18

63.13
150 75.76
150 75.76





TWIP5
150 75.76

75.76
Table 3.3.1 Charpy



113

0
20
40
60
80
100
120
140
160
180
-50 0 20 150
Temperature (C)
A
b
s
o
r
b
e
d

E
n
e
r
g
y

(
J
/
c
m
2
)
TWIP 1
TWIP 2
TWIP 3
TWIP 4
TWIP 5

Figure 3.3.1 Charpy tests results for the five TWIP compositions.



Conclusions task 3.3
Comparing the Charpy values of TWIP variants arise that TWIP1 reveals the best results at all tested
temperature. TWIP2 and TWIP3 are slightly better than TWIP4 and TWIP5. Qualitatively the Charpy
energy behavior of TWIP steels as a function of the temperature is quite similar to stainless steels such
as AISI304. In fact the Charpy energy remains of the same order from +150C down to -50C, with a
slight increase from RT down to -50C.


Task 3.4 Plain strain compression tests
Plain strain compression tests were completed and the stress-strain curve relevant to TWIP2 is shown in
the fig. 3.4.1. The work hardening of TWIP2,3,4,5 steels is significantly higher than stainless steels
(AISI304). At a true strain of 0.5 the difference in terms of stress is about 38%. TWIP1 reveals a softer
behavior quite different to other TWIP2-3-4-5 steel grades and is more similar to AISI304 probably due
to presence of softer ferrite in microstructure. In table 3.4.1 are reported the stress corresponding at a
strain of 0.5.


Fig. 3.4.1: Plain strain compression tests results on
TWIP2 variant.
Table 3.4.1: Stress after a true strain
of 0.5.



114


Conclusions Task 3.4
The work hardening of TWIP2,3,4,5 steels is significantly higher than stainless steels; at a true strain of
0.5 the difference in terms of stress is about 38%. The above result implies difficulties in cold rolling in
terms of loads, number of passes or reduction ratio at each stage.
Depending on the hot strip thickness, an intermediate annealing treatment (two step cold rolling
process) could be necessary for obtaining the aimed final cold strip thickness (<2.0 mm).















































115

WP 4 Basic characterisation of application properties: formability, weldability and coating
ability

Task 4.1 Formability characterisation by means of Erichsen test and High-velocity forming tests.

Task 4.1.1 Erichsen test
The Erichsen cupping test is a simple stretch forming test of a sheet clamped firmly between blank
holders to prevent in-flow of sheet material into the deformation zone. The punch is forced onto the
clamped sheet with tool contact (lubricated, but with some friction) until cracks occur. The depth (mm)
of the punch is measured and gives the Erichsen index 'IE', standardised under DIN 50101.
In the table 4.1.1.1 and figure 4.1.1.1 it can be seen the results of the Erichsen tests on the TWIP steels.
These results demonstrate that TWIP steels are characterized by quite good forming ability.


Material
N of
tests
Thickness
[mm] IE [mm] Average
1.28 12.4
1.28 12.3 TWIP 1 3
1.28 12.5
12.40
2.12 11.7
1.76 11.9 TWIP 2 3
2.11 12.4
12.00
2.18 10.4
2.18 10.3 TWIP 3 3
2.18 10.4
10.37
1.23 10.9
1.21 11
1.21 11.5
TWIP 4 4
1.18 10.8
11.05
1.37 10.9
1.34 11.3 TWIP 5 3
1.35 11.3
11.17
Table 4.1.1.1: Erichsen tests results.

9.00
9.50
10.00
10.50
11.00
11.50
12.00
12.50
13.00
T
W
I
P

1
T
W
I
P

2
T
W
I
P

3
T
W
I
P

4
T
W
I
P

5
Erichsen test results

Fig. 4.1.1.1: Graphic representation of the Erichesen tests results for the five TWIP compositions.



116

Task 4.1.2 High-velocity forming tests
During the project the formability of TWIP-steels at a high deformation rate [1] has been investigated
and compared to the formability results using conventional Erichsen tests.
Cold rolled sheets of high-Mn TWIP steels with 1.5 mm thickness were prepared and supplied by CSM
for high-velocity forming testing. In the present work, a special high-speed Erichsen testing was
employed using an electro-hydraulic impulse forming unit (at the Stainless Steel Studio, Tornio,
Finland). In this instance, the Erichsen tests were carried out using a hemispherical punch with a
diameter of 20 mm at room temperature to investigate the stretch formability in accordance with ASTM
643-84 [2]. Some grease was set as a lubricant between the punch and the sheet. The Erichsen index
(IE) is the value of the punch penetration before cracking of the sheet. However, in a high-velocity
Erichsen test, the punch cannot be stopped in the instance of cracking, but the displacement of the
stroke must be adjusted beforehand. In the used equipment, the displacement can be adjusted at the
intervals of 0.25 mm, so that the actual IE value is something between the two dome heights (stroke
displacements) of highest crack-free and the first fractured Erichsen cups. However, in present tests the
displacements varied much more and problems appeared to adjust it precisely. Therefore, intervals in
the displacements obtained in the tests were often much longer.
To analyze the strains on the sheet samples occurred in forming, a circle grid was etched by applying an
electrochemical marking method on the samples to create arrays of overlapping circles (the diameter 2
mm).

Results
Figure 4.1.2.1 compares IE values (solid dome - first cracked dome heights) obtained for the
investigated TWIP steels in high-speed Erichsen testing in relation to the total elongation obtained in
quasi-static tensile tests. The figure also contains the corresponding data for AISI 304 austenitic
stainless steel [5].
It can be seen that variation among the steels is quite small. Generally, IE is higher if the elongation is
higher, and the best values are obtained for TWIP_2. However, better IE values were obtained at high-
speed Erichsen testing.


Fig. 4.1.2.1: Comparison between the Erichsen index (IE) in high-speed (and conventional) testing and
the total elongation (A) from quasi-static tensile tests [3] and that of AISI 304 [5].

In literature is reported that [7] the formability of a TWIP (Fe-15Mn-3Al-3Si) steel having a very
pronounced TRIP effect at different strain rates was enhanced with increasing strain rate from 2x10
-3
to
10
-1
s
-1
. The explanation is that due to the adiabatic heating of the deformed sheets (heated up to 70C)



117

at higher strain rates, the martensitic transformation was retarded, and consequently the ductility was
improved by more intense twinning.
In contrast the ductility of TWIP (Fe-25Mn-3Al-3Si) steel was found to decrease with increasing strain
rate from 10
-3
to 10
-1
s
-1
in tensile tests [8]. This can be attributed to the adiabatic heating of the sample
during the tensile test increasing the SFE and resulting in decreasing density of mechanical twins.
However, with increasing the strain rate up to 1000 s
-1
, the total elongation increases again reaching
values above that in tensile testing at the strain rate of 0.1 s
-1
.
It is possible to make comparison between the elongation in dynamic tensile tests ( 1000 & s
-1
) using
the Hopkinson split bar method and that in quasi-static tensile tests [3]. Then, for example, for TWIP_2
the total elongation is 83% under quasi-static tension and 80% under high-speed tensile testing, i.e. the
total elongation in these two cases is almost equal (note: the specimen shapes are very different).
In the conventional Erichsen testing according to the DIN 50101, the typical strain rate can be estimated
to be order of 0.01 s
-1
. (For instance, no 0.4 cylinder speed is 0.56 mm/s). In high-speed Erichsen
testing, where the speed of impact front is about 200 m/s, the strain rate can be order of 5 s
-1
(dome
height 10 mm; at 200m/s it takes 0.05 s. Strain is 0.26, hence, the strain rate =0.26/0.05s =5/s), i.e.
about 500 times higher.

Conclusions of task 4.1.2
Comparing quasi-static IE values with high-speed Erichsen testing arise that the total elongation
variation is quite small. Generally, IE is higher if the elongation is higher, and the best values are
obtained for TWIP_2. However, better IE values were obtained at high-speed Erichsen testing for all
TWIP grades except for TWIP1 grade.


Task 4.2 Laboratory coating tests and coating layer characterisation
Eight samples (four TWIP steel studied materials) were zinc coated using the batch hot-dip galvanizing
process. The batch hot-dip galvanizing process, also known as general galvanizing, produces a zinc
coating on steel products by immersion of the material in a batch of liquid zinc, which then forms a
durable bond to the iron at the atomic level. Before the coating is applied, the steel is cleaned to remove
all oils, greases, soils, mill scale, and rust. The cleaning cycle usually consists of a degreasing step,
followed by acid pickling (heated sulphuric acid) to remove scale and rust, and fluxing, which inhibits
oxidation of the steel before dipping in the molten zinc. In this project two different pre-treatment
preparations were used: The conventional one (chemical picking - marked DQ) and the replacement of
the two first chemical cleaning steps by mechanical pickling (marked DM). The reason for this
variation is related to the observation of possible hydrogen contamination of the samples in the first
situation.
After galvanization, i.e., after the deposition of the Zn based coating layer, the samples were
characterized. The visual control of samples surfaces revealed a general uniformity of the coating layer
(eventually, in two cases, with an over-thickness of coating that was confirmed in coating layer
thickness measurement) with no bulges. The samples were then subjected to a test to evaluate the
adhesion of their galvanized layer.
The galvanization adhesion test was made through the cross test method according to standards NF
A91-121 and NP EN ISO 1461. As shown in figures 4.2.1-2 for TWIP2 (the results for other TWIP
grades were similar) all the tests were acceptable according to the standard since no detachment of any
small square was verified. No noticeable differences were detected between the two pre-treatments in
the galvanized adhesion layer test.





118


Fig. 4.2.1: sample TWIP 2 DM. Fig. 4.2.2: sample TWIP 2 DQ.


The thickness of the coating layers was determined through its measurement in a transversal section of
the samples. The results obtained are presented in the table below.





Sample
s ref.
Thickness (m)
Averag
e
Standar
d
deviatio
n
TWIP 2
DM
119,
2
95,7
140,
5
126,
7
140,
4
105,
4
166,
0
140,
4
138,
3
106,
4 127,9 21,4
TWIP 2
DQ
134,
8
138,
3
130,
9
107,
5
110,
7
120,
2
109,
6
106,
4
112,
8
112,
8 118,4 12,0
TWIP 3
DM
113,
8
134,
1
117,
1
138,
3
126,
7
109,
6
114,
9
110,
6
121,
3
101,
1 118,7 11,5
TWIP 3
DQ
103.
4
97.7
104.
6
117.
1
114.
8
122.
8
117.
1
111.
4
95,5
101.
2 108.6 9.3
TWIP 4
DM
140,
4
128,
7
121,
3
131,
9
124,
5
130,
9
128,
7
156,
4
125,
5
140,
6 132,9 10,4
TWIP 4
DQ
95,0
100,
1
93,8
100,
0
98,9
104,
3
119,
2
117,
0
121,
9
126,
8 107,7 12,2
TWIP 5
DM
136,
2
125,
5
124,
5
117,
0
124,
5
123,
4
94,7
104,
3
112,
9
98,0
116,1 13,4
TWIP 5
DQ
180,
9
211,
7
243,
7
267,
2
239,
4
210,
7
264,
6
186,
6
191,
5
204,
5 220,1 31,6
Table 4.2.1: Thickness of coating layers.

