Microstructure–Property Correlation in Low-Si Steel

Processed Through Quenching and Nonisothermal

Partitioning
GAURAV K. BANSAL, V. RAJINIKANTH, CHIRADEEP GHOSH,
V.C. SRIVASTAVA, S. KUNDU, and S. GHOSH CHOWDHURY

In the present investigation, an attempt has been made to stabilize austenite by carbon
partitioning through quenching and nonisothermal partitioning (Q&P) technique. This will
eliminate the need for additional heat-treatment facility to perform isothermal partitioning or
tempering process. The presence of retained austenite in the microstructure helps in increasing
the toughness, which in turn is expected to improve the abrasion resistance of steels. The carbon
partitioning from different quench temperatures has been performed on two different alloys,
with low-Si content (0.5 wt pct), in a salt bath furnace atmosphere, the cooling profile of which
closely resembles the industrially produced hot-rolled coil cooling. The results show that the
stabilization of retained austenite is possible and gives rise to increased work hardening, better
impact toughness and abrasive wear loss comparable to that of a fully martensitic microstruc-
ture. In contrast, tempered martensite exhibits better wear properties at the expense of impact
toughness.

https://doi.org/10.1007/s11661-018-4677-1
 The Minerals, Metals & Materials Society and ASM International 2018

I. INTRODUCTION A possible alternative to the above approach is

quenching and nonisothermal partitioning.[11,12] In this
RECENTLY, quenching and isothermal partitioning process, carbon partitioning occurs nonisothermally,
(Q&P) process[1] has been employed for austenite during extremely slow cooling of industrially produced
stabilization between martensitic laths.[2–10] The retained hot-rolled coils, immediately after quenching on the
austenite in Q&P steels transforms to martensite during run-out table. The quenching and partitioning temper-
deformation that leads to improved work hardening and atures for isothermal partitioning can be chosen sepa-
ductility. Several researchers have reported that quench- rately, while nonisothermal partitioning is limited by the
ing and isothermal partitioning (Q&P) process engen- choice of a single temperature for both quenching as
ders better property combinations in comparison with well as partitioning. Hence, both the initial austenite
fully martensitic[8] and tempered steels.[2,9,10] However, fraction after quenching and the driving force for
the isothermal partitioning or tempering step requires carbon partitioning is controlled by a single tempera-
additional facilities and energy after hot rolling, adding ture, which makes the process more constrained than the
to the production cost. isothermal partitioning. A study on nonisothermal
partitioning from different quench temperatures will
help to arrive at an optimal quench temperature for
industrial production of hot-rolled Q&P steels.
GAURAV K. BANSAL, V.C. SRIVASTAVA, and S. GHOSH Most of the recent researches on nonisothermal
CHOWDHURY are with the Academy of Scientific and Innovative partitioning have mainly focused on automotive appli-
Research, CSIR-National Metallurgical Laboratory, Jamshedpur, cations. Thomas et al.[11,12] and Tan et al.[7,13] have
831007, India and also with the Materials Engineering Division, shown, in their initial works on nonisothermal parti-
CSIR-National Metallurgical Laboratory, Jamshedpur, 831007, India.
Contact e-mail: sgc@nmlindia.org V. RAJINIKANTH is with the
tioning, achievement of microstructure and properties
Materials Engineering Division, CSIR-National Metallurgical similar to that obtained by other researchers using
Laboratory. CHIRADEEP GHOSH is with the Research and isothermal partitioning. It is important to note that
Development Division, Tata Steel Limited, Jamshedpur, 831001, industries encounter an average financial loss of about
India. Contact e-mail: chiradeepghosh@gmail.com S. KUNDU is 0.25 pct of their total turnover due to wear and the
with the Academy of Scientific and Innovative Research, CSIR-
National Metallurgical Laboratory and also with the Research and contribution from abrasive wear is around 63 pct of this
Development Division, Tata Steel Limited. loss.[14] Therefore, it is of high relevance to make an
Manuscript submitted January 26, 2018. attempt to study the effect of nonisothermal partitioning

