Materials Science & Engineering A 673 (2016) 467–475

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Effects of tempering mode on the structural changes of martensite

D.C. Saha a,n, E. Biro b, A.P. Gerlich a, Y. Zhou a
a
Centre for Advanced Materials Joining, Department of Mechanical & Mechatronics Engineering, University of Waterloo, 200 University Avenue West,
Waterloo, Ontario, Canada N2L 3G1
b
ArcelorMittal Global Research, 1390 Burlington Street East, Hamilton, ON, Canada L8N 3J5

art ic l e i nf o a b s t r a c t

Article history: Tempered martensite obtained from four different tempering modes were characterized using trans-
Received 9 June 2016 mission electron microscopy, high-angle annular dark field scanning transmission electron microscopy,
Received in revised form and nanoindentation techniques. Crystallographic analysis of tempered martensite revealed that ferrite
20 July 2016
(α) and cementite (θ) obtained via furnace and Gleeble heat treatment obeyed the Isaichev orientation
Accepted 22 July 2016
̅ ]θ 0.91° from [111
(or close to it) with [311 ̅ ]α ||⎡⎣ 001⎤⎦ Bagaryatsky orientation relationship.
̅ ]α and the [ 112
Available online 25 July 2016 θ
A strict orientation relationship between ferrite and cementite could not be determined on the tempered
Keywords: structure extracted from the sub-critical heat affected zone of two different laser beam welded samples.
Martensite tempering Extensive recovery and reduction of boundary regions was identified on the structure tempered slowly,
Transmission electron microscopy
whereas rapidly tempered structures retained a high density of dislocation and less decomposition of the
Crystallography
lath structure. The relationship between dislocation density and modified tempering parameter was
Dislocation density
Nanoindentation determined and their contributions on tensile strength were evaluated.
Strength & 2016 Elsevier B.V. All rights reserved.

1. Introduction tempering applications. In rapid tempering, the tempering occurs

Tempering of martensitic steels is essential to suppress brittle
fracture and ensure a desired combination of strength and ducti-
lity. During tempering, the strength of martensitic steel decreases
due to ejection of carbon atoms from the carbon supersaturated
martensite phase [1]. Martensite tempering involves a series of
processes. In the first stage of tempering which occurs between
temperature 80–200 °C, the segregation and redistribution of
carbon atoms take place into lattice defects such as dislocations,
lath boundaries, and prior-γ grain boundaries. In addition, the
transitional epsilon-carbides (ε-Fe2.4C) also formed in this tem-
pering stage [2–4]. The interlath film like retained austenite de-
composes into ferrite (α) and cementite (θ-Fe3C) in the second
stage of tempering (200–300 °C). In the third stage of tempering,
segregated carbon and transitional carbides transform into stable
carbides such as cementite (Fe3C), which occurs at higher tem-
perature, in the range of 250–350 °C [4]. At temperatures above
350 °C, the cementite spheroidizes and coarsens [4]. There are
numerous factors which influence the martensite tempering pro-
cess, such as: tempering temperature [5,6], tempering time [5,6],
heating rate [7–9], and the steel chemistry [10,11]. Tempering is
used in variety of applications, these can be divided broadly into
rapid tempering applications and slow (or conventional)
n
Corresponding author.
E-mail address: dcsaha@uwaterloo.ca (D.C. Saha).
on the order of seconds or less. Industrial examples of rapid
tempering include: induction heating, laser heat treatment, and
tempered heat-affected zone (HAZ) transformations during
welding and joining [10–12]. Slow tempering is typically used in
furnace post weld heat treatments, and tempering parts made of
quench and temper steels. Tempering technique can also affect
process costs. For example, induction heating process is cost ef-
fective due to the shorter processing time [7,9,13,14]. On the other
hand, a conventional tempering cycle is used to obtain a desired
homogeneous microstructure with a uniform optimum mechan-
ical property [15]; therefore, the conventional furnace tempering
process is suitable for a large-scale component which requires
slow cooling to obtain a homogeneous microstructure.
Typical microstructural features such as crystal defect sites
(especially with high dislocation densities), lath sizes, and block or
packets sizes are influenced by the mode of heating and heating
rate. Hernandez et al. [10] studied the consequences of isothermal
and nonisothermal tempering process on dual-phase steel. They
reported that the nonisothermal process employed using a re-
sistance spot welder produces finer cementite and lesser recovery
in the ferrite structure compared to that obtained in a furnace heat
treatment (isothermal tempering) process. It has been also re-
ported that steel containing rich alloying elements such as Mn,
and Cr has higher resistance to softening compared to a lean Mn
and Cr containing steels [11].
The objective of the present study is to examine the tempered
structures of 0.24% C containing fully martensitic steel produced