The coatings layer thickness measurement shows that sample TWIP 5 DQ presents the highest value
but, with this exception no noticeable difference exists between the two sets of samples obtained with
two different pre-treatments. The most common reason for the different zinc coating thickness, when
using the same galvanization conditions, is the chemistry of the steel pieces. There are two elements of
steel chemistry which most strongly influences the final thickness and appearance; silicon and
phosphorous. Both silicon and phosphorous promote coating growth.



119

The recommended silicon composition is either less then 0.04% or between 0.15% and 0.25%. Any
steels outside these ranges are considered reactive steels and are expected to form zinc coatings that
tend to be thicker resulting of the rapid zinc-iron intermetallic growth. In this project the steels under
analysis have silicon contents near the maximum limit (between 0.2 and 0.22%); this could be a reason
for the different thickness values in the galvanized samples. With the objective of determining the
galvanisation composition EDS analysis in the pure zinc layer of the zinc coating was performed. As
reported in the following table the used Zinc bath presented small additions of Phosphorus and
Aluminium.

Weight % Element Weight %
Sigma
Zn K 97.68 0.14
Al K 0.91 0.09
P K 0.75 0.07
TABLE 4.2.2: EDS ANALYSIS.

All the samples were metallurgically characterized after the galvanization process.
In general, the typical galvanization structure was observed. The batch hot-dip galvanized coating
consists of a series of zinc-iron alloy layers with a surface layer of almost pure zinc. The alloy layer is
as much as 50% of the total thickness and it consists of two or more distinct zinc/iron layers. Each layer
has a specific amount of iron and zinc. A representative photomicrograph of the alloy layer that forms
while the steel is immersed in the bath is shown in Figure 4.2.3.



Fig. 4.2.3: Sample TWIP 5 DM (200X).


However some quality defects were observed. In all the chemical picking samples large black spots in
the Zn coating defined as gas pockets can be observed. In the fig. 4.2.4-4.2.7 are shown some example
of such defects relevant to TWIP2 and TWIP5. This could be an effect related to hydrogen absorption
by steel overpickled before galvanizing. Hydrogen absorbed by overpickled steel, if not completely
expelled at the temperature of the molten zinc bath, may be trapped in the coating, causing gas pockets
and blisters trapped in the alloy layers.
This defect was not present in the mechanical pickling samples since in this process sulphuric acid was
not used.



120


Fig. 4.2.4: Sample TWIP 2 DM (200X). Fig. 4.2.5: Sample TWIP 2 DQ (500X).

Fig. 4.2.6: Sample TWIP 5 DM (200X). Fig. 4.2.7: Sample TWIP 5 DQ (500X).

Other defect was the lack of uniformity and reproducibility in the quality of the interface zinc/steel.
Even after mechanical or chemical surface preparation it was impossible to eliminate all the superficial
defects resulting from the samples production. For this reason in the same sample it was possible to find
areas with a very good quality of the interface between the steel and the coating and others with
adhesion defects caused by strip surface irregularities (cracks). In the TWIP steel material it was
impossible to etch the area near the zinc coating due to the zinc coating cathodic effect. Nevertheless
the galvanising temperature used (451C) do not seem to be enough to promote any phase
transformation or zinc inter-grain diffusion on the TWIP material.


Conclusions of task 4.2
The visual control of samples surfaces revealed a general uniformity of the coating layer.
The galvanization adhesion test was made all the tests were acceptable according to the
standard since no detachment of any small square was verified. No noticeable differences were
detected between the two pre-treatments in the galvanized adhesion layer test.
All the samples after the galvanization process revealed the typical galvanization structure. The
batch hot-dip galvanized coating consists of a series of zinc-iron alloy layers with a surface
layer of almost pure zinc. The alloy layer is as much as 50% of the total thickness and it
consists of two or more distinct zinc/iron layers. Each layer has a specific amount of iron and
zinc.
Some quality defects were observed. In all the chemical picking samples large black spots in
the Zn coating defined as gas pockets can be observed. This is the effect of hydrogen absorption
by steel overpickled before galvanizing. This defect was not present in the mechanical pickling
samples since in this process sulphuric acid was not used.




121

Task 4.3 Characterization of Weldability

TWIP laser welding
During the project it was decided to concentrate the welding tests on laser welding. This decision was
taken having in mind that this is in fact a very common method in the automotive industry for welding
thin sheet steel (<2.0 mm). Some preliminary tests with resistance spot welding were performed and
were sufficient to conclude that the use of these steels in spot welding is adequate. The laser welding
was the process chosen to be fully tested because the application of laser in the automotive industry has
increased in the last years replacing several times resistance spot welding. The following study was
focused on the understanding of TWIP steel behaviour in joining, particularly in laser welding.
Four high-Mn based Fe-alloys with austenitic structure developed by alloying with carbon, aluminium
and silicon elements aiming to obtain different grades of TWIP steels were studied. TWIP 1 was not
characterized because it cannot be considered a TWIP steel due to its mixed microstructure
(ferrite+austenite).
Laboratory cast ingots were homogenized at 1200 C for 1 hour to remove the segregation of the
alloying elements, especially those Mn based. Subsequently, they were hot rolled to 2 mm thick bands
in a laboratory rolling mill. Finally, the bands have suffered a heat treatment at 1000 C for 5 min.
The used laser system was a diode laser unit, with a maximum power of 3KW working at a wavelength
of 940 nm and 808 nm. This laser is connected to a KUKA robot (model R125F/2)
An in-depth detailed observation of the diode laser welded joint to explain how weldability assessment
was done and confirm the absence of the heat affected zone as well as welding defects. Some conditions
of the metallurgical structure were emphasized as important for the welding final structure. Four of the
five TWIP materials welded with the following laser welding conditions were fully characterized
Diode laser welded joints were made using 2 mm-thick plates in a butt joint configuration.
The optimisation of the studied welds using the different steel compositions has been carried out
following a sequence of trials. The criterion for optimisation was the full penetration and absence of
defects.
The final selection of the welding procedure has been based on the technical experience, visual analysis
and X-ray tests. A full metallurgical characterization of each welded sample was made after the process
optimisation. Table 4.3.1 summarizes the optimal laser welding parameters for each steel composition.

Gas protection Thickness With Power Speed
Argon [l/min] [mm] [mm] [W] [mm/s]
2 15 2.0 180 1500 10
3 15 1.5 140 1500 12
4 15 2.0 90 1600 15
5 15 2.1 140 1500 10
Table 4.3.1: Optimal laser welding parameters for each TWIP steel composition.

Some observations made during the welding tests are considered relevant:

- high quantity of fumes (probably Mn evaporation) was observed especially in TWIP4;
- oxide contamination of the welding surface existed even with inert gas atmosphere (argon).

Vickers hardness tests were performed to evaluate the mechanical properties in the welded joints.
Measurements were extended to the entire thickness along the centreline of the WZ (welded zone) with
a load of 2.5 Kg.






122


Visual and Macrographic Analysis
The samples submitted to visual and macrographic inspections confirmed the possibility of having
sound welds with a good repeatability for all the studied compositions. In all cases, the penetration was
complete along all the plate thickness, and the welds were free from cracks or other defects. Some of
the detected defects were a consequence of the non-homogeneity of the sheets thickness and difficulty
in joint positioning. Figure 4.3.1 and 4.3.2 illustrates the diode laser weld performed on the TWIP3
steel where we can emphasize the presence of surface oxide contamination even with gas protection and
the full penetration of the welding. This oxide contamination proves not to have any consequences on
the welding quality as we can see later on this article.




Fig. 4.3.1: Visual observation of the front
surface of the TWIP3 diode laser weld.


Fig. 4.3.2: Visual observation of the root
surface of the TWIP3 diode laser weld.

Three examples of typical cross sections of the welded joints are shown in figures 4.3.3 to 4.3.5. These
allow to observe different regions of the welded joint, namely the base and welded materials and to
conclude that no visible heat affected zone exists.


Fig. 4.3.3: Low-magnification light optical
micrograph from TWIP2 steel showing a cross
section of the welded joint.
Fig. 4.3.4: Low-magnification light optical
micrograph from TWIP3 steel showing a cross
section of the welded joint.
0.5 mm
0.5 mm



123



Fig. 4.3.5: Low-magnification light optical
micrograph from TWIP4 steel showing a cross
section of the welded joint.
Fig. 4.3.6: Micrography of TWIP2 steel base
material (500X).



Optical Observation
All the four TWIP base materials present a microstructure representative of this steel grade. It was a
fully austenitic structure with globular and fully recrystallised grains. Figure 4.3.6 presents TWIP2
base material microstructure. Figure 4.3.7-8 show the microstrutural variation in TWIP3 sample from
the base material to the welded zone, making clear the transition zone. The absence of an actual heat
affected zone derives from the low heat input of the laser process. Figure 4.3.9 presents, as an example,
the welded zones microstructures as observed in TWIP2 samples. The typical microstructure observed
in most of the welded samples is constituted of an austenitic structure superimposed in a cellular-
dendritic solidification structure. However, figure 4.3.9 pertaining to the welded material of TWIP2
sample shows the presence of -martensite. The zone where the -martensite appeared corresponds
nearly to the top face of weld axis, which is a zone of higher cooling rate.



Fig. 4.3.7: Micrography of TWIP3 welded
sample showing the transition base material-
welded material (200X).

Fig. 4.3.8: Micrography of TWIP3 welded joint
(200X).


The appearance of -martensite is not desirable due to the significant reduction that it implies in
ductility. As the welding conditions were quite similar in all experiments then some reason should exist
to justify the observed behaviour in TWIP2 sample.
0.5 mm



124



Fig. 4.3.9: Micrography of TWIP2 welded material showing the presence of -martensite (200X).


As referred before, the quite high ductility behaviour of TWIP steels is associated to the stacking fault
energy (SFE) which is the ignitor of the twinning mechanism. A possible explanation of the occurrence
of martensite in the welded zone could be related to a change in chemical composition in particular the
content of Mn and C during welding. Although the difference in terms of composition could be small,
the risk of reaching the austenite instability (deformation induced) could be the cause of -martensite
formation.

