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Abstract
Thermal fatigue cracking is an important life-limiting failure mechanism in die casting tools. It is observed as a network of fine cracks on
the surfaces exposed to thermal cycling. The crack network degrades the surface quality of the tool and, consequently, the surface of the
casting. Surface engineered materials are today successfully applied to improve the erosion and corrosion resistance. However, their
resistance against thermal fatigue is not fully explored.
In this work, a selection of hot work tool steel grades was surface modified and experimentally evaluated in a dedicated thermal fatigue
simulation test. The surface modifications included boriding, nitriding, Toyota diffusion (CrC), and physical vapour deposition (PVD) of
coatings (CrC, CrN and TiAlN), both as single-layers and deposited after nitriding (duplex treatment). Untreated specimens of each tool steel
grade were used as references. The test is based on cyclic induction heating and internal cooling of hollow cylindrical test rods. The surface
strain is continuously recorded through a non-contact laser speckle technique.
Generally, all surface treatments decreased the resistance against surface cracking as compared to the reference materials. The reason is
that the engineering processes influence negatively on the mechanical properties of the tool materials. Of the processes evaluated, duplex
treatment was the least destructive. It gave a lower crack density than the reference steel, but the diffusion layer is more susceptible to crack
propagation. In addition, the single-layered CrN coating showed almost comparable thermal fatigue cracking resistance as the reference
material. Finally, the resistance against thermal crack propagation of surface engineered tool steels is primarily determined by the mechanical
properties of the substrate material.
D 2004 Published by Elsevier B.V.
Keywords: Thermal fatigue; Heat checking; Surface strain; Surface engineering; Hot work tool steel; Die casting
1. Introduction
In die casting, molten metal of e.g. aluminium, zinc,
magnesium, and copper based alloys is forced by the
application of pressure to flow with high velocity during
injection and completely and rapidly fill an internally cooled
mould, typically within the order of milliseconds [1 3]. The
high melt velocity during injection and the continuos
internal cooling of the tool during the process allow production of thin-walled and complex near net-shaped cast
products at high manufacturing rates, typically of the order
of 100 castings per hour. When the casting has solidified,
the die is opened and the casting ejected. Subsequently, the
tool surfaces may be externally cooled and lubricated by
2. Experimental
2.1. Materials and characterisation
Three Uddeholm hot work tool steels, Orvar Supreme
(premium AISI H13 grade), QRO 90 Supreme and Hotvar,
were used as test material. Their nominal chemical compositions, and hardening (austenitizing, followed by air
quenching) and tempering treatment are given in Table 1.
The austenitizing treatment gives a nominal austenite grain
size of about ASTM 10 for Orvar, and about ASTM 9 for
QRO 90 and Hotvar. All heat treatments resulted in different
microstructures of tempered martensite. The heat treatments
were followed by grinding to a surface roughness (Ra) of
0.38 F 0.05 Am, as obtained by optical surface profilometry.
The Orvar specimens were further ground and polished with
1-Am diamond paste in a last step to a surface roughness
(Ra) of 20 F 14 nm. Test specimens of each tool steel grade
of these conditions were used as references, denoted Orvar,
QRO 90, and Hotvar, respectively.
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Table 1
Nominal chemical compositions in wt.% and austenitizing (A) and
tempering (T) treatments of the tool steels
Steel grade
Si
Mn
Cr Mo
A
T
[jC/min] [jC/h]
QRO 90 Supreme 0.38 0.30 0.75 2.6 2.25 0.9 1020/30 625/2 2
Orvar Supreme
0.39 1.0 0.4 5.2 1.4 0.9 1025/30 600/2 2
Hotvar
0.55 1.0 0.75 2.6 2.25 0.85 1050/30 575/2 2
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Table 2
Characteristics of the test materials, including deposition time and temperature during the boriding, TDP, and nitriding and/or PVD coating treatments
Denotation
Substrate
hardness
[HV 30 kgf]
Nitriding
hardness
[HV 25 gf]
Diffusion
depth [Am]
Coating
hardness
[HV 25 gf]
Coating
thickness
[Am]
QRO 90
Q-B
Q-TDP CrC
Q-CrN
Q-DCrN
Orvar
O-GN
O-DCrC
O-DTiAlN
Hotvar
H-GN
H-DCrC
H-DTiAlN
507 F 5
520 F 5
522 F 5
495 F 5
507 F 5
486 F 5
482 F 5
485 F 5
476 F 5
640 F 10
604 F 5
606 F 5
596 F 5
915 F 15
1030 F 30
955 F 30
975 F 30
955 F 20
845 F 25
910 F 25
30 F 2
30 F 2
160 F 3
250 F 15
120 F 10
115 F 10
295 F 5
175 F 10
170 F 10
1740 F 100
1970 F 70
2000 F 100
2060 F 100
1710 F 55
2285 F 170
1690 F 45
2275 F 200
6.1 F 0.1
4.5 F 0.2
5.5 F 0.4
5.5 F 0.7
3.8 F 0.1
2.9 F 0.1
f 25/ f 850
6/1030
/300 400
15/480, /300 400
48/510
/ f 480, /450 500
/ f 480, /450 500
48/510
/ f 480, /450 500
/ f 480, /450 500
a
Single time/temperature values refer to the single treatments, and double values refers to those for the duplex treatments (nitriding followed by PVD
coating).
mens treated by boriding, the surface hardness was measured below the compound layer.