http://dx.doi.org/10.1016/j.msea.2016.07.092
0921-5093/& 2016 Elsevier B.V. All rights reserved.
468 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475

with various tempering modes such as a furnace heat treatment

(FHT), Gleeble heat treatment (GHT), diode laser welding (DLW),
and fiber laser welding (FLW) via transmission electron micro-
scopy (TEM), high-angle annular dark-field scanning TEM (HAADF-
STEM) imaging, and nanoindentation study. Crystallographic
analysis using selected area diffraction (SAD) patterns and na-
noscale microstructure-properties correlations are evaluated. In
addition, the strength contribution from high dislocation densities
and precipitation are evaluated for the four tempering conditions
considered.

2. Experimental

A 1.20 mm thick 0.24% C containing fully martensitic steel were

used; the chemical compositions of the investigated steel is shown
in Table 1. In order to obtain various tempered structures, different
tempering methods were employed with different heating and
cooling rates, temperatures, and times (Fig. 1, and Table 2). To
produce a FHT sample, tempering was carried out in a muffle
furnace at 500 °C for 1 h; and a GHT sample was obtained by
heating the sample at a heating rate, temperature, and time of
100 °C/s, 495 °C, and 1 s, respectively (Fig. 1). Two other samples
were prepared from the sub-critical HAZ (Ac1 isotherm line) of
diode and fiber laser welded samples, which are henceforth re-
ferred as the DLW, and FLW sample, respectively (Fig. 1). It can be
noted that the thermal profiles presented in Fig. 1 were measured
(using a thermocouple welded to the sheet surface) directly from
the HAZ during diode laser and fiber laser welding. Due to the
narrow HAZ width (about 400 mm) of FLW, it was not possible to
record the temperature close to the Ac1 isotherm line; however,
the heating and cooling sections of the thermal profile was suc-
cessfully predicted (using a suitable curve fitting method) and
extended to Ac1 line (725 °C) as shown in Fig. 1. The cooling rate in
the sub-critical HAZ of the laser welded samples were estimated
using the Rosenthal Eq. (1) [16]:
2
∂Θ 2πks2 ⎛ υ∆x ⎞ 3
=− ⎜ ⎟ ( Θ − Θ0)
∂t α ⎝ Q ⎠
where ∂Θ/∂t is the cooling rate, ks is the thermal conductivity of
the steel (30 W/m/K), α is the thermal diffusivity of the steel
(5.613
10  6 m2/s), υ is the welding speed (m/s), Δx is the sheet
thickness (mm), Q is the power input (J/mm2), Θ, and Θ0 are
temperature (K) of the sub-critical HAZ (998 K) and the ambient
temperature (298 K), respectively [17]. The parameters used to
temper the samples such as heating rates, cooling rates, tem-
perature, and time are presented in Table 2. In this work, the FHT
and DLW processes are categorized as slow tempering modes, and
the FLW and GHT are regarded as fast tempering modes due to the
differences in heat input, and heating rates.
The microstructure of the tempered structure of the samples
were analyzed using a field-emission scanning electron micro-
scope (FE-SEM, Model: Zeiss Leo 1550), and TEM. The particle sizes
were measured using an image analysis software (imageJ) from
several high-resolution FE-SEM micrographs with a magnification
of 100,000
; more than 1000 particles were measured for each
condition. The carbide sizes presented here are the equivalent
circular diameter of the particles with the equivalent area. TEM
Table 1
Nominal composition of the martensitic steel used in this investigation.
C Mn P S Si Cr Mo
0.24 0.4 0.01 0.01 0.20 o 0.1 o 0.1
Fig. 1. Thermal cycles imposed on martensitic steels during tempering using a
Gleeble heat treatment (GHT), fiber (FLW), diode laser welder (DLW), and furnace
heat treatment (FHT).
samples were prepared using twin-jet electropolishing of the
3 mm disks punched from the foils of o50 mm thickness. Micro-
structure was analyzed using a JEOL 2010F (Japan Electron Optics
Ltd., Tokyo, Japan) electron microscope operated at 200 kV.
Vickers microhardness measurements were carried out using a
load of 1 kg with 15 s dwell time; the microhardness value pre-
sented here is the average value of 12 individual indents (the
tolerance limit represents 95% confidence interval) separated with
a spacing of 200 mm. To estimate nanoscale properties of the
tempered structures, same Vickers microhardness indented sam-
ples were used for the nanoindentation; the study was performed
using a Hysitron Triboindenter TI-900 equipped with a scanning
probe microscope in a load control condition with a loading rate of
500 μN s  1 up to a maximum load of 5000 mN. 12 nano indents
(3
4 matrix) were made in a 50 mm
50 mm area with a spacing
of about 10 mm between indents.
(1)
3. Results and discussion
3.1. As-received martensitic microstructure
Fig. 2 shows the microstructure of as-received material which
contains fully autotempered [18] typical lath-like martensite with
an estimated prior-γ grain size (measured using a linear intercept
method [19]) of about 6.3 7 0.72 mm (marked with arrows in Fig. 2
(a)). Each prior-γ grain is divided into four packets as outlined
with dotted lines in Fig. 2(a). Two kinds of laths were developed
during martensitic transformation due to the differences in
transformation sequences and temperatures [20]. The coarse laths
were formed at the beginning of the martensite formation with
relatively high temperature and exhibited reasonably low dis-
location density due to greater recovery of dislocations throughout
the extended period of transformation [20,21]. On the other hand,
thin martensite laths formed at a later stage of martensite trans-
formation which maintained a high dislocation density (Fig. 2(b)).
The intralath carbides associated with the autotempered marten-
site are also delineated in Fig. 2(a). It was observed that the au-
totempered carbide likely to be precipitated on the coarse mar-
tensite laths (thickness: 4 500 nm) whereas thin laths with an
approximate width of 200 nm were free of autotempered carbides
(Fig. 2(b)). TEM micrograph of lath martensite (Fig. 2(b)) indicated
Ti different contrast of martensite variants (bright and dark) under
0.04
certain incident directions of the electron beam. SAD patterns ta-
ken from the martensite laths were indexed by following the
 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475 469