ASTM Grain
Size
2 6.994
3 9.895
4 7.754
5 7.379
Table 4.3.2: ASTM grain size measurements using the circular interception
technique according with the ASTM E 112 standard.


Vickers Hardness Measurements
Figure 4.3.10 shows the Vickers hardness distribution through the weld transverse cross section in the
different welded TWIP steel samples. The measurements were performed in three longitudinal rows
(top, middle and bottom weld metal levels). The base materials hardness of TWIP3, TWIP4 and TWIP5
steels present similar values, and all the weld zones present acceptable values which indicate that the
mechanical properties will be maintained. By contrast, TWIP2 shows lower hardness values in the base
materials which seem to agree with the measured higher average grain size and, in addition, an abrupt
increase in the weld zone hardness is observed. The later is in agreement with the observed presence of
-martensite.



125

150
160
170
180
190
200
210
BM1 WM BM2
Welding Zones
V
i
c
k
e
r
s

H
a
r
d
n
e
s
sTWIP 1
TWIP 2
TWIP 3
TWIP 4

Fig. 4.3.10: Vickers hardness measurements.


Based on the experimental laser welding analysis of four TWIP steel compositions, weldability of these
materials was established as well as the main influencing factors. The work allowed to conclude that
the joining of TWIP steels is easily achievable by laser welding. The factors that could influence the
steel welding behaviour and its quality are intrinsically related to the steel composition and
crystallographic structure. All the factors influencing stacking fault energy of base materials are the key
for a sound joining of TWIP steels.


Dissimilar Welds
J oining dissimilar materials became inevitable in engineering industries for both technical and
economic reasons. The adoption of dissimilar-metal combinations provides possibilities for the flexible
design of the product by using each material efficiently, i.e., benefiting from the specific properties of
each material in a functional way. For this reason a study of the weldability of TWIP steels in dissimilar
welds was carried out.
After receiving from the industrial partners more TWIP material all the samples for welding were
prepared to eliminate the bad superficial conditions of the as received material. High strength steels to
perform the dissimilar welds were acquired (DOCOL 600 DP and DOCOL 800 DP). Docol DP are cold
reduced dual phase steels subjected to special heat treatment in the continuous annealing line, which
produces a two-phase structure in which the ferrite that imparts unique forming properties is one of the
phases, and martensite that accounts for the strength is the other. The microstructure of DOCOL 800DP
steel can be seen in figure 4.3.11 .




126


Figure 4.3.11 Docol 800DP steel microstructure taken in a scanning microscope (X500).


The following tables describe the high strength steels characteristics (chemical composition and
mechanical properties). In the DP steels, the difference between the yield strength and the tensile
strength is wide, which means that the steel has good ability to distribute the strain during working.
Typical applications of this material are safety components in cars like door beams, bumper
reinforcement and seat tracks.


Steel grade C [%] Si [%] Mn [%] P [%] S [%] Al
t
[%] Nb
[%]
Docol 600DP 0.10 0.20 0.80 0.010 0.002 0.040 0.015
Docol 800DP 0.13 0.20 1.50 0.010 0.002 0.040 0.015
Table 4.3.3 Docol DP chemical composition.

Due to serious malfunctions in ISQ diode laser it was necessary to perform the welds outside ISQ in a
CO
2
laser. The steels combinations were the ones described in table 4.3.4.


TWIP 2 TWIP 3 TWIP 4 TWIP 5
DOCOL 600 TWIP 2/600 TWIP 3/600 TWIP 4/600 TWIP 5/600
DOCOL 800 TWIP 2/800 TWIP 3/800 TWIP 4/800 TWIP 5/800
Table 4.3.4 Steels combinations welded with CO
2
laser.

CO
2
laser welded joints were made using a tailored blank joint configuration. This option was taken to
give an idea of the potentialities of this material in this kind of application. A TWIP steel plate of 3 mm
was welded to a Docol DP steel plate of 1.5mm as illustrated in the figure 4.3.12.

Martensite
Ferrite



127


Fig. 4.3.12: Tailored blank weld configuration used in the welding tests.



The welds were processed using a 1.7 kW CW-CO
2
laser consisting of the laser source, a beam delivery
system, and a CNC worktable. The laser parameters used were: laser power 1500 W, speed 25 mm/s
and frequency 50000Hz. Figure 4.3.13 illustrates the CO
2
laser weld performed on the TWIP4-600
steels combination where we can emphasize the absence of superficial defects and the full penetration
of the weld.



Fig. 4.3.13: Visual observation of the front surface of the TWIP4 Docol 600DP CO
2
laser weld.



The samples submitted to macrographic inspections confirmed the possibility of having sound welds
with a good repeatability for most of the studied compositions. In TWIP 2 and TWIP 3 welds, the
penetration was complete along all the plate thickness, and the welds were free from cracks or other
defects. However, in TWIP 4 and TWIP 5 welds with some porosity were detected. The porosity was
present both in the welds with DOCOL 600 DP steel and the ones with Docol 800DP steel.
Four examples of typical cross sections of the welded joints are shown in figures 4.3.14 to 4.3.17. It
allows to observe the different regions of the welded joint, namely the base and welded materials and to
conclude that heat affected zones were only present in Docol steel sides.


Docol DP steel
TWIP steel
Welding position
Dissimilar weld



128



Fig. 4.3.14: Low-magnification light optical
micrograph showing a cross section of the welded joint
- TWIP2 and Docol 600DP steels.
Fig. 4.3.15: Low-magnification light optical
micrograph showing a cross section of the
welded joint - TWIP2 and Docol 800DP steels

0.3 mm
0.3 mm



129

.




Fig. 4.3.16: Low-magnification light optical micrograph
showing a cross section of the welded joint - TWIP3 and
Docol 600DP steels.
Fig. 4.3.17: Low-magnification light optical
micrograph showing a cross section of the welded
joint - TWIP3 and Docol 600DP steels.





Vickers hardness tests were performed to evaluate the mechanical properties in the welded joints.
Measurements were extended to the entire thickness along the centreline of the WZ (welded zone) with
a load of 0.2 Kg.
As a reference figure 4.3.18 represents the hardness distribution curve of a Docol 800 DP laser weld.

0.3 mm
0.3mm



130

150
200
250
300
350
400
450
500
-8 -6 -4 -2 0 2 4 6 8
Dist ance (mm)
H
a
r
d
n
e
s
s

(
H
V
5
)
Docol 800DP

Fig. 4.3.18: Hardness distribution curve of a Docol 800 DP laser weld.


Figures 4.3.19 to 4.3.24 show the Vickers hardness distribution through the weld transverse cross
section in the different welded TWIP - Docol steels combinations samples. The measurements were
performed in one longitudinal row.



Fig. 4.3.19: Graphic representation of the hardness measurements performed on the TWIP 2 DOCOL
600DP weld.

150
200
250
300
350
400
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 2 - 600
D Do oc co ol l 6 60 00 0 D DP P
T TW WI IP P 2 2 Z ZT TA A
W We el ld d z zo on ne e



131


Fig. 4.3.20: Graphic representation of the hardness measurements performed on the TWIP 2 DOCOL
800DP weld.



Fig. 4.3.21: Graphic representation of the hardness measurements performed on the TWIP 4 DOCOL
600DP weld..



Fig. 4.3.22: Graphic representation of the hardness measurements performed on the TWIP 4 DOCOL
800DP weld.

150
200
250
300
350
400
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 4 - 600
D Do oc co ol l 6 60 00 0 D DP P T TW WI IP P 4 4 Z ZT TA A W We el ld d z zo on ne e
150
200
250
300
350
400
450
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 4 - 800
D Do oc co ol l 8 80 00 0 D DP P T TW WI IP P 4 4
Z ZT TA A
W We el ld d z zo on ne e
150
200
250
300
350
400
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 2 - 800
D Do oc co ol l 8 80 00 0 D DP P T TW WI IP P 2 2
Z ZT TA A
W We el ld d z zo on ne e



132


Fig. 4.3.23: Graphic representation of the hardness measurements performed on the TWIP 5 DOCOL
600DP weld.




Fig. 4.3.24: Graphic representation of the hardness measurements performed on the TWIP 5 DOCOL
800DP weld.



In a general way the weld zone present hardness values similar to the TWIP steel base material values.
The exception to the previous was found in TWIP 4 welds were the weld zone hardness value increases
to around 350 HV. Another consistent trend was the high hardness values presented in the heat affected
zone of the Docol steels. Figures 4.3.25 and 4.3.26 allow a comparative observation of the hardness
measurements performed on the studied welds.




150
200
250
300
350
400
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 5 - 600
D Do oc co ol l 6 60 00 0 D DP P
T TW WI IP P 5 5 Z ZT TA A
W We el ld d z zo on ne e
150
200
250
300
350
400
450
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 5 - 800
D Do oc co ol l 8 80 00 0 D DP P T TW WI IP P 4 4
Z ZT TA A
W We el ld d z zo on ne e



133

0
50
100
150
200
250
300
350
400
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 2 - 600
TWIP 3 - 600
TWIP 4 - 600
TWIP 5 - 600
0
50
100
150
200
250
300
350
400
450
0 2 4 6 8 10 12 14 16 18 20 22 24 26
H
a
r
d
n
e
s
s

(
H
V

0
,
2
)
TWIP 2 - 800
TWIP 3 - 800
TWIP 4 - 800
TWIP 5 - 800
Fig. 4.3.25: Graphic representation of all the hardness
measurements performed on Docol 600DP steel welds.

Fig. 4.3.26: Graphic representation of all the
hardness measurements performed on Docol
800DP steel welds.


Conclusions Task 4.3
Based on the experimental laser welding analysis of four TWIP steel compositions, weldability of these
materials was established as well as the main influencing factors. The work allowed to conclude that
the joining of TWIP steels is easily achievable by laser welding. The factors that determine the good
welding behaviour and quality of TWIP steels are intrinsically related to the steel composition and
austenitic structure.
Concerning the dissimilar steel welding all the weld and heat affected zones present acceptable
hardness values which indicate that the mechanical properties of the base materials are matched or
improved after laser welding. This study permitted to prove the good potentialities of TWIP materials
on automotive applications where the welding ability is one the the main requirements.


















































































135

WP5: Industrial trial
The industrial trial foreseen in the WP5 was not performed and for this reason the activities scheduled
in WP5 have been only partially accomplished. The reasons at the basis for the delay of the cast and
finally for cancelling are discussed in the following section 5.2. Anyway the results achieved in WP5
can be summarised as follows:
Metallurgically based selection of TWIP steel to be cast (Task 5.1).
Analysis of the impact of TWIP steel production on manufacturing route.


