Materials and Design 54 (2014) 1049–1055

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Materials and Design

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Technical Report

Comparing microstructure and mechanical properties of AISI D2 steel

after bright hardening and oil quenching
H. Torkamani ⇑, Sh. Raygan, J. Rassizadehghani
School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, P.O. Box 11155-4563, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: D2 is a high carbon-high chromium cold work tool steel. The main problems of hardening treatment of
Received 24 January 2013 this steel include risk of crack distortion and formation because of thermal shocks induced by oil quench-
Accepted 17 September 2013 ing (conventional hardening treatment for D2 steel). For this purpose, in this study, the possibility of
Available online 26 September 2013
improving microstructure and mechanical properties of AISI D2 steel and decreasing the risk of cracking
by bright hardening in comparison with oil quenching was investigated. The quenchant used in bright
hardening included 60% of KOH and 40% of NaOH. The bright-hardened samples showed no cracks during
their heat treatment, which was in contrast to oil-quenched ones. Moreover, microstructural examina-
tions of the samples revealed that, compared with oil-quenched samples, quenching in hot alkaline salt
bath resulted in finer and more uniform distribution of carbides and also lower amount of retained aus-
tenite in the matrix. Different microstructures caused the samples to possess different mechanical prop-
erties; e.g. bright-hardened samples possessed higher impact toughness (3.7 J) and tensile strength
(1764 MPa) as well as higher level of hardness (792 HV) than those of oil-quenched samples, which were
3.2 J, 1608 MPa and 710 HV, respectively.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction bides, their distribution and morphology can strongly affect

AISI D2 steel has high level of hardness but poor toughness
behavior. The main objective is not only to improve toughness
behavior of steel but also to maintain high level of hardness. The
amounts of retained austenite at room temperature and carbon
supersaturated fresh martensite make the steel both brittle and
susceptible to cracks. Thus, after hardening treatment, this steel
must be double or triple-tempered [1–4]. During the tempering
process of this steel, large volumes of secondary carbides (mainly,
M7C3) are precipitated because of high carbon and the content of
alloying elements [1,5–7]. Since chromium content in D2 steel is
high, M would be mostly chromium. On the one hand, it has been
well determined that temper process causes reduction of disloca-
tion density and quench stresses, which reduces steel hardness
[1–4,8]. On the other hand, formation of carbides accompanied
by transformation of the retained austenite to martensite leads
to retardation of hardness drop in this stage [2,3]. Beside the tem-
per process, quench process could be considered as one of the most
important parts of heat treatment cycles. The more generated
stresses due to fast heat removal in the quench process, the more
driving force for carbide precipitation and also the more the pref-
erable sites (mainly, dislocations) for carbide nucleation during
the temper process [4,8,9]. In addition to volume fraction of car-
⇑ Corresponding author. Tel.: +98 9122213206.
E-mail address: H.torkamani@ut.ac.ir (H. Torkamani).
mechanical properties of steel. For instance, refinement of carbides
with high population density can coincidently improve hardness
and toughness behaviors of steel [4,10–12]. Accordingly, with re-
spect to D2 steel behavior in quench and temper processes, it is
possible to obtain different properties from D2 steel by utilizing
different quench methods. The method should be fast enough in
heat removal to permit formation of the desired microstructure
and reduces the amount of retained austenite; also, it should be
slow enough to minimize residual stresses and distortion of the
part [2,3,8,13,14]. It seems that hot alkaline salt bath, 60% of
KOH and 40% of NaOH, could be a proper bath for this purpose. It
should be mentioned that NaOH and KOH melt at 328 °C and
360 °C, respectively, while the mixture of these compounds (60%
of KOH and 40% of NaOH) melts at around 160 °C. Accordingly, this
medium has low viscosity in its operational temperature range
(180–350 °C), resulting in better heat removal with higher H
parameter compared with oil bath (conventional quench medium
for D2 steel) [8,14–17]. It is also claimed that salt bath does not in-
clude the vapor blanket stage during the quench process and has a
uniform heat removal rate [8,13–16]. The aforesaid stage occurs
only if surface temperature of the samples exceeds a certain tem-
perature known as characteristic temperature, which is higher
than boiling point of the bath and varies in different conditions
[8,14].
Briefly, it can be deduced that the targeted medium provides
uninterruptable and more uniform heat removal during quench