Table 2
The parameters used to temper the samples.

Sample ID Heating rate (°C/s) Temperature (°C) Time (s) Cooling rate (°C/s) Tempering parameter

FHT Isothermal 500 3600 Air cooled 15,460

DLW 115 725 Nonisothermal 1248 18,740
GHT 100 495 1 50 13,000
FLW 517 725 Nonisothermal 10,856 13,550

Fig. 2. Typical martensitic microstructure of as-received material; (a) FE-SEM micrograph of a prior-austenite grain of martensite with four packets and several blocks,
(b) TEM image with indexed SAD pattern (inset) of lath martensite showing the zone axis of [013]α′; the faint diffraction spots corresponding to nanoscale autotempered
carbides are marked with circles.

body-centered tetragonal (bct) structure of martensite (α′) show-
ing the projection plane of [013]α′. The faint diffraction spots
(marked with circles on the inset SAD) were also observed illus-
trating the presence of autotempered carbides as identified on the
FE-SEM micrograph (Fig. 2(a)). The carbide spots were indexed to
be orthorhombic crystal structure of cementite (Pnma) with a d-
spacing of 2.102 Å corresponding to <211>θ cementite reflection as
marked on inset SAD pattern in Fig. 2(b).
3.2. Characterization of tempered martensite
The sheet was tempered using various tempering methods and
parameter as described in the experimental section (Table 2) and
the resulting high-resolution FE-SEM micrographs are shown in

Fig. 3. Representative high-resolution FE-SEM micrographs of the tempered martensite obtained via various tempering methods; (a) DLW, (b) FHT, (c) FLW, and (d) GHT.
470 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475