Task 5.1 Selection of the most interesting TWIP steel variant, for automotive applications, on the
basis of the previous WPs results.

Introduction
The principal aims of the industrial trial heat can be summarized in the following points:

Metallurgical characterization of the TWIP strip produced by industrial cycle;
Evaluation of TWIP steel processing ability in terms of casting, hot and cold rolling process,
etc.

All the strip produced will be used exclusively for the in-depth characterization in terms of
microstructure, mechanical properties, and technological properties (forming ability, welding ability,
etc).

Selection of the TWIP variant for the industrial trial
In view of the industrial trial, to be performed at Duferco steel works, an in-depth review of the TWIP
variants properties was carried out. It is worthy to remind that in the present project 5 TWIP steel
compositions were selected (table 5.1.1) and the relevant properties were investigated.


TWIP Variant Fe Nb Al C N Si Mn
1 Bal. - 3.02 0.01 0.0015 3.00 21.30
2 Bal. - 0.012 0.59 0.0040 0.22 22.30
3 Bal. 0.019 0.010 0.60 0.0040 0.20 17.80
4 Bal. - 1.54 0.29 0.0060 0.21 16.40
5 Bal. - 0.011 0.23 0.2 0.20 21.00
Table 5.1.1: TWIP compositions investigated in the metaldesign project.


TWIP1 and 2 were selected as reference steel. Nevertheless also for these steel grades the knowledge of
metallurgical properties in terms of SFE, recrystallization kinetics, strain hardening behavior, etc , was
largely lacking.
In parallel, at the start of the project, the basic metallurgical parameters controlling the TWIP effect in
high Mn steels were identified and investigated. The SFE (stacking fault energy) was identified as the
main metallurgical parameters controlling the steel metallurgical properties. Thermodynamical models
based on empirical equations (Allain, Grssel, Dumay, etc) together with Thermocalc calculations were
used in order to evaluate the SFE and the effect of the main alloy elements on SFE. In addition to SFE
was also recognized that the austenite stability during deformation or temperature variations (both at
low and high temperature) is an other important metallurgical parameter to taken into account when
different TWIP steels are compared.



136

On the basis of the selected reference steels (named TWIP1 and TWIP2) three further compositions
were designed aiming to achieve with different alloy contents the range of SFE able to guarantee a good
TWIP effect during deformation. The reasons and the approach underlying the metallurgical design of
the newer chemical compositions selected are described in the task 1.1.
For the selection of the TWIP steel for the industrial trial the following aspects were focused:

Stable austenitic microstructure revealing a TWIP effect (deformation induced twinning ) on a
wide range of temperature (at least +50C -50C).
Tensile properties: in particular high elongation to rupture and strain hardening coefficient. This
requirement is necessary for a good forming ability and for a high energy absorption property.
Technological properties: welding ability, forming ability, coating ability, etc. These properties
are of particular importance for these steels because the main applications for TWIP steel is for
automotive sector.
Processing ability: good casting ability, hot and cold rolling ability, pickling ability.
Lower industrial costs and impact on environment (as low Mn content as possible);

During the project almost all of these aspects were deeply investigated and now a enough clear frame of
the behavior of the steel grades designed is available.
Taking into consideration all the above aspects the best performing steel, as well as documented in this
and previous reports, is represented by TWIP2. Nevertheless the choice of this steel grade was excluded
from the start of the project because it was introduced in the project only for reference aim and is patent
covered. The selection was therefore focused on the newer steel grades metallurgically designed in the
present project i.e. TWIP3, TWIP4 and TWIP5.
On the basis of the above metallurgical and economical aspects all the steel grades designed show
several attractive features. TWIP3,4,5 steels in terms of tensile, forming ability and welding properties,
even if, in some instances lower than the reference TWIP2 steel grade, revealed quite interesting
properties that could find a good favor in the automotive market. Tensile elongation larger than 50%
with yield stress and tensile strength of respectively 280-300MPa and >800MPa were found. The strain
hardening behavior of TWIP3,4,5 is also very interesting and in the case of TWIP 3 is really very close
to TWIP2 steel.
From the metallurgical point of view one of the most relevant topic is represented by austenite stability
during deformation both at low and high temperature. At low temperature TWIP4 and TWIP5 as well as
TWIP1 revealed a significant TRIP behavior (formation of martensite during deformation even at room
temperature). TWIP3 showed a higher austenite stability and a behavior closer to TWIP2 steel.
At higher temperatures TWIP 3 also revealed a clear TWIP behavior even at 250C. Finally hot torsion
tests carried out on TWIP2 and TWIP3 revealed a very good intrinsic ductility for both steel.
On the basis of all these metallurgical aspects, of processing ability and finally in order to reduce the
extra alloy costs and impact on environment for the industrial heat was preferred the TWIP3 variant.


Conclusions of task 5.1
TWIP3 is the selected TWIP grade to be cast at Duferco steelworks. TWIP3 steel grade (chemical
composition reported in following table) is characterized by a markedly lower Mn content (25% less
than TWIP2) that is the most expensive element in TWIP steels and, as well known, the element that
could have unwished impact on environment during steel making due to Mn evaporation. The
properties revealed by this steel if, in some instance, are below the TWIP2 are really promising and



137

could be further improved by means of a fine tuning of the alloy design and industrial processing
conditions.


Fe Mn C Si Nb
min bal 16.00 0.60 0.20 0.015
max bal 17.50 0.65 0.30 0.030
Table 5.1.2 Range of elements for TWIP3 steel grade to be cast at Duferco steelworks.



Task 5.2 Coil supplying and material processing (hot and cold rolling, annealing treatments,
pickling and coating).
The scheduling of the TWIP industrial heat suffered the major deviation of the activities of the present
project because of more than expected difficulties and technical challenges related to TWIP steel
production. Two were the main issues:
1. Installation of a vacuum degassing plant due to risk of hydrogen embrittlement
susceptibility of high Mn steel;
2. Definition of the steelmaking route of high Mn steel using a direct current electric arc
furnace (DC-EAF).
In the following are summarized the activities carried out on these topics.

Installation of a vacuum degassing plant due to risk of hydrogen embrittlement susceptibility of
high Mn steel
The development of high Mn TWIP steel faces a number of technical challenges related to
steelmaking, casting and strip processing. On the basis of recent literature, even if unclear, could be
inferred that TWIP steels, could be sensitive to hydrogen embrittlement even in relation with the
formation of martensitic phases in the microstructure of deformed parts. This phenomenon should be
carefully examined in the case of the high Mn steels production without vacuum degassing facilities.
Duferco La Louviere steelworks planned the installation of a VD facility aiming to achieve with this
facility a significant improvement not only for hydrogen content reduction in steel but also to widen the
range of feasible steel grades (low C content). For this reason the scheduling of the TWIP heat was
postponed of 1 year. In fig. 5.2.1 is shown a typical kinetics of hydrogen removal curve during a VD
process. As can be noted into about 20 min of VD process is possible to reduce the hydrogen content in
steel from 3.5 ppm down to 1.0-1.5 ppm.




138


Fig. 5.2.1 Typical kinetics of hydrogen removal curve during a VD process using different Argon
pressure.

Unfortunately several causes determined a larger delay of the VD facility completion inclusive, of
course, the recent steel markets crisis (2008-09) that widened the time for VD installation and
commissioning work.

Evaluation of the steelmaking route of high Mn steel in a direct current electric arc furnace (DC-
EAF).
The feasibility of TWIP steel on a direct current arc furnace required a in depth study of the
metallurgical interactions of steel and furnace soils electrodes for the evaluation of the potential risks of
furnace damagement. Whatever was the chosen operating practice at EAF (selected scrap without deP
or normal scrap with deP and deslagging operations, the addition of an high amount of Mn ferroalloys
in the furnace was required. The only way to perform this additions was to use a charge basket when the
first baskets of scrap were melt. This operation led to the formation of a small mountain of Mn alloy
on the bottom of the furnace, just in contact with the soils electrodes. It is well known that the melting
of a ferroalloy happens for the formation of low melting points alloys between steel and the ferroalloy
added, the risk was to have a heavy consumption of the soils electrodes (which are steel billets) due to
the contact with Mn ferroalloys and the local high temperature in the arcing zone. The study was carried
out on the basis of thermo dynamical calculation and they showed that low melting point high
manganese content alloys forms during melting, but taking into account that soils electrodes are cooled
and of big dimensions, it was important to evaluate the time needed to reach an homogeneous chemical
condition in the liquid melt just to have an idea of possible real soils electrodes consumption.



139


Fig. 5.2.2: Fe-Mn diagram phase.

From the diagram phase Fe-Mn it can be seen that in the worst condition, the liquidus temperature of a
Fe-Mn alloy, with more than 60% of Mn, is around 1250C.
In AC furnace, the experience showed that about 15 minutes are needed to melt the whole Mn
ferroalloy bulk added with the basket. The time in Duferco DC furnace should be quite similar, and
taking in consideration that the soils electrode are water cooled, and that an important portion of them is
at a temperature lower than 1200C, it should be reliable that no catastrophic damages to the bottom of
the furnace should occur. This hypothesis is realistic even thinking that some DC Furnaces use instead
of steel billets, copper billets as soils electrodes. The melting point of copper is lower than that of
whatever kind of steel, but the water cooling enables the use of this kind of soils electrodes.
Moreover, when the bulk or ferroalloy is quite melt, the argon stirring performed by bottom porous
plugs should enhance the chemical homogenization, bringing rapidly to non dangerous conditions (the
Fe-Mn alloy at 20% of Mn has a melting point which is similar to some stainless steels, which can be
produced by DC furnaces). As the chemical and thermal homogenization of melt, is function even of
steel recirculation inside the furnace, induced by the use of porous plugs which are present on the
bottom of Duferco La Louvieres EAF, fluid dynamic simulations, by the use of numerical and physical
modeling (water models) should be necessary to evaluate the real industrial risk and to optimize the
production route. Laboratory tests were moreover required to validate the theoretical study. It was not
possible to perform such kind of laboratory tests due to lack of time so the heat was not performed,
even if it is quite clear that, determining the necessary right conditions, it should be possible to perform
the production of high Mn steels even in a DC Furnace.