0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.09.043
1050 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055
process compared with oil; consequently, temperature of the sam-
ple drops more rapidly, which continues with an almost constant
cooling rate due to the absence of vapor blanket stage.
2. The experimental procedure
Chemical compositions of the steel used in this study as well as
standard composition of D2 steel are shown in Table 1 [1,2]. The
samples were fully prepared for performing the tests before the
hardening processes because of high level of hardness that samples
obtained after the treatment. Dimensions of the prepared samples
are shown in Fig. 1a and b.
Performing the heat treatment process began by preheating the
samples at 650 °C for 20 min prior to austenitizing. Then, they
were austenitized at 1050 °C for 45 min under the protective CO/
CO2 atmosphere to avoid decarburization or oxidation of the alloy-
ing elements. The interrupted quench procedure was used for
quenching. The first step of the quench process was done by
immersing the samples in conventional salt bath (sodium nitride)
at 520 °C for 10 min and then quenching in one of the following
media:
 Salt bath containing 60% of KOH and 40% of NaOH at 230 °C.
 Stationary oil at 60 °C.
The immersion time for both quenchants was 5 min. The salt
quenched samples were cooled in air and then washed with mild
water. Hardening process by means of quenching in hot alkaline
salt bath is called bright hardening because the remaining salt on
the surface of the parts can be easily swept by mild water and a
bright surface can be obtained [18]. Some of the quenched samples
were double-tempered immediately at 540 °C for 1 h plus 1 h. Each
stage of double-tempering process was carried out when the sam-
ples were air cooled and reached the temperature of about room
temperature. It is well advised to temper the D2 steel after the
quench process as soon as possible. Delaying the tempering stage
might result in serious risk of cracking, particularly if the retained
austenite is present, because the retained austenite is decomposed
and transformed to un-tempered brittle martensite and the expan-
sion caused by this transformation might deform the part [2,3]. It
should be mentioned as one of the main outcomes of this study
that there was no observation of cracking in bright-hardened sam-
ples. But, some of the samples, which were quenched in oil bath,
were cracked and distorted during the hardening or tempering
stages, which could be attributed to high level of residual stress de-
rived from non-uniform heat removal of the oil bath.
After polishing, the specimens were etched using the picral
solution (3 g picric acid in 100 ml ethanol). Microstructural exam-
inations were done on the micrographs taken by scanning electron
microscope (SEM Camscan MV 2300) at different magnifications
and also optical microscope. Image analysis was carried out on
the randomly selected optical micrographs by using MIP software
to estimate roundness factor, volume fraction and size of the car-
bides. The estimation of the carbide factors was done on five ran-
dom microstructures from each sample and the average was
reported. Moreover, identification of the carbides in the matrix
was checked using energy dispersive X-ray spectroscopy (EDS)
technique on the oil-quenched sample.
Table 1
Chemical composition of the steel used in this study and standard D2 steel.
Element Mo
Weight % Used steel 0.77
D2 (standard) 0.70–1.20
Measurement of the retained austenite in quenched samples
can verify differences between characteristics of the quench media.
For this purpose, X-ray diffraction (XRD) patterns of as-quenched
samples were evaluated. Volume fraction of the retained austenite
was measured according to ASTM: E975.
Hardness test was done by a Vickers indentor at 30 kgf load. The
tests were done at least five times on each as-quenched and dou-
ble-tempered sample and the average was reported.
Impact tests were performed at least three times at room tem-
perature using a WOLPERT testing machine (model AMSLER D-
6700) on the double-tempered charpy specimens, prepared
according to ASTM: E23 (Fig. 1a).
Because of high hardness level that D2 steel obtained after
hardening process, it was not possible to perform tensile tests
using the conventional tension grips. For this reason, a pair of grips
shown in Fig. 1c was used.
Tensile tests were performed on double-tempered specimens
according to ASTM: E8. A GOTECH AL-7000 LA 30 tensile machine
was used to carry out this test.
3. Results and discussion
3.1. Microstructure
It has been reported that volume fraction, size and distribution
of carbides and also the amount of retained austenite are the most
effective microstructural features affecting mechanical properties
of D2 steel [19–22]. Fig. 2 shows results of EDS line scan analysis
of the quenched sample. The results illustrated that weight per-
centage of the carbide-forming elements (especially Cr) increased
in dark areas, implying that these regions were carbides and the
bright area was the matrix.
For measuring the amount of retained austenite in the
quenched samples, volume fractions of the carbides were esti-
mated by an image analyzer on the random optical microstruc-
tures of the quenched samples, the results of which are shown in
Table 2. Different volume fractions of carbides in these two condi-
tions can be attributed to bath temperature which was 230 °C and
60 °C for salt bath and oil bath, respectively, and more diffusion at
higher temperature. X ray diffraction patterns of the quenched
samples are shown in Fig. 3. The results of XRD analyses demon-
strated that the amount of retained austenite in bright-hardened
samples was lower than that of oil-quenched sample (Table 2).
Consequently, there existed lower possibility of cracking in
bright-hardened samples. In fact, in comparison with oil quench-
ing, quench in hot alkaline salt bath caused more martensitic
transformation due to its higher H parameter. It has been asserted,
in other investigations, that deep cold treatment (cryogenic
treatment) is a procedure, which can reduce or eliminate retained
austenite in many steels and thus eliminate the need for multiple
tempering. However, there is some uncertainty about its effects on
the final properties [10,19,23].
Fig. 4a indicates that only long time isothermal holding (about
4000 s at 250 °C) might lead to the formation of bainite in the
matrix. Therefore, bainite phase cannot exist in microstructure of
the quenched steel due to insufficient holding time. So, the matrix
mainly consisted of martensite through the considered heat
V Cr Si Mn C Fe
0.54 11.63 0.79 0.45 1.48 Rest
1.10 11.00–13.00 0.60 0.60 1.40–1.60 Rest
 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055 1051