Table 3 dispersedly distributed finer carbides; however, the carbides in the

Carbide size measurements at different samples obtained with different tempering GHT sample had an elongated shape with an aspect ratio of about
modes.
3.857 0.47. On the other hand, many small quasi-spherical car-
Tempering Sample Low-angle High-angle Inter-par- Particle bides were observed in the FLW sample with a diameter of about
mode conditions boundaries boundaries ticle dis- density 3571.05 nm. The morphological differences of the carbides
(nm) (nm) tance (nm  2) among these two samples (FLW and GHT) were solely related to
(nm)
differences in heating rates (Table 2), where heating rate in the
Slow heat- DLW 457 1.23 1707 3.51 245 1.6E  5 FLW process was about five times higher than the one applied in
ing mode FHT 587 2.10 1457 3.68 201 2.5E  5 the GHT process (100 °C/s). The spherical shape of carbides on the
Fast heating FLW 357 1.05 957 1.58 100 10.0E  5 FLW sample representing short range carbon diffusion due to
mode GHT 397 0.61 567 1.49 134 5.6E  5
higher particle density and shorter inter-particle spacing. It is
well-known that the maximum number of precipitates is directly
Fig. 3. The micrograph from the DLW sample (Fig. 3(a)), indicates a proportional to the density of nucleation sites [24]; therefore, it
severely tempered structure, and the GHT sample (Fig. 3(d)) ex- can be presumed that the precipitates nucleated at dislocation
hibits a comparatively less tempered structure. The DLW sample sites maintain an identical size and shape distributions (Fig. 3(c)).
shows highly decomposed martensite with spheroidized carbides As per Perrard et al. [24], when there is a high dislocation density,
at laths boundaries (with particle diameters: 45 71.23 nm, the nucleation process is accelerated due to greater solute con-
marked with smaller arrows) and prior-γ grain boundaries (with sumption; as a result, the growth period is ceases and the particles
particle diameters: 17073.51 nm, marked with bigger arrows). In directly go from nucleation to coarsening. Conversely, directional
the DLW sample, the intra-lath carbides are almost dissolved (less diffusion of carbon may occur along the length axis of carbides
particle density: 1.6
10  5 nm  2 compared to other conditions found on a GHT sample; therefore, an elongated shape of carbides
(Table 3)) representing a greater reduction of dislocation density was precipitated.
as intra-lath carbides mainly precipitated at dislocation cell
structures. 3.3. TEM and HAADF-STEM analysis of matrix and precipitates
In addition, the inter-particle distance (245 nm) was also larger
on the DLW sample compared to the other conditions (Table 3) In order to investigate the influences of the tempering modes
suggesting less Orowan looping effect [22,23]. While the sample on subtle microstructural changes of martensite, TEM and HAADF-
was tempered in a furnace at 500 °C for an hr (FHT sample, Fig. 3 STEM imaging were performed and the results are presented in
(b)), similar morphologies of spheroidized carbides were identi- Figs. 4 and 5. TEM study revealed disc-shape, and spherical-shape
fied. However, some of the smaller intra-lath carbides in the FHT carbides at high- and low-angle boundaries, in the DLW and FHT
sample (marked with small arrows) were also observed indicating samples, respectively. In the HAADF-STEM images (Fig. 4(b) and
the presence of a low dislocation density, which was further ob- (e)), the precipitated carbides appeared to be brighter in contrast
served via TEM and HAADF-STEM imaging as will be discussed in a resulting from very high-angle, incoherently scattered electrons.
later section. The FLW (Fig. 3(c)) and GHT (3(d)) showed more The carbides observed on the DLW sample are well-developed,