2.2. Thermal fatigue testing
The test equipment is based on cyclic induction heating and internal cooling of hollow cylindrical test rods
with a diameter of 10 mm, a length of 80 mm, and
having a 3-mm axial hole for internal cooling. Surface
strain measurements through a non-contact laser speckle
technique make it possible to calculate the strains induced
in the specimen surface during thermal cycling. An
induction unit (25 kW, 3 MHz) heats the surface layer
of approximately 20 mm of the middle of the test rod.
Continuous cooling is performed by circulating silicon oil
(flow rate c 2.5 l/min) of 60 jC through the specimen,
and also externally with either argon (forced convection),
which also decreases oxidation during the thermal cycling, or air (natural convection).
Argon was used as cooling medium because the tools
are exposed to an environment with reduced oxygen
content during actual die casting. The oxygen in the die
cavity is partly consumed through oxidation of tool material and casting alloy. For the tests in argon, the specimen
was contained in a glass tube and argon was flowing
between the specimen and the glass tube wall. Unfortunately, this glass tube makes it impossible to obtain surface
strain recordings by the laser speckle technique. However,
the surface strains could be recorded during the first 100
cycles in a separate test series performed in air. More
information about this test method is presented elsewhere
[21].
Two temperature cycles were used to simulate aluminium
and brass die casting temperature conditions, see Table 3, in
the following, designated according to their maximum
temperatures, 700 and 850 jC, respectively. The latter
temperature corresponds to the maximum tool surface
temperature during actual brass die casting [22]. The thermal cycles included a steep ramp to the maximum temperature and subsequent cooling to the minimum temperature,
with or without a short holding time ( < 0.1 s) at the
maximum temperature.
Thermal cycling by induction heating above the Curie
transition temperature of Fe (768 jC) does not ideally
generate the temperature profile representative for die
casting of, e.g. brass [22]. Thus, the 850 jC heat cycle
is not as representative for die casting as that to 700 jC,
and only the reference specimens of QRO 90 and those
treated by boriding and TDP were tested to 850 jC. In the
following, only the surface strains for the 700 jC tests are
considered.
Prior to testing, the specimens were pre-oxidised in
order to get a thin oxide layer, which facilitates the
pyrometer temperature control during heating. The reference specimens were pre-oxidised by electrochemical
oxidation in a NaOH-solution at 70 jC for about 5
min, followed by 1-h heat treatment at 200 jC in air
[21]. All surface engineered specimens were pre-oxidised
0.5 h at 600 jC. This temperature, which is comparable
to the tool steel tempering temperature, and the relatively
short time were selected not to affect the mechanical
properties of the tool material. A previous study showed
that 20 000 thermal cycles to 600 jC did not affect the
mechanical properties of these tool steels [21]. A K-type
Chromel-Alumel thermocouple with thin wires (/ 0.13
Table 3
Thermal cycles used in the thermal fatigue tests
Maximum
temperature
[jC]
Minimum
temperature
[jC]
Heating
time [s]
Total cycle
time [s]
External
cooling
700
850
170
170
0.3 0.4
2.2 2.5
14.3 14.4
26.2 26.5
Argon or air
Argon or air
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2.3. Evaluation
During the heat cycling, the surface strain is continuously
obtained by the laser speckle technique from the change in the
specimen dimensions, and it is represented as surface strain vs.
temperature. Any thermal fatigue damage of the specimen
surface was revealed using scanning electron microscopy
(SEM). It was further characterised with respect to crack
growth (crack length vs. number of cycles) and crack density
(number of cracks per unit of length) by crack length measurements on polished axial cross-sections by LOM. All evaluations of cracks are based on cracks larger than about 5 Am,
detected along two lines, each of 8-mm length.
Hardness vs. depth profiles and relative coating hardness
after exposure to the heat cycling were assessed by microVickers indentations on polished cross-sections and directly
on the top of the surface of the coatings, respectively, using
a load of 25 g.
3. Results
3.1. Recorded surface strain during thermal cycling
Fig. 2. Typical surface cracking after 10 000 cycles to 700 jC in argon (QB, SEM).