METALLURGICAL AND MATERIALS TRANSACTIONS A

on abrasion behavior of steel and correlate the same and B. Also, an attempt has been made to correlate the
with the tensile and impact properties. This will open a microstructures with different mechanical properties
new paradigm where these steels are obtained directly (namely, tensile, impact, and wear properties) for
from the hot strip mill eliminating additional tempering optimal heat-treatment conditions. In order to compare
treatment for toughness improvement. The extensive the microstructural features and properties of these
work of Wolfram et al.[2] on isothermal partitioning has Q&P alloys, similar measurements were conducted on
shown improvement of the abrasion resistance with the water quenched samples having fully martensitic
increased retained austenite content, despite their similar microstructure. This was followed by fractography to
hardness values. This is due to the fact that retained interpret the operating fracture and wear mechanisms.
austenite experiences microshearing during service and
thus delays the removal of chips from the surface of a
component. In addition, the deformation of austenite at II. ALLOY DESIGN AND PROCESSING
surface induces surface hardening by transformation-
induced plasticity (TRIP) effect, i.e., transformation of Table I shows the chemical composition, carbon
retained austenite to hard martensite. The hard marten- equivalent, and Ms temperature of the investigated
sitic surface coupled with a tough core, containing alloys (i.e., Alloy-1 and Alloy-2). The carbon equivalent
untransformed austenite, is beneficial for both abrasion (CE) and Ms temperature were calculated based on
as well as impact properties.[2,15–17] Dearden and O’Neill formula[34] and Andrews equa-
Some of the recent studies have shown that small tion,[35] respectively. Simulation software package Ther-
amount of austenite (generally < 16 pct) can be stabi- mo-Calc classical version-S with TCFE7 database was
lized through nonisothermal partitioning pro- used to predict the evolution of different phases with
cess.[7,11–13,18] This small amount of retained austenite temperature and their chemical composition, under
is attributed to competing mechanisms. These include equilibrium condition. The amount of V present in the
carbon trapping at defects,[19] carbon clustering[20] and Alloy-1 is predicted to consume all the nitrogen without
precipitation of cementite and transition carbides consuming much of the carbon (Figure 1(a)). In con-
(mainly e and g carbides),[6,10] which are also likely to trast, Ti in Alloy-2 is predicted to consume all the
happen during coil cooling. These mechanisms in nitrogen present in the alloy along with a small amount
operation, reduce the available carbon for austenite of carbon (~ 20 ppm) (Figure 1(b)). It ensures, there-
stabilization. To avoid these competing mechanisms, fore, that the addition of these two microalloying
steels are generally alloyed with a higher amount of Si elements will lead to only marginal reduction in the
and/or Al (generally > 1.5 wt pct).[1,21] The presence of available carbon for partitioning to austenite.
high-Si content leads to surface oxides and excessive During slow cooling below the quench temperature,
rolled-in scale after hot rolling, which deteriorates the carbon from martensite can either partition to austenite
steel properties.[22,23] Although high Al increases Ms or can precipitate as carbides. The formation of carbides
temperature, it results in smelting difficulties and lowers consumes most of the carbon and in turn reduces the
solid solution hardening.[22] Hence, it is important to available carbon for austenite stabilization. These car-
study the carbon partitioning behavior at lower Si and/ bides can be avoided by alloying with Si and Al.[1,21] It
or Al levels. The microalloying additions in TRIP has been shown that 1.5 wt pct Si can retard cementite
steels[24–26] and in the steels processed through quench- formation during bainitic transformation, while less
ing–partitioning–tempering process[27,28] have shown to than 0.38 wt pct is ineffective for the same.[36] Although
enhance the strength through grain refinement and Al is also added for the same purpose in TRIP steel, it
precipitation hardening. Although the Q&P treatment has been shown to be less effective during Q&P.[21,37,38]
on microalloyed steels has been performed by some Considering these facts, in the present investigation, Si
researchers,[29–33] there is a lack of published literature content has been restricted to 0.5 wt pct to avoid
focusing on Q&P steel involving microalloying elements, harmful effects of rolled-in scale and brittleness[22,23] as
particularly Ti, V, and B. well as to prevent carbide formation.
In view of the above, the present investigation aims to A refined microstructure improves the abrasion resis-
study the microstructural evolution during nonisother- tance[39,40] and impact toughness.[15,40,41] The refinement
mal partitioning from different quench temperatures, for of prior austenite grains through microalloying addition
low-Si steel involving microalloying elements like Ti, V is well known, and this improves both strength and