Economical impact of high Mn TWIP steel grade production
In the present section will be summarised the results of an indepth analysis aiming to evaluate for all the
processes involved in the industrial manufacturing route the impact of the TWIP steel production due to
the very peculiar characteristics of this grade in terms of chemical composition, steel physical



140

properties, etc. First of all it is worthy to separate the aspects related to different process area of
manufacturing route:

1) Steelmaking.
2) Continuous casting.
3) Hot rolling.
4) Cold rolling and final annealing.

For what concern the first two points (primary area) the impact represented by TWIP production is
mainly related to:
Steelmaking process: The impact of TWIP steel production in the primary area can be
envisaged both in terms of process and environment. In terms of steelmaking process the issue
related to hydrogen embrittlement susceptibility resulted with an importance stronger than
expected in the technical annex. This issue has suggested to delay the industrial heat
scheduling in order to evaluate the risk of hydrogen embrittlement for TWIP steels and the
need to include a vacuum degassing facility (VD) for industrial TWIP steel manufacturing.
The total time for EAF+LF process is strictly related to the specific steelmaking practice
adopted. This means that different practice (in terms of type of Fe alloy additions) and
different facilities adopted (LF/VD, deslagging), could yield to dramatically different total
working time. As discussed in the previous section the specific steelmaking route of high Mn
steel has to be tailored according if DC or AC EAF process is adopted. The total steelmaking
process time is expected longer than conventional carbon steel and this could result in higher
energy consumption and higher refractory wear (EAF, ladle) due to high MnO content in the
slag. In terms of enviromental impact the high Mn content of TWIP steels determines during
both steelmaking and continuous casting large amount of smoke constituted mainly of
Manganese oxides. The management of so large amount of smoke constitute a environmental
problem that could require investments in terms of facilities necessary to avoid pollution. This
problem is not limited only to steelmaking process but also during continuous casting process
in the transitory of tundish filling (without covering powder) smoke can be developed. The
implementation of a tundish cover could be a solution.
Continuous casting process: TWIP steels are characterized by lower liquidus temperature with
respect to low-carbon steel and also the solidification range (liquidus-solidus) is wide (84C
for TWIP2 steel). These peculiarities have a strong impact on the casting process. It is worthy
to mention, among others, the following topics:

o Set-up/design of tailored casting powder for high Mn steel: the low liquidus
temperature and high Mn content does not allow the use of the same casting powders
used for low-C steels. Lubrication unevenness could be a cause of break-out and other
casting problems (cracks, depressions).
o Optimization of slab secondary cooling: Due to TWIP steel high temperature strength
the adoption of not correct practice of slab secondary cooling (below mould) could
damage seriously the bending and strengthening rolls of casting machine after only
one sequence cast.

If all these aspects are not optimized additional costs in terms of production loss and maintenance costs
could occur.

Concerning the hot rolling process the most critical aspect is represented by insertion of relatively small
number of TWIP slabs within the charge of walking beam furnace production. Due to quite different
physical properties of TWIP steel with respect to conventional carbon steel the adoption of hot charging



141

of slabs is necessary because is not recommended to change the working conditions (in terms of
soaking temperature and time) of the walking beam furnace. Of course this means that suitable facilities
for hot slab stacking as to be considered. The impact of hot charging can be assumed mainly on the
level of management of production planning and in case of stop at the hot rolling mill.

Finally for what concern the cold rolling and annealing process the impact of TWIP steel production is
mainly related to
Cold rolling process: TWIP steels work harden very quickly during cold deformation. The
work hardening of TWIP steels is significantly higher than stainless steels as shown by plain
strain compression tests. At a true strain of 0.5 the difference in terms of stress is about 38%.
The above result implies difficulties in cold rolling in terms of loads, number of passes or
reduction ratio at each stage. Depending on the hot strip thickness, an intermediate annealing
treatment (two step cold rolling process) could be necessary for obtaining the aimed final cold
strip thickness (<2.0 mm).

Annealing process: As stressed in previous WP3, TWIP steels tensile properties are seriously
affected by decarburization. The choice of a suitable annealing furnace atmosphere is of
paramount importance to avoid the occurrence of decarburization.



























































































143

Objectives of the project
The main objectives of this project are:
1. To complete the understanding of the TWIP steel metallurgy particularly for what regard
the following fields:
Solidification microstructure;
Recrystallization behaviour (dynamic and static) and texture formation.
Tensile properties and work hardening ability, precipitation behaviour as a function of
the steel chemical composition and its influence on the strip properties.
Influence of steel chemical composition on microstructure, mechanical properties,
strain hardening behaviour as well as on application properties such as formability,
weldability and coatability.

2. To design a metallurgically based manufacturing route (hot/cold rolling process, annealing
treatment) taking into account the specific capability of the DUFERCO plants.


Comparison of initially planned activities and work accomplished
The major deviation of the activities of the present project was caused by more than expected
difficulties and technical challenges related to steelmaking of TWIP steel. Two are the main issues:
On the basis of recent developments, one particular challenge is represented by the fact that TWIP
steels, could be sensitive to hydrogen embrittlement even in relation with the presence of
martensitic phases in the microstructure of deformed parts. This phenomenon should be carefully
examined in the case of the high Mn steels production without vacuum degassing facilities.
Evaluation of the steelmaking route of high Mn steel in a direct current electric arc furnace (DC-
EAF).
The above issue determined the delay of the project of 1,5 years and the solution was pointed out in the
installation at Duferco La Louviere of a vacuum degassing facility (VD) in order to produce a
significantly lower H content in steel.
The second issue is related to the fact that the world-wide experience on TWIP steelmaking is only on
alternate current electric arc furnace. The feasibility of TWIP steel on a direct current arc furnace
required a in depth study of the metallurgical interactions of steel and furnace soils electrodes for the
evaluation of the potential risks of furnace damagement. Whatever was the choosen operating practice
at EAF (selected scrap without deP or normal scrap with deP and deslagging operations, the addition of
an high amount of Mn ferroalloys in the furnace was required. The only way to perform this additions
was to use a charge basket when the first baskets of scrap were melt. This operation led to the formation
of a small mountain of Mn alloy on the bottom of the furnace, just in contact with the soils electrodes.
It is well known that the melting of a ferroalloy happens for the formation of low melting points alloys
between steel and the ferroalloy added, the risk was to have a heavy consumption of the soils electrodes
(which are steel bars) due to the contact with Mn ferroalloys and the local high temperature in the
arcing zone. The study was carried out on the basis of thermo dynamical calculation and they showed
that low melting point high manganese content alloys forms during melting, but taking into account that
soils electrodes are cooled and of big dimensions, it was important to evaluate the time needed to reach
an homogeneous chemical condition in the liquid melt just to have an idea of possible real soils
electrodes consumption. As the chemical and thermal homogenization of melt, is function even of steel
recirculation inside the furnace, induced by the use of porous plugs which are present on the bottom of
Duferco La Louvieres EAF, fluid dynamic simulations, by the use of numerical and physical modeling
(water models) should be necessary to evaluate the real industrial risk and to optimize the production



144

route. Laboratory tests were moreover required to validate the theoretical study. It was not possible to
perform such kind of laboratory tests due to lack of time so the heat was not performed, even if it is
quite clear that, determining the necessary right conditions, it should be possible to perform the
production of high Mn steels even in a DC Furnace. The study was carried out on the basis of
thermodinamical calculation and also taking into account the steelmaking experience of other high Mn
steels nevertheless laboratory tests to validate the theoretical study were needed and the time was not
enough. The missed realization of the industrial heat has determined the impossibility to perform the
Task 5.3 and Task 5.4 mainly relevant to characterization of the industrial hot and cold rolled strip.

Conclusions
Five TWIP steel grades (Fe-Mn-C-N and Fe-Mn-Al-Si-C) were selected on the basis of literature
review and thermodynamical calculations adopting as main characteristics for alloy design the SFE and
austenite phase stability. The chemical composition are reported in the following table.

Table 5.1.3: Selected TWIP grades chemical analysis.

The selected TWIP grades were characterised in terms on SFE, mechanical properties, microstructure
evolution during deformation, recrystallization, precipitation behaviour. The results revealed that TWIP
steel have really excellent tensile properties that make them extremely attractive for automobile and for
structural reinforcement. In addition, the positive strain rate sensitivity make TWIP steels suitable for
applications devoted to energy absorption (crashworthiness). The performances analysis revealed that
only TWIP2 and TWIP3 clearly behave as expected from TWIP steels, with the typical hardening stage
associated to profuse deformation twinning The TWIP steel variants with significant Al and Si content
(TWIP1 and TWIP4) require a additional tuning of steel chemistry to better balance the effect of Mn
and C and avoid the formation of second phases (ferrite or deformation induced martensitic phases). Al
seems to be effective on suppress the -martensite transformation but the formation of -martensite
has been detected on strained samples. At same way the variant TWIP5 with high nitrogen and low C
requires an additional set-up of the steel chemical composition in order to increase the SFE and improve
the austenite stability during deformation. This grade could be interesting for a significantly lower
carbides precipitation in the range 500-600C. The results achieved in the project allowed to define the
suitable manufacturing route to produce the TWIP steel. Concerning the strip annealing process the
avoidance of strip surface decarburization was stressed. This means that a proper atmosphere control
during annealing at high temperature must be taken. Even if a technical work relevant to the feasibility
study has been carried out, due to the steel market crisis, the proposed industrial TWIP steel heats was
not carried out for two main reasons: too much increased time and costs for installation of a vacuum
degassing facility (VD), compared to the RFCS scheduled duration of the project and the industrial
available resources, and the not completely in time explored comprehension of the process
(thermodynamical modellization and calculations) for the production of high Mn steel by direct current
electric furnace even with further expertise of external consultants.
The criticality of the industrial heat is at least in part balanced by an indepth not foreseen work aimed
on focus to theroretical (diffusion evaluation inside austenitic lattice steel) and experimental (tensile
tests on hydrogen charged specimens, TDA) study on the hydrogen embrittlement for TWIP steel and at
the same time a not foreseen work done on the decarburization effect of TWIP tensile properties during
the annealing step of the production process.