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those of the reference material (see Fig. 1b). No remarkable differences among the tested materials were observed
during the initial 100 heat cycles recorded.
3.2. Surface cracking
Thermal fatigue cracking of a surface engineered tool
steel after thermal cycling to 700 jC is exemplified in Fig.
2. Polished cross-sections revealed that the crack path was
strongly dependent on the maximum temperature during
each cycle. Essentially two different types of crack paths
were distinguished. Relatively straight cracks dominated
Fig. 4. Maximum crack length (a), mean crack length (b), and crack density (c) after cycling to 700 and 850 jC, respectively, in argon. Each pile is the average
value of two to four specimens of each material, and the error bars indicate the maximum and minimum recording.
after heat cycling to 700 jC, cp. Fig. 3a. Both straight and
branched cracks (Fig. 3b) were observed after thermal
cycling to 850 jC.
3.2.1. Crack length and crack density of surface engineered
QRO 90
The crack length was strongly dependent on the number
of cycles and the maximum temperature during each cycle,
see Fig. 4. In addition, the crack density of each material
was almost constant or slightly increasing within the number of cycles tested, for the two maximum cycle temperatures. It is also seen that the crack length and density of
cracks differ significantly among the surface engineered
QRO 90 substrates.
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Fig. 5. Maximum crack length (a), mean crack length (b), and crack density (c) after cycling to 700 jC in argon. Each pile is the average value of two to four
specimens of each material, except that for O-TiAlN 10 000 cycles at 700 jC which is based on one specimen, and the error bars indicate the maximum and
minimum recording.
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Fig. 6. Surface hardness vs. depth for the tested materials. (a) QRO 90 systems, (b) Orvar systems, and (c) Hotvar systems after 10 000 cycles to 700 jC in
argon. (d) QRO 90 systems after 1000 cycles to 850 jC. The reference steels are included.
4. Discussion
4.1. Surface layer conditions during thermal cycling
Induction heating of steel using a frequency of 3 MHz
give rise to very fast heating of only a thin surface layer, of
the order of 10 Am (skin-effect). When applying this
method to the test rods, the thermal expansion of the surface
layer material is retained by the cooler bulk material, cp.
Fig. 1. During the initial cooling phase, the surface contracts
but the material below still expands due to heat conduction
and, thereby, the decrease in surface strain with temperature
is delayed, see Fig. 1.
4.1.1. Stresses in the surface layer
The fact that the thermal strain of the surface layer is
constrained during the thermal cycling exposes the surface
layer material to cyclic stresses. The hypothetical strains
corresponding to these stresses are defined as mechanical
strains emech. Crack nucleation and growth is determined by
fluctuations in emech. Similarly, thermal strains eth defined as
strains without any constraint are defined from the thermal
expansion coefficient of the material a(T) and the minimum
surface temperatures Tmin as:
eth T aT T Tmin
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Note that the surface layer conditions above are estimated without any knowledge of the temperature profile below
the surface.
From the surface strain recordings such as those of Fig.
1, and using Eqs. (1) and (2), the three types of surface
strains (i.e. etot, eth, and emech) during heat cycling can be
deduced, see Fig. 7. Similarly, these calculations give the
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Fig. 8. Hardness vs. depth for the reference tool steels after 10 000 cycles to
700 jC; constructed from Figs. 6a c.
Fig. 9. Maximum crack length vs. thickness of diffusion layer after thermal
cycling constructed using Table 2 and Figs. 4a and 5a. (a) 5000 and 500
cycles to 700 and 850 jC, respectively. (b) 10 000 and 1000 cycles to 700
and 850 jC, respectively. The solid lines are included to visualise any
correlation.
225
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5. Conclusions
In this study, a selection of hot work tool steel grades was
surface modified and experimentally evaluated in thermal
fatigue. The following conclusions can be made.
Fig. 10. Example of hardness vs. depth for duplex-treated materials after
10 000 cycles to 700 jC; constructed from Figs. 6a c.
Acknowledgements
The authors are grateful to Uddeholm Tooling AB, Tour
and Andersson AB, Bodycote Heat treatment AB, Balzers
Coating AB, and ABB Motors AB. The financial support
from the Swedish Knowledge Foundation is also acknowledged. Special thanks to Mrs. Anna Persson for all
valuable help with specimen preparation for light optical
microscopy.
References
[1] L.J.D. Sully, 9th ed., Metals Handbook vol. 15, ASM International,
Metals Park, OH, 1988, p. 286.
[2] J.R. Davis (Ed.), ASM Speciality Handbook, Tool Materials, ASM
International, Materials Park, Ohio, 1995, p. 251.
[3] D.F. Allsop, D. Kennedy, Pressure Diecasting, Part 2: The Technology of the Casting and the Die, Pergamon, Oxford, 1983.
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