Table I. Chemical Composition (Weight Percent), Carbon Equivalent (CE), and Ms Temperature of the Investigated Alloys

Sample C Mn Si Cr Mo Ni V Ti
Alloy-1 0.16 1.10 0.50 0.20 0.10 0.50 0.030 —
Alloy-2 0.21 1.47 0.50 0.20 0.10 0.55 — 0.025

Sample P S N Al B Fe CE Ms (C)
Alloy-1 0.029 0.012 0.0095 0.016 — bal. 0.44 425.9
Alloy-2 0.021 0.009 0.0048 0.020 0.001 bal. 0.55 392.6

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 1—Thermodynamic calculations showing evolution of carbide/nitrides of microalloying elements with respect to temperature for (a) Alloy-1
and (b) Alloy-2.

ductility simultaneously.[41,42] Out of all the microalloy- in salt bath furnace atmosphere ranged from 17 C/h for
ing elements, V is cost effective and obviates the harmful QT of 170 C to 56 C/h for QT of 370 C.
effect of nitrogen in solid solution by forming precipi- The variation of retained austenite content with QT
tates.[42] Furthermore, the presence of V in Q&P steel was calculated using the model developed by Speer
has been shown to increase the fraction of retained et al.[45] (Figure 3). To cover a broad range of retained
austenite and to increase the strength and ductility.[26,29] austenite content, different QTs were selected that are
Hence, V was added in the Alloy-1. In the Alloy-2, Ti shown by vertical arrows in Figure 3.
was added in a stoichiometric amount such that it Samples were austenitized at 1200 C for 10 minutes
consumes all the nitrogen and boron remains freely followed by quenching to selected QTs (namely 170 C,
available for hardenability improvement. As depicted in 210 C, 250 C, 290 C, 330 C, and 370 C) in a salt
Figure 1(b), Ti carbonitrides are stable up to 1200 C, bath and holding there for 30 seconds to achieve
which is the typical temperature in industries for temperature homogenization. This was followed by
reheating of cast steel slabs. The presence of Ti extremely slow cooling in a salt bath furnace atmo-
carbonitrides prevents the austenite grain growth during sphere. To get the fully martensitic microstructure, few
austenitization prior to rolling.[15,24] samples were directly quenched in water after
To avoid ferrite, pearlite, and bainite formation austenitization.
during quenching, austenite stabilizers such as Mn and
Ni are added.[43] The addition of Ni and Mo helps in
improving the impact toughness[40] and gives rise to III. EXPERIMENTAL METHODS
significant improvement in hardenability when used in
combination (Ni + Mo).[44] Considering the fact that The designed alloys were melted in a vacuum induc-
abrasion resistant steels are generally produced in larger tion furnace and cast in a cast-iron mold in the form of
thickness, boron is added in Alloy-2 to obtain a further ingots (40 kg). The ingots were cut into small pieces
increase in hardenability and to ensure martensitic (10 9 10 9 6 cm3), and each piece was homogenized at
microstructure throughout the cross section.[40,44] To 1200 C for 2 hours followed by open die forging to a
achieve a given martensite to austenite ratio, the quench plate of dimension 220 9 120 9 18 mm3. The samples
temperature generally increases with increase in Ms for salt bath treatment and mechanical testing were cut
temperature. A high quench temperature enhances the from these forged plates. All the microstructural anal-
kinetics of carbon partitioning due to faster diffusion yses, after heat treatment, were carried out at the center
Therefore, industrially produced hot-rolled coil with of the sample.
high heat content will show efficient carbon partitioning. The phase identification of the heat-treated samples
Also, a low quench/coiling temperature is difficult to was done by analyzing the samples on Bruker D8
achieve industrially on run-out table. Hence, to achieve Advance X-ray diffractometer (XRD). In order to
high Ms temperature, the content of alloying elements is remove the deformed surface layer, which arose during
restricted. grinding, the samples were electropolished with a 90:10
The nonisothermal partitioning involves diffusion of ethanol–perchloric acid solution. The samples were
carbon from martensite to austenite during slow cooling analyzed in the 2h range from 40 to 100 deg with a
from quench temperature (QT) to room temperature step size and scan time per step of 0.02 and 5 seconds,
(RT). The cooling profile of a sample, in furnace respectively. Cu-Ka radiation with Ni filter was used for
atmosphere surrounding a salt bath (see Figure 2(a)), XRD analyses. The material analysis using diffraction
was recorded using a K-type thermocouple. As depicted (MAUD) software was employed for quantitative phase
in Figure 2(b), this shows a reasonable match with the analysis. The carbon content in the retained austenite
cooling profile of a hot-rolled coil.[11] The cooling rates was calculated using Eq. [1].[2]