145

Exploitation and impact of the research results
The present project consisted in the metallurgically based design of TWIP steels assuming as main key
parameters the stacking fault energy (SFE) and the austenite stability. The performances of the TWIP
variants studied, reveal that also small difference in chemical composition yield to quite different
proprierties in terms of deformation mechanisms and austenite stability.
The approach used and the quite large amount of results gathered, among which data on
recrystallization behaviour, precipitation, tensile properties at low and high strain rate, high temperature
flow stress, will be useful to outline the guideline for design of TWIP steel manufacturing route.
For the development and application of high Mn steels a further continuation of the investigations on
hydrogen embrittlement of TWIP steels seems to be necessary. In particular the activities should be
focused on fracture mechanics tests to measure critical stress intensity factor, crack growth rate, delayed
failure tests and slow strain rate tests (SSRT). Fundamental aspects concerning the main trapping sites
of diffusible hydrogen and activation energies for its desorption, and thermal desorption analysis
(TDA), has to be clarified. Similarly the effect of process conditions (for example annealing,
galvanization) on embrittlement of TWIP steel has to be investigated. Another field of investigation
completely lacking at moment is represented by characterization of creep behaviour of TWIP steel. This
investigation could open new applications fields for TWIP steels.
The investigated TWIP steel have shown excellent tensile properties that could open new innovative
application fields in addition to utilize them as extremely attractive for automobile, even for the positive
strain rate sensitivity make TWIP steels suitable for applications devoted to energy absorption
(crashworthiness) and for structural reinforcement as for body in white.
New activities could be therefore directed, to fill up an existing gap in particular for the automotive
industry, on an innovative metallurgically based design of TWIP steel, on a dedicated manufacturing
route, to obtain a new product combining high-strength, improved crash resistence and reduction of gas
emissions through lightweighting.
The following pubblications were carried out using the results achieved in the present project:
1) Fatigue Behavior of four high-Mn TWIP steels, Metallurgical and Materials Transactions A, 41A,
2010, 1102-1108.
2) Fatigue behavior of high-Mn TWIP steels, Materials Science and Engineering A, 517, 2009, 68-77.
3) High-Cycle Fatigue Behavior of Ultrafine-Grained Austenitic Stainless and TWIP steels, submitted
to Materials Science and Engineering A.
4)Kinetics of recrystallization and grain growth of cold rolled TWIP steel, Advanced Materials
Research Vols. 89-91 (2010) pp 153-158
5) Fatigue Behavior of Four High-Mn Twinning Induced Plasticity Effect Steels, 1102VOLUME
41A, MAY 2010 METALLURGICAL AND MATERIALS TRANSACTIONS A.
6) J avier Gil Sevillano, An alternative model for the strain hardening of FCC alloys
that twin, validated for twinning-induced plasticity steel, Scripta Materialia, 60 (2009) 336-339.
7) Kinetics of recrystallization and grain growth of cold rolled TWIP steel, Advanced Materials
Research, 89-91 (2010) 153-158
8) Hall-Petch relationship of a TWIP steel, Key Engineering Materials, 423 (2010) 147-152.
9) F. de las Cuevas, M. Reis, A. Ferraiuolo, G. Pratolongo, L.P.Karjalainen, J . Alkorta, J . Gil Sevillano,
Efecto Hall-Petch en un acero TWIP, XI Congreso Nacional de Propiedades Mecnicas de los
Slidos PMS2008, Cdiz, Spain, 2008.
10) F. de las Cuevas, a, M. Reis, A. Ferraiuolo, G. Pratolongo, L.P. Karjalainen, V. Garca Navas, J . Gil
Sevillano, Kinetics of recrystallization and grain growth of cold rolled TWIP steel, THERMEC 09,
Berlin (Germany), 2009.


List of figures and tables
WP1: Testing material supply and basic metallurgical characterisation of cast materials
Fig.1.2.1.1: CSM VIM facility.



146

Fig. 1.3.1: Images of TWIP1 ingot. a) Macrostructure of the TWIP1 ingot sample, polished and Nital
2% etched b) SEM image of structure 2% Nital etch.
Fig. 1.3.2: a) Optical microstructures of TWIP1 in the cast state of lathy (black) and vermicular ferrite;
b) XRD of TWIP-1 in the cast state showing the presence of duplex structure.
Fig. 1.3.3: The element distribution (X-ray map) in the austenite and ferrite phases in cast TWIP1, (a)
SEM image, (b) Al distribution, and (c) Mn distribution.
Fig. 1.3.4: Isothermal cross-sections of Fe-Mn-Al system. (a) 1200C, (b) 1000C [2].
Fig. 1.3.5: SEM-EDS analysis locations on the cast TWIP1.
Fig.1.3.6: OM photo of the microstructure of the cast TWIP2.
Fig. 1.3.7: Presence of alfa-martensite in the cast TWIP3.
Fig. 1.3.8: OM photo of TWIP4 in the cast state.
Fig. 1.3.9: OM photos of the microstructure of the cast TWIP-5.
WP2: Fundamental investigations on the physical metallurgy of TWIP steels
Fig 2.1.1.1: TWIP2 microstructure after annealing treatments at 1000Cx5 min (average grain size 32
m).
Fig. 2.1.1.2: Extended nodes detected on a TWIP2 sample.
Fig. 2.1.2.1: Measure of hcp-martensite fraction on sample deformed at 0.30 at low temperature.
Fig. 2.2.1.1: Schedule used in double-hit compression tests.
Fig. 2.2.1.2: SEM-EBSD photo of TWIP-2 steel as heated at 1200C for 2 min and water quenched.
Red lines reveal high-angle (>15) grain boundaries.
Fig. 2.2.1.3: Typical true stress-strain curves of TWIP-2 (Fe-22Mn-0.6C) steel at high temperatures and
constant strain rate of 0.1 s
-1
. Curves for the low-carbon steel are included for comparison.
constant strain rate of 0.1 s
-1
. Curves for the low-carbon steel are included for comparison.
Fig. 2.2.1.4: Dependence of peak stress (
p
) and peak strain (
p
) on the inverse temperature at the strain
rate of 0.1 s
-1
for TWIP-2 and low-C steels.
Fig. 2.2.1.5: Plot of ln(
p
) vs ln Z for the low-C and TWIP-2 (22Mn-0.6C) steels.
Fig. 2.2.1.6: SRX rates of TWIP-2 at constant strain rate of 0.1 s
-1
. Double-hit compression data and
fitted curves. Times for 50% recrystallization, t
50
, and the Avrami exponents are listed.
Fig. 2.2.7: Typical true stress-strain curves of TWIP-3 (Fe-18Mn-0.6C-0.02Nb) steel at high
temperatures and the constant strain rate of 0.1 s
-1
. A curve for Fe-26Mn-0.14C steel is included for
comparison.
Fig. 2.2.1.8: SRX of TWIP-3 (0.2 strain at constant strain rate 0.1 s
-1
). Double compression data and
fitted curves.
Fig. 2.2.1.9: SRX of TWIP-3 determined in a relaxation test at 1000C/0.2/0.1 s
-1
.
Fig. 2.2.1.10: Typical true stress-strain curves of TWIP-4 (Fe-16Mn-1.5Al-0.3C) at the constant strain
rate of 0.1 s
-1
. Flow stress curves for 25Mn1Al [9] steel are included for comparison.
Fig. 2.2.1.11: SRX rates of TWIP-4 at the constant strain rate of 0.1 s
-1
. Double-hit compression data
and fitted curves. Data for 25Mn1Al at 1000C from [9].
Fig. 2.2.1.12: True stress-strain curves of TWIP-5 (Fe-22Mn-0.2C-0.2N) steel at high temperatures and
at the constant strain rate of 0.1 s
-1
. Curve for TWIP-2 (Fe-22Mn-0.6C) is included for comparison.
Fig. 2.2.1.13: SRX of TWIP-5 at the constant strain rate of 0.1 s
-1
. Double-hit compression data and
fitted curves.
Fig. 2.2.1.14: SRX rates (strain 0.2, strain rate 0.1 s
-1
) for the 25Mn1Al steel. Double-hit compression
data and fitted curves.
Fig. 2.2.1.15: Comparison of SRX kinetics of 25Mn1Al to low-carbon, Nb and Type 304 steels. Data
for the Nb-steel from [2].
Fig. 2.2.1.16: Plot of t
50
vs strain to calculate
Fig. 2.2.1.17: Plot of t
50
vs strain to calculate the power of strain for 25Mn1Al.
Fig. 2.2.1.18: Time t
50
of SRX for 25Mn1Al vs the inverse absolute temperature.
Fig. 2.2.2.1: OIM image of hot rolled TWIP2 sample (inverse pole figure and grain maps, rolling plane
normal



147

Fig. 2.2.2.2: Hall-Petch plot relationship for TWIP 2 steel with composition 22% Mn- 0.6% C, of the
hardness, H, as a function of the inverse of the square root of the grain size, D, for structures after fully
recrystallization or after fully recrystallization and grain growth. The grain size was determined as the
mean linear intercept using EBSP-OIM images, counting both, twin boundaries together with other
high-angle boundaries with misorientation higher of 12.
Fig. 2.2.2.3: Recrystallization kinetics for all reductions derived from the softening by annealing
temperature of 700C as function of time. TWIP 2 steel with composition 22% Mn- 0.6% C
Fig. 2.2.2.4: Grain growth equation. D* is calculated from mean linear intercept method, twin
boundaries not counted as grain boundaries. TWIP 2 steel with composition 22% Mn- 0.6% C.
Fig.2.2.2.5 Macro-textures, pole figures.a) TWIP steel 60% cold rolled with the typical brass-type
texture {011}<211>.b) Recrystallization texture, D 2 m.c) Grain growth texture with D 9 m.
Fig. 2.2.3.1: Comparison of model 1 (black line) with experimental data for a cold reduction of 60%
with an annealing temperature of 600C.
Fig. 2.2.3.2: Comparison of model 2 (red line) with (corrected) experimental data for a cold reduction
of 60% with an annealing temperature of 600C.
Fig. 2.2.3.3: Comparison of model 3 (blue line) with (corrected) experimental data for a cold reduction
of 60% with an annealing temperature of 600C.
Fig. 2.2.3.4: Comparison of model 3 with a range of experimental data, for a constant annealing
temperature of 600C. A) 40% reduction B) 50% reduction C) 60% reduction and D) 70% reduction.
Fig.2.3.1: Microstructure of the TWIP variant after soaking at 800C for 10h.
Fig. 2.3.2: TWIP1 - 700Cx10h
Fig. 2.3.3: SEM image of the TWIP2 sample after soaking at 700C for 10h
Fig. 2.3.4: SEM image of the TWIP3 sample after soaking at 700C for 10h.
Fig. 2.3.5: SEM image of the TWIP2 sample after soaking at 600C for 10h.
Fig. 2.3.6: TWIP3: SEM +EDS image of the cementite precipitated on the austenitic grain boundaries
after a soaking at 600C for 10h.
Fig. 2.3.7: TWIP4 at 700C: within some grains is detected a precipitation of ferrite +carbides
Fig. 2.3.8: SEM +EDS image of the TWIP 4 samples after a soaking at 600C for 10h.
Fig. 2.3.9: SEM +EDS image of the TWIP 4 samples after a soaking at 500C for 10h.
Fig. 2.3.10: TWIP 5 specimen after soaking for 10h at 500C
Fig. 2.3.11: TWIP1-700C: Low magnification image
Fig. 2.3.12: TWIP1-700C: Carbide of cementite type (FeMn)
3
C, the analysis is reported in fig. 2.3.11.
Fig. 2.3.13: (Fe,Mn)
3
C carbide image with relevant diffraction
Fig. 2.3.14: Vanadium carbo-nitride image with relevant diffraction.
Fig. 2.3.15: Nb content of the precipitates selected on extraction replica.
Fig. 2.3.16: TWIP3 600C: (Fe,Mn)
3
C carbide image
Fig. 2.3.17: TWIP5 at 700Cx10h - (Ti, Al) carbo-nitrides
Fig. 2.4.1: Typical slab temperature in conventional route.
Fig. 2.4.2: Typical slab cooling evolution adopting the hot charge route (piling up in a box).
Fig 2.4.3: Comparison of the MFS of TWIP2 and a conventional low-C steel.
Fig 2.4.4: TWIP1 scale analysis Fig 2.4.7 TWIP4 scale analysis
Fig 2.4.5: TWIP4 scale analysis
Fig. 2.4.6: Scale microstructure and main phases detected on: a) TWIP2 and; b) TWIP3 steel samples.
Fig. 2.4.7: Scale microstructure and main phases detected on TWIP5
WP3 Study of the deformation mechanisms and strain hardening behaviour
Fig. 3.1.1.1a): tensile tests results carried out at room temperature and higher temperature 150-350C.
Fig. 3.1.1.1b): tensile tests results carried out at room temperature and higher temperature 150-350C.
Fig. 3.1.1.2: The strain rate sensitivity of the five TWIP steel grades was evaluated collecting all the
data, torsion, tensile tests and Hopkinson bar tests as well.
Fig. 3.1.1.3: Calculated work hardening curves for each TWIP grade.
Fig. 3.1.1.4: True stress-true strain curves for TWIP3-4.