Fig. 4. Bright-field TEM micrographs and HAADF-STEM images and their corresponding indexed matrix-precipitates SAD patterns; (a)–(c) DLW sample, and (d)–(f) FHT
sample.
 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475
Fig. 5. Bright-field TEM micrographs and HAADF-STEM images and their corresponding indexed matrix-precipitates SAD patterns; (a)–(c) FLW sample, and (d)–(f) GHT
sample.
coarser, and randomly distributed. Similar coarser carbides at
high-angle boundaries were identified on the FHT sample (Fig. 4
(d) and (e)); in addition, spherical intralath carbides (diameter:
o100 nm) are also observed. The presence of these intralath
carbides may be attributed to: (i) precipitation at the final stage of
carbide precipitation or (ii) a dissolution state (as per classical
nucleation theory) due to smaller than the critical carbide size
[25,26]. On the other hand, the high-angle boundary carbides are
interconnected (Fig. 4(e)) illustrating a short-circuit diffusion path
[26]. The carbides observed in the tempered martensite structures
were indexed to be orthorhombic crystal structure of cementite
(θ-Fe3C) whereas the matrix phase was identified as body-cen-
tered cubic (bcc) phase of ferrite. The orientation relationships
(OR) between ferrite (α) and cementite (θ) were determined to be
[023]α ||[110]θ , and [111
̅ ]α ||[311
̅ ]θ for the DLW (Fig. 4(c)), and FHT
sample (Fig. 4(f)), respectively. The ferrite and cementite OR in the
FHT sample was matched with Isaichev OR [27,28] (or close to it)
with [311 ̅ ]θ at an angle of 0.91° from [111 ̅ ]α .
Conversely, intra- and inter-lath carbides became extremely
fine and densely spaced when rapid thermal cycles were em-
ployed using a fiber laser and Gleeble thermal cycling (Fig. 5
(a) and (d)). It was noticeable that the size distribution of carbides
at low-angle boundaries were similar for both the FLW and GHT
samples; however, the size of the carbides located at the high-
angle boundary in the FLW was about three times larger than
those from the GHT sample (Table 3). Interestingly, the intra-lath
carbides found on the FLW sample were randomly distributed and
spherical in shape (Fig. 5(b)); however, the carbides in the intra-
lath position of the GHT sample maintained a specific orientation
relation with the adjacent laths. It was observed that the multi-
variate carbides were oriented along o112 4 direction of the
ferrite matrix with an approximate angular position of 33° to the
lath boundary (inset of Fig. 5(d)). The indexed SAD patterns pre-
sented in Fig. 5(c) and (f) confirmed the OR of [012]α ||[241 ¯ ] , and
θ
471
̅ ]α ||⎡⎣ 001⎤⎦ for the FLW, and GHT sample, respectively. It is
[ 112
θ
noted that the cementite precipitated on the GHT sample main-
tained a well-defined Bagaryatsky orientation relationship [29,30].
TEM study of the slowly tempered structures (Fig. 4) revealed a
low dislocation density on the ferrite structure, suggesting that the
recovery of dislocation substructure was more pronounced in the
case of slowly heated samples [10]. Conversely, the faster thermal
cycles provided less tempering time, retained more dislocation cell
structures (Fig. 5) [7]; with some of the dislocation lines marked
with arrows for example in Fig. 5(e). In addition, the dislocation
lines observed on the GHT sample are almost parallel to the length
axis of the cementite platelets attributing the growth of the plate-
like cementite occurred along the dislocation line.
3.4. Dislocation density and tempering parameters
The dislocation density is an important parameter which im-
pedes the lattice movement, thus increases the strength of the
steels. To estimate the dislocation density, several experimental
methods are usually employed such as X-ray diffraction line-
broadening method [31], TEM [32], electron backscattered dif-
fraction (EBSD) [9,33]. In the present investigation, the dislocation
density of untempered martensite was estimated using a syn-
chrotron X-ray measurement at the 33-ID-D beamline of the Ad-
vanced Photon Source (APS) at the Argonne National Laboratory.
The dislocation density of the steel sample was estimated to be in
the order of 4.90 70.5
1015 m  2, which is about three times
compared to other studies (about 1.6
1015 m  2 [32,34]) for the
identical martensitic steel carbon content (0.2%). It is well-known
that dislocation density is not uniform throughout the sample,
therefore, the values measured using TEM and EBSD technique
may provide local dislocation density. On the other hand, the
synchrotron measurement is considered a bulk area analysis
472 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475

Fig. 6. (a) Relationship between dislocation density and the carbon content of lath martensite, and (b) a plot of dislocation density as a function of the modified tempering
parameter.