Fig. 1. Scheme of (a) impact, (b) tensile test samples beside and (c) tension grips.

Fig. 2. (a) SEM micrograph of the oil quenched sample, (b and c) EDS line scan microanalysis of the determined line on the micrograph.
1052 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055

Table 2
Volume fraction of carbides and amount of retained austenite in hot salt and oil-quenched samples.

Quench medium Volume fraction of carbides (%) Amount of retained austenite (%)
Alkaline salt (230 °C) 9 17
Stationary oil (60 °C) 6 26

roundness factor close to 1. This sort of carbide distribution in

the matrix leads to decrease in average free distance from one car-
bide to others (mean free path of the carbides, k). Volume fraction
(V) and mean diameter of carbides (dm) affect magnitude of k
according to one of the following equations [6,9,12]:

4ð1  VÞ
k¼ dm ð1Þ
3V

Fig. 3. X-ray diffraction patterns of (a) oil-quenched and (b) bright-hardened
samples (philips PRO-PW 1730 X-ray diffractometer with Cu Ka radiation).
treatment cycles. This could be better realized when the heat treat-
ment cycles are considered beside the TTT diagram (Fig. 4b).
Carbide particles are categorized as primary carbides (PCs) and
secondary carbides (SCs), which are rounder than the PCs. SCs are
further classified as large secondary carbides (LSCs) and small sec-
ondary carbides (SSCs). SSCs are considered less than or equal to
1 lm and LSCs are > 1 but 6 5 lm while carbide particles > 5 lm
are PCs. Justification for the classification of carbides and selection
of their size limits has been reported earlier in Ref. [10].
Fig. 5 shows dispersion of carbides in the matrix after double-
tempering and characteristics of carbides are reported in Table 3.
It is deduced from Fig. 5a and Table 3 that high volume fraction
of carbides including a large number of SCs is presented in the
microstructure of bright-hardened samples which have a
ð1  VÞ
k¼ dm ð2Þ
V
Both equations indicate that increase in volume fraction of car-
bides along with decrease in carbide diameter decreased magni-
tude of k. It has been well documented that decrease in k is one
of the most important strengthening mechanisms in steels [4,9,12].
It can be seen in Fig. 5b that microstructure of the oil-quenched
samples after double-tempering consisted of coarse carbides with
non-uniform distribution in the martensite matrix, which led to in-
crease in free path between the carbides (k) (Table 3). Also, in this
microstructure, there were free carbide zones in martensite matrix,
which could disturb mechanical properties of steel. Morphology,
size and types of carbides (PC or SC) could be assessed in SEM
micrographs (Fig. 6), which would tally with the results extracted
from optical images.
Different microstructure characterizations obtained in different
samples can be explained by different H parameters of the baths. In
fact, quench in alkaline salt bath with a higher H parameter re-
moves the heat more uniformly and rapidly from the sample and
consequently more martensitic transformation occurs, which is
known to produce high density of defects. In contrast to the vacan-
cies, dislocations are thermodynamically unstable and, when steel
is heated up, there is a tendency to reduce their energy or density.
The rearrangement or elimination of these dislocations will reduce
internal energy of the system [4,12]. During the tempering treat-
ment, elimination of dislocations and reduction of lattice distor-
tions provide the driving force for diffusion of carbon and
alloying elements to the nearby defects. These segregated areas
are preferable sites for small secondary carbide nucleation [19].

Fig. 4. (a) TTT (IT) diagram of D2 steel austenitized at 1050 °C [2] and (b) heat treatment cycles performed in this study.
 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055 1053

Fig. 5. Microstructure of double-tempered samples quenched in different (a) bright-hardened and (b) oil-quenched media.

Table 3
Carbide characteristics in different samples.