148

Fig. 3.1.1.4: TWIP 2 x500 a) head region etchant I, b) strain =0.4, etchant I
Fig. 3.1.1.5: TWIP 3 x500 a) head region etchant I, b) strain =0.4, etchant I.
Fig. 3.1.1.6: TWIP 4 x500 a) head region (strain=0) etchant I, b) strain =0.4 etchant II.
Fig. 3.1.1.7: TWIP 5 x500 a) head region etchant I, b) strain =0.4 etchant II.
Fig. 3.1.1.8: Calculated volume fractions of constituents in TWIP steels during tensile straining. A)
TWIP 1, B) TWIP 2, C) TWIP 3, D) TWIP 4 and E) TWIP 5.
Fig. 3.1.1.9: Ferritoscope measurements of
bcc
martensite on strained TWIP steels samples
(deformation 10%).
Fig. 3.1.1.10: Ferritoscope measurements of
bcc
martensite on strained TWIP steels samples
(deformation 30%).
Fig 3.1.1.11: TWIP1: deformed at 250C (strain 0.3 - strain rate =0.01).
Fig.3.1.1.12: TWIP3: microstructure deformed at: a) 250C; and b) 350C (strain 0.3 - strain rate =
0.01).
Fig.3.1.1.13: TWIP4: deformed structure at: a) 250C; b) 350C (strain 0.3).
Fig.3.1.1.14: TWIP5: deformed at 250C (strain 0.3 - strain rate =0.01).
Fig. 3.1.1.3.1a): Longitudinal cross section of a TWIP3 tensile specimen close the fracture surface.
Fig. 3.1.1.3.1b): Subsurface microstructure after tensile test (TWIP3) Klem II etching
Fig. 3.1.1.3.2: TWIP2 microstructure after annealing at 1000C x 300s
Fig. 3.1.1.3.3: TWIP2 microstructure after annealing at 1200C x 1100s.
Fig. 3.1.1.3.4: Comparison of the decarburization depth of TWIP steels and C45 steels at 1000C and
1200C.
Fig. 3.1.1.3.5: GDOES Carbon and manganese concentration profiles on TWIP2,3,4.
Fig. 3.1.1.3.6: Tensile test curve of hydrogen charged TWIP3 sample.
Fig. 3.1.1.3.7: Results of tensile tests carried out on sample with different hydrogen content.
Fig. 3.1.1.3.8: DTA plot on blank and hydrogen pre-charged sample.
Fig. 3.1.2.1a): Comparison between the quasi-static mechanical properties, yield strength R
p0.2
, tensile
strength R
m
, and fracture elongation A of the present TWIP steels [15] and those of TRIP700, DP600
and H340LAD [17] at RT (the strain rate 10
-3
s
-1
).
Fig. 3.1.2.1 b): Comparison between the dynamic mechanical properties, yield strength R
p0.2
, tensile
strength R
m
, and fracture elongation A of the present TWIP steels and those of TRIP700, DP600 and
H340LAD [17] at RT (the strain rate of order of 10
3
s
-1
).
Fig. 3.1.2.2: Comparison between the stress ratio in quasi-static and dynamic tensile tests of the present
TWIP steels and those of TRIP700, DP600 and H340LAD [17].
Fig. 3.1.2.3: Strain-hardening coefficient (n-value) from the Hollomon equation vs. true plastic strain
for TWIP2 tested at 1210 s
-1
and RT.
Fig. 3.1.3.1: Torsion shear stress-plastic shear strain curves at = 1.410
-3
s
-1
and corresponding
Kocks-Mecking plots (strain rate vs. flow stress).
Fig. 3.1.3.2: Torsion shear stress-plastic shear strain curves at = 0.113 s
-1
and corresponding Kocks-
Mecking plots (strain rate vs. flow stress).
Fig. 3.1.3.3: Torsion shear stress-plastic shear strain curves at = 3.73 s
-1
and corresponding Kocks-
Mecking plots (strain rate vs. flow stress).
Fig. 3.1.3.4: Torsion shear stress for three shear strain levels, 0.173, 0.520 and 1.040, as a function of
temperature, for the three strain rates tested (TWIP2, TWIP3).
Fig. 3.1.3.5. Torsion shear stress for three shear strain levels, 0.173, 0.520 and 1.040, as a function of
temperature, for the three strain rates tested (TWIP4, TWIP5).
Fig. 3.1.3.6: TWIP steels, maximum shear stress in torsion as a function of temperature for different
strain rates.
Fig. 3.1.3.7: Torsion shear failure strain of the four TWIP steels as a function of temperature and strain
rate.
Fig. 3.1.4.1: Hot ductility curve for TWIP1 (Fe-22Mn-3Al-3Si).
Fig. 3.1.4.2: Hot ductility curve of TWIP2. Curve of AISI 304 is included for comparison.



149

Fig. 3.1.4.3: Hot ductility curve of TWIP3. Curve of TWIP2 is included for comparison.
Fig. 3.1.4.4: Hot ductility curve of TWIP4. Curve of TWIP2 is included for comparison.
Fig. 3.1.4.5: Hot ductility curve of TWIP5. Curve of TWIP2 is included for comparison.
Fig. 3.1.5.1: Hall-Petch plot of the tensile yield stress at 10
-3
s
-1
(flow stress for 0.002 tensile plastic
strain) of steel TWIP1 and TWIP2.
Fig. 3.1.5.2: Hall-Petch slopes for the flow stress at fixed true plastic tensile strain values, steels TWIP1
and TWIP3 as a function of plastic true tensile strain, up to =0.15.
Fig. 3.1.5.3: Hall-Petch slopes of steel TWIP2 at room temperature and three tensile strain rates, as a
function of tensile plastic strain.
Fig. 3.1.5.4: Work hardening rate vs. true flow stress of the TWIP 2 steel with composition 22% Mn-
0.6% C. Tensile tests at room temperature and 10
-3
s
-1
for a equiaxed grain size in the range 1.5 m <D
<50 m.
Fig. 3.1.5.5a: D
*
grain size (mean linear intercept) without considering twin boundaries .
Fig. 3.1.5.5b: D id., with twin boundaries counted as grain boundaries.
Fig. 3.1.5.6. Twin Boundary Fraction vs. Grain size D
*
(twin boundaries not counted).
Fig. 3.2.1. S-N curves of the investigated TWIP steels and those of 301LN and 316L and high-strength
TRIP steel are included for comparison [1,2].
Fig. 3.2.2: The final fatigued structure of TWIP (Fe-22Mn-0.6C) steel after failure.
Fig. 3.2.3: Effect of the grain size on the fatigue life of the TWIP steel (Fe-22Mn-0.6C). All tests were
carried out at the amplitude of 500 MPa.
Fig. 3.3.1: Charpy tests results for the five TWIP compositions.
Fig. 3.4.1: Plain strain compression tests results on TWIP2 variant.
WP 4 Basic characterisation of application properties: formability, weldability and coating
ability
Fig. 4.1.1.1 Graphic representation of the Erichesen tests results for the five TWIP compositions.
Fig. 4.1.2.1 - Comparison between the Erichsen index (IE) in high-speed (and conventional) testing and
the total elongation (A) from quasi-static tensile tests [3] and that of AISI 304 [5].
Fig. 4.2.1: Sample TWIP 2 DM .
Fig. 4.2.2: Sample TWIP 2 DQ.
Fig. 4.2.3: Sample TWIP 5 DM (200X).
Fig. 4.2.4: Sample TWIP 2 DM (200X).
Fig. 4.2.5: Sample TWIP 2 DQ (500X).
Fig. 4.2.6: Sample TWIP 5 DM (200X).
Fig. 4.2.7: Sample TWIP 5 DQ (500X).
Fig. 4.3.1: Visual observation of the front surface of the TWIP3 diode laser weld.
Fig. 4.3.2: Visual observation of the root surface of the TWIP3 diode laser weld
Fig. 4.3.3: Low-magnification light optical micrograph from TWIP2 steel showing a cross section of the
welded joint
Fig. 4.3.4: Low-magnification light optical micrograph from TWIP3 steel showing a cross section of the
welded joint
Fig. 4.3.5: Low-magnification light optical micrograph from TWIP4 steel showing a cross section of the
welded joint
Fig. 4.3.6: Micrography of TWIP2 steel base material (500X).
Fig. 4.3.7: Micrography of TWIP3 welded sample showing the transition base material- welded
material (200X).
Fig. 4.3.8: Micrography of TWIP3 welded joint (200X).
Fig. 4.3.9: Micrography of TWIP2 welded material showing the presence of -martensite (200X).
Fig. 4.3.10: Vickers hardness measurements
Fig. 4.3.11: Docol 800DP steel microstructure taken in a scanning microscope (X500).
Fig. 4.3.12: Tailored blank weld configuration used in the welding tests.
Fig. 4.3.13: Visual observation of the front surface of the TWIP4 Docol 600DP CO
2
laser weld.