which provides more representative values of the average through TPn = Tn( 20+logtn ) (2)
the thickness.
Fig. 6(a) shows a relationship between dislocation density and
the carbon content of steels [7,9,32,35,36], which indicates that T
{ n −1 ( 20 + logtn −1) −20}
dislocation density increases with carbon content due to local tn = 10 Tn +∆t (3)
distortion induced by the interstitial carbon atoms. Aside from
carbon content, dislocation density is also influenced by cooling
rate, and martensite start temperature during transformation [32]. Tn = Tn −1 + α∆t (4)
However, when a highly dislocated martensite phase is exposed to
an elevated temperature, then dislocation density decreases due to where α and Δt are the heating or cooling rate and the isothermal
annihilation and recovery process [1,23]. Dislocation density is time step at Tn  1 temperature, respectively. By plotting dislocation
expected to decrease with tempering temperature, and holding density as a function of modified tempering parameters of fully
time; however, a slow heating cycle results in more annihilation martensitic steels [7,9], it is found that the dislocation density of
and recovery rate than rapid heating as observed in Figs. 4 and 5
the tempered martensite varied as a cubic function (fitting coef-
are in accordance with other studies [7,9].
ficient, R2 ¼0.96) of the modified tempering parameter (Fig. 6(b)).
In the present study, the tempering processes considered have
Using the fitted function, the dislocation density of the studied
different heating rate, temperature, and time (Table 2); therefore,
samples are predicted based on their modified tempering para-
the influences of these factors were combined in the form of a
meter as shown in Fig. 6(b); the highest recovery of dislocations is
modified tempering parameter as proposed by Tsuchiyama [37].
predicted for the DLW sample which is due to greater heat input
The proposed model applies the additivity rule for time in order to
consider heating and cooling time during tempering. In this and higher tempering parameter [12]. Conversely, the GHT sample
method, the heating and cooling cycles are divided into several experiences less recovery and a high amount of dislocation density
small isothermal time (tn) segments at Tn temperature. After n is retained as observed experimentally via TEM as shown in Fig. 5
isothermal steps, the tempering parameter (TPn) can be presented (d) and (e).
as:

Fig. 7. (a) Vickers microhardness and nanohardness of tempered martensite plotted as a function of tempering conditions, and (b) plot of hardness ratio (Hn/HV) with respect
to Vickers microhardness.
 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475
3.5. Micro- and nano-scale properties
Microhardness and nano-scale properties of the tempered
martensite were further assessed using Vickers microhardness and
nanoindentation tests as shown in Fig. 7. There are four micro-
structural units in a low carbon lath martensite, prior-γ grains,
packets, blocks, and laths. The prior-γ grain is typically divided
into four packets (Fig. 2(a)), which is composed of six blocks with
identical crystal orientation, and each block is further subdivided
into several parallel laths (Fig. 2(b)) with a high density of lattice
defects [38–41]. The lath boundaries are considered to be low-
angle grain boundaries (θmin ¼2.8–2.9°) and do not provide ef-
fective dislocation barriers. On the other hand, block boundaries
effectively impede dislocation propagation; therefore, these are
considered major boundaries in lath martensite [42]. The hardness
measured using a Vickers indentation combines all of the micro-
structural units including high- and low-angle boundaries, dis-
location, solid solution, precipitation. Conversely, using a na-
noindenter (Berkovich type) with a smaller tip size (about 50 nm
tip diameter) which is less than the lath width (about 200 nm);
therefore, the effects of high-angle boundaries (θmin Z15°) on the
nanohardness may be disregarded [43,44].
Fig. 7(a) illustrates the Vickers micro- and nanohardness of four
tempered martensite structures considered here; in which the
microhardness values are converted to GPa for comparison. Both
hardness measures increase as heat input decrease (signifying a
lower tempering parameter (Table 2)), due to a fewer structural
changes, a larger boundary area, and the higher matrix strength.
Nanohardness measured on the samples are higher than adjacent
microhardness tests which is due to the effect of various bound-
aries present on a martensite phase as reported by Ohmura et al.
[43–45]. The structure containing a large amount of boundaries
has a higher hardness compared to the structure with a fewer
boundaries. The largest hardness differences were measured on
the DLW sample which was due to the absence of a high amount of
dislocation density in the vicinity of boundaries. It has been re-
ported that nano-indents located at a boundary exhibit higher
nanohardness than inside the laths [20,21,46]; therefore, the ab-
sence of boundaries resulted in a lower microhardness value on
the DLW sample. However, the deviation of hardness values de-
creases as it approaches to rapidly heated condition; it is notice-
able that for the GHT sample, both hardness values are similar due
to less softening of the boundary areas. It may be concluded that
when the structure is heated slowly, the high-angle boundary
regions softened more than the low-angle boundaries as carbon
diffusion occurred much faster in the high-angle boundaries dur-
ing tempering [4,7,47].
Fig. 7(b) shows a plot of hardness ratio (Hn/Hv) as a function of
Vickers microhardness; the hardness ratio represents the con-
tribution of matrix strength on the total macroscopic hardness of
the structure as can be approximated by the following relation-
ship.
1
Hn k′d− 2
=1−
HV HV
Where, the locking parameter k′ is a constant, and d is the grain
size. Ohmura et al. [43–45] reported that the higher the Hn/Hv
ratio, the greater the reduction of the grain boundary effect on
macroscopic strength. Therefore, from Fig. 7(b), it may be con-
cluded that DLW sample has higher destruction of the boundary
regions (greater recovery) so in this sample, grain boundary
strengthening will give less contribution to overall strength as to
the FLW and GHT samples.
473
3.6. Contribution of dislocations and precipitates on martensite
strength
Typically, the yield strength of lath martensite is correlated
from the contributions of lattice friction stress of pure iron, the
solid solution strengthening, the precipitation strengthening (spct),
grain boundary strengthening, and forest dislocation density
strengthening (sρ) at lath and sub-block boundaries. However,
considering the tempering effect on the strength, in this study,
only dislocation density and precipitation strengthening are
evaluated. The solid solution hardening effects on the tensile
strength have been disregarded as only a single steel chemical
composition was used and negligible carbon remained in the solid
solution after tempering. A separate study carried out using Dila-
tometry confirmed that the carbide precipitation has completed
when the sample was tempered with a tempering parameter of
13,000 (GHT sample) which was the lowest tempering parameter
among the four types of the sample considered. Therefore, it can
be presumed that all of the carbon atoms already diffused and
combined with the iron atoms to form stable cementite, justifying
the decision to omit the effect of solid solution strengthening on
tensile strength. The strength contribution in relation to the dis-
location density is estimated using Taylor formula [48]:
∆σρ = MαGb ρ (6)
where M ¼3 is the Taylor factor, α ¼0.25 is a fitting constant re-
lated to the interaction between forest dislocations [49],
G ¼76 GPa is the elastic isotropic shear modulus of lath martensite
[50], b is the Burgers vector, and ρ is the dislocation density. The
ferrite lattice constant of the investigated steel was estimated from
the TEM selected area diffraction patterns to be a ¼2.915 70.015 Å.
The value of b is considered to be 2.52 Å along o111 4 slip
direction.
The strength of lath martensite can be correlated from the
contributions of the carbide precipitation which may increase the
strength by impeding dislocation glide [22,51]. The contribution of
precipitation strengthening is predicted using the Orowan-Ashby
model [22,23] as presented in Eq. (6).
f
σpct =10. 8 ln(1630d)
d (7)
where, f and d are the volume fraction of precipitate and mean
particle diameter (mm), respectively. The volume fraction and the
mean particle diameter are estimated from the high-resolution FE-
(5)
Fig. 8. Dislocation density and precipitation strength predictions as a function of
the modified tempering parameter for four different tempered martensite samples.
474 D.C. Saha et al. / Materials Science & Engineering A 673 (2016) 467–475

SEM and TEM micrographs by following the formula as described Innovation in Automotive Manufacturing Initiative (IAMI) in Ca-
in Ref. [22]. nada for financing this project. Authors are thankful to Arce-
The contribution of strength due to a high density of forest lorMittal Dofasco Inc. in Hamilton, Canada for providing the ma-
dislocations and precipitation are plotted in Fig. 8 with respect to terials to carry out this work. The authors would like to thank Dr.
the modified tempering parameter. The graph shows that the Levente Balogh from the Department of Mechanical and Materials
dislocation density has prominent contribution over that of the Engineering, Queen's University, for the dislocation density mea-
carbide precipitation, and the observation is consistent with other surements from the Synchrotron data, and Dr. Yuquan Ding from
researchers [42]. The structure heated with rapid nonisothermal the Mechanical and Mechatronics Engineering Department, Uni-
process (FLW sample) possessed the highest precipitation hard- versity of Waterloo for his kind cooperation with the na-
ening effect due to highest particle density (10
10  5 nm  2) re- noindentation study.
sulting from a short carbon diffusion and shorter growth period,
although the high-angle boundary carbides were larger than the
one on GHT sample (Table 3). In overall, rapidly tempered GHT and References
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