Quench medium Carbides (%) Volume fraction of carbides (%) Average size of carbides (lm) k (lm)
0 < R 6 0.65 0.65 < R 6 0.8 0.8 < R 6 1
Alkaline salt at 230 °C 9.64 7.66 82.70 15 1.87 10.60
Stationary oil at 60 °C 20.86 12.23 66.91 10 2.13 19.17

R: roundness factor of carbides.

Fig. 6. SEM images of double-tempered samples at different magnifications quenched in hot alkaline salt bath (a and b) and oil bath (c and d).

Hence, a larger volume of martensite obtained in bright-hardened between preferable nucleation sites decreased and caused
samples provided more driving force as well as more preferable formation of secondary carbides with high population density
sites available for carbide nucleation. In this manner, the distance (Table 3). During tempering of the oil-quenched samples, carbides
1054 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055

Table 4
Impact energy and hardness of D2 samples quenched in different media in as-quenched and double-tempered conditions.

Quench medium Vickers hardness (HV) (as-quenched) Vickers hardness (HV) (double tempered) Impact energy (J) (double tempered)
Alkaline salt at 230 °C 934 792 3.7
Stationary oil at 60 °C 890 710 3.2

3.2. Mechanical properties

The amount of retained austenite and martensitic transforma-

Fig. 7. Hardness of D2 steel versus tempering temperature [2].
tion largely affected the D2 steel hardness in as-quenched condi-
tion. It was demonstrated that the amount of retained austenite
in the samples quenched in salt bath was lower than that of the
oil-quenched sample (Table 2), which resulted in higher hardness
of bright-hardened samples (Table 4).
Temper is one of the most important processes affecting hard-
ness, which has twofold effects: recovery (decreasing hardness)
and formation of secondary carbides (increasing hardness). As far
as tempering behavior of D2 steel was concerned, the former effect
outweighed the latter one and hardness of steel showed insignifi-
cant drop during the temper stage. But, at high temperature (above
500 °C), hardness decreased rapidly (Fig. 7) [2]. Hardness reduction
rate depends on the amount of secondary carbides precipitated
during the temper stage and also temper temperature. It was found
that SCs were more precipitated in bright-hardened samples.
Therefore, bright-hardened samples did not show a great hardness
drop after tempering compared to the oil-quenched samples
(Table 4).
The results of impact test of double-tempered samples are
illustrated in Table 4. It can be seen that impact energy for
bright-hardened samples was higher than that of oil-quenched
samples despite the fact that the former one had a higher hard-
ness value. Microstructural examination showed that microstruc-
ture of the bright-hardened samples consisted of uniform
distribution of fine carbides with high volume fraction in the
martensite matrix. This sort of distribution improved toughness
behavior of steel because of a large number of fine carbides,
which acted as failure barriers. On the other hand, the coarse car-
bides observed in oil-quenched samples not only were the stress
concentration centers but also tiny initiated cracks propagated
along these coarse carbides.
Fig. 8 demonstrates the tensile test curves for both double-tem-
pered samples with different quench media. The results obtained
from the tensile curves are shown in Table 5. This table shows that,
in spite of insignificant lower elongation, higher ultimate tensile
strength was obtained by bright hardening. Elongation is directly
related to the dislocation motion [12]. Accordingly, the shortened
k obtained in bright-hardened samples restricted the distance
through which dislocations could pass, which resulted in elonga-
tion reduction (Table 5) while causing strengthening. Moreover,
the salt bath quenched samples showed a higher value of failure
energy per unit of volume (the area under tensile test curve) com-
pared with the oil-quenched samples, which was in agreement
with impact test results.

4. Conclusions
Fig. 8. Tensile test curves of the samples quenched in different media after double-
tempering. The main outcomes of this study can be briefly highlighted in
the following statements:

nucleated in the preferable sites, which were less than those in (1) No distortion or crack was observed in the bright-hardened
bright-hardened samples, and grew more on the primary and sec- samples; but, some of the oil-quenched samples were
ondary precipitated carbides (Fig. 6). cracked and distorted during the heat treatment process.
 H. Torkamani et al. / Materials and Design 54 (2014) 1049–1055
Table 5
Results of tensile tests.
Quench medium Ultimate tensile stress (UTS) (MPa)
Alkaline salt at 230 °C 1764
Stationary oil at 60 °C 1608
(2) Carbide distribution in martensite matrix was more uniform
and finer in the molten salt quenched samples compared
with the oil-quenched samples.
(3) The bright-hardened samples had a lower amount of
retained austenite in as-quench condition in comparison
with the oil-quenched samples.
(4) More precipitation of secondary carbides in the bright-hard-
ened samples caused less hardness drop through tempering
stage.
(5) The bright-hardened samples possessed higher hardness,
toughness and UTS values than the oil-quenched samples.
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