150

Fig. 4.3.14: Low-magnification light optical micrograph showing a cross section of the welded joint -
TWIP2 and Docol 600DP steels
Fig. 4.3.15: Low-magnification light optical micrograph showing a cross section of the welded joint -
TWIP2 and Docol 800DP steels.
Fig. 4.3.16: Low-magnification light optical micrograph showing a cross section of the welded
Fig. 4.3.17: Low-magnification light optical micrograph showing a cross section of the welded joint -
TWIP3 and Docol 600DP steels.
Fig. 4.3.18: Hardness distribution curve of a Docol 800 DP laser weld Figure 4.3.21 Low-
magnification light optical micrograph showing a cross section of the welded joint - TWIP3 and Docol
600DP steels.
Fig. 4.3.19: Graphic representation of the hardness measurements performed on the TWIP 2 DOCOL
600DP weld.
Fig. 4.3.20: Graphic representation of the hardness measurements performed on the TWIP 2 DOCOL
800DP weld.
Fig. 4.3.21: Graphic representation of the hardness measurements performed on the TWIP 4 DOCOL
600DP weld.
Fig. 4.3.22: Graphic representation of the hardness measurements performed on the TWIP 4 DOCOL
800DP weld.
Fig. 4.3.23: Graphic representation of the hardness measurements performed on the TWIP 5 DOCOL
600DP weld.
Fig. 4.3.24: Graphic representation of the hardness measurements performed on the TWIP 5 DOCOL
800DP weld.
Fig. 4.3.25: Graphic representation of all the hardness measurements performed on Docol 600DP steel
welds.
Fig. 4.3.26: Graphic representation of all the hardness measurements performed on Docol 800DP steel
welds
WP5 Industrial trial
Fig. 5.2.1 Typical kinetics of hydrogen removal curve during a VD process using different Argon
pressure.
Fig. 5.2.2: Fe-Mn diagram phase

List of table
WP1 table
Table 1.1.1.1 Selected TWIP steel compositions (Fe balance).
Table 1.1.2.1: Numerical values and functions used for the calculations of SFE in two models
Table 1.1.2.2: Calculated SFE for TWIP steels at 298 K.
Table 1.2.1.1 Ingots chemical analysis.
Table 1.3.1: Partition ratios PD of alloying elements between austenite and ferrite in TWIP 1.
Table 1.3.2: Tsolidus and Tliquidus of TWIP steels.
Table 1.3.3 Ingots chemical analysis.
WP2 table
Table 2.1.1.1: SFE results achieved on TWIP 2
Table 2.1.1.2: Model parameters for calculation of SFE in Dumay et al model [4].
Table 2.1.1.3: Calculated SFE for TWIP steels at 298 K.
Table 2.1.2.1: Md30

evaluation from fig.2.1.2.2.


Table 2.2.1.1: Peak stress at 1000C of different TWIP steels.
Table 2.2.1.2: Values of t50 at 1000C and 1100C relevant to TWIP steels variants.
Table 2.2.2.1. Annealing treatments
Table 2.2.2.2. Values of ksoft and B obtained from Avrami fittings to the recrystallization results
obtained for different reductions and annealing temperatures.
Table 2.2.2.3. Annealing processes map of the TWIP steel in T-t space. Not explored regions in blank.



151

Table 2.3.1: thermal treatments for precipitation study.
Table 2.4.1: Bending after a sag test with 3h soaking at 1200C.
Table 2.4.2: Calculated T
solidus
and T
liquidus
of TWIP steels.
Table 2.4.3: HRM Rolling schedule - TWIP 22Mn 0.6C steel- slab format 1000x250x28 mm
Table 2.4.4: Calculated TWIP steel finishing rolling schedule for strip format: 1000x28x4 mm.
Table 2.4.5: Results of the pickling tests.
WP3 table
Table 3.1.1.1: Tensile test at 20C results (cold rolled and annealed at 1000Cx5min)
Table 3.1.1.2: Tensile test results at different temperature with mechanically polished surface
Table 3.1.1.3: Values of physical parameters used in modelling
Table 3.1.1.4: Obtained model fitting parameters
Table 3.1.1.5: Microstructural constituents/phases before and after testing of TWIP steels at room
temperature.
Table 3.1.1.6 Mechanical twins occurrence during deformation at high temperature (strain rate 0.01s
-1
)
Table 3.1.1.3.1: Annealing tests carried out to study the strip surface decarburization.
Table 3.1.1.3.2: Comparison of Vickers hardness (HV200g) average values on bulk and decarburized
zone.
Table 3.1.1.3.3
Table 3.1.1.3.4 Low strain rate tensile tests reference and hydrogen charged TWIP3 sample.
Table 3.1.1.3.5 LECO RC-412 main features.
Table 3.1.5: TWIP2, numerical results of tensile tests.
Table 3.3.1 Charpy tests results.
Table 3.4.1: Stress after a true strain of 0.5
WP4 Table
Table 4.1.1.1 Erichsen tests results.
Table 4.1.1.2 Erichsen testing parameters.
Table 4.1.1.3 Characteristics of the TWIP_1 (Fe-22Mn-3Al-3Si) samples
Table 4.1.1.4 Results of conventional Erichsen tests performed at ISQ.
Table 4.1.1.5 Characters of the TWIP_2 samples after the high-speed Erichsen tests.
Table 4.1.1.6 Characteristics of the TWIP_3 samples after the high-speed Erichsen tests.
Table 4.1.1.7 Characteristics of the TWIP_4 specimens after the high-speed Erichsen tests.
Table 4.1.1.9 Hardness (HV5) of the TWIP steels before and after high-speed Erichsen testing.
Table 4.2.1 Thickness of coating layers.
Table 4.2.2 EDS analysis.
Table 4.3.1 Optimal laser welding parameters for each TWIP steel composition
Table 4.3.2 ASTM grain size measurements using the circular interception technique according with the
ASTM E 112 standard.
Table 4.3.3 Docol DP chemical composition.
Table 4.3.4 Docol DP mechanical properties.
WP5: Table
Table 5.1.1: TWIP compositions investigated in the metaldesign project.
Table 5.1.2 Range of elements for TWIP3 steel grade to be cast at Duferco steelworks.

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8. Frommeyer, G., Brx, U. and Neumann, P., ISIJ Int., 3, 438 (2003).
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Dformation et dcrouissage dAciers Austnitiques Haute teneur en Manganse Application
lEffet TWIP . Doctoral thesis, INPL, cole des Mines de Nancy, France (2004).
10. Allain, S., Chateau, J . P., Dahmoun, D. and Bouaziz, O., Mater. Sci. Eng. A, 387-389, 272 (2004).
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Analysis. Doctoral Thesis, Katholieke Universiteit Leuven (Belgium), 2004.
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14. Krger, L., Halle, Th., Meyer, L. W., Brx, U. and Frommeyer, G., Mat.-wiss. U. Werkstofftech.,
35, 299 (2005).
15. Cornette, D., Cugy, P., Hildebrand, A. Bouzekri, M and Lovato, Rev. Mtall.-CIT, 102, 905 (2005).
16. Scott, C., Allain, S., Faral, M. and Guelton, N., Rev. Mtallurgie-CIT, 103, 293 (2006).
17. Humphreys, F. J . and Hatherly, M., Recrystallization and Related Annealing Phenomena, 2nd
ed., Elsevier, Amsterdam, 2004.



154

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Task 2.3
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Task 3.1.1
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3. S C MITTAl, ISIJ International. Vol. 35 (1995). No. 3, pp. 302 308



155

4. Hydrogen Delayed Fracture Properties and Internal Hydrogen Behavior of a Fe18Mn1.5Al0.6C
TWIP Steel, Kyoung Ho SO, ISIJ International, Vol. 49 (2009), No. 12, pp. 19521959.
Task 3.2
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Report No. 64 (1995), p. 20
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(2004), p. 331
4. Information on http://www.outokumpu.com/files/Group/HR/Documents/Fatigueproperties.pdf
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6. H-P. Heikkinen, Master's thesis, University of Oulu, Finland, 2008.
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8. O. Grssel, L. Kruger, G. Frommeyer and L.W. Meyer, Int. J . Plast., 16 (2000), 1391-1409.













European Commission
EUR 25063 Metallurgical design of high-strength austenitic Fe-C-Mn steels with
excellent formability (METALDESIGN)
A. Ferraiuolo, A. Smith, J. G. Sevillano, F. de las Cuevas, P. Karjalainen, G. Pratolongo,
H. Gouveia, M. Mendes Rodrigues
Luxembourg: Publications Office of the European Union
2012 155 pp. 21 29.7 cm
Research Fund for Coal and Steel series
ISBN 978-92-79-22205-4
doi:10.2777/14874
ISSN 1831-9424
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Five TWIP steel grades (Fe-Mn-C-N and Fe-Mn-Al-Si-C) were selected, adopting stack-
ing fault energy (SFE) and austenite phase stability as the main metallurgical character-
istics for alloy design. The selected TWIP grades were characterised in terms of SFE,
mechanical properties, microstructure, recrystallisation, welding and forming ability.
The performance analysis revealed that only TWIP2 and TWIP3 clearly behave as
expected from TWIP steels, with the typical hardening stage associated with profuse
deformation twinning. The variants with lower Mn and C content (TWIP1, TWIP4, TWIP5)
require a further set-up of steel chemistry to better balance the SFE and avoid the for-
mation of second phases (ferrite or deformation-induced martensitic phases). The results
achieved in the project allowed to define the suitable industrial manufacturing route to
produce the TWIP steel. However two main issues resulted with an importance stronger
than expected in the technical annex: hydrogen embrittlement susceptibility and strip
surface decarburization. The first issue has suggested to delay the industrial heat sched-
uling to evaluate the risk of hydrogen embrittlement for TWIP steels and the need to
include a vacuum degassing facility for industrial TWIP steel manufacturing. The decar-
burization issue revealed that during the annealing process a proper atmosphere control
is necessary to avoid within the decarburised layer the formation of deformation induced
martensitic phases (+).The activity results revealed that the investigated TWIP steels
have excellent tensile properties together with good welding and galvanising ability that
make them extremely attractive for automotive applications both for structural reinforce-
ment (body in white) and for energy absorption.