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 2—(a) Schematic showing the setup used for recording the thermal profile of sample in salt bath furnace atmosphere, and (b) comparison of
cooling profiles of salt bath furnace atmosphere and hot-rolled coil.

Charpy impact specimens of dimensions

10 9 10 9 55 mm3 were prepared in accordance with
EN 10045-1 standard and tested using a 300 J charpy
impact tester. The tensile samples were prepared accord-
ing to the ASTM E8M standard with a gage length of
32 mm and gage diameter of 6.25 mm. The tensile tests
were carried out using the universal tensile machine of
100 kN capacity at a strain rate of 103 s1. Dry sand
rubber wheel (DSRW) abrasion experiments were car-
ried out as per ASTM G 65-04 procedure B using dry
abrasion test rig AR-50 machine (Make: DUCOM,
Bangalore, India). The abrasion-tested samples were
cleaned with acetone in an ultrasonic cleaning bath
before and after the tests, and weight loss was measured.
This was further converted to volume loss in order to
nullify the density difference among different materials.
Fig. 3—Variations of the theoretically calculated retained austenite The samples for mechanical testing were prepared such
content with quench temperatures for Alloy-1 and Alloy-2. that principal direction of the forging was parallel to the
length of charpy specimen, the gage length of tensile
specimen, and the width of wear specimen. At least three
tests on each condition were performed, and the average
ao ¼ 3:555 þ 0:044Xc ; ½1 of these values have been calculated.
where Xc is the carbon concentration in wt pct, and ao is
the lattice parameter of the austenite in Å.
The hardness measurement was done using EMCO IV. RESULTS AND DISCUSSIONS
Test DuraScan Vickers hardness testing machine at
9.8 N load with a dwell time of 10 seconds. The A. Retained Austenite and Hardness with Quench
reported hardness value is the average of at least five Temperatures (QTs)
separate measurements. The XRD profiles of Q&P-treated samples are
The samples for microstructural analysis were prepared depicted in Figure 4. The samples from Alloy-1,
using standard metallographic technique, etched with 2 quenched at 250 C followed by cooling in water, air,
pct nital solution and examined under FEI Nova Nano and salt bath furnace atmospheric conditions, were
scanning electron microscope (SEM) 430 operated at analyzed to quantify the retained austenite. Figure 4(a)
15 kV. Elemental distribution maps were captured using shows that the slowest cooling in a salt bath furnace
wavelength-dispersive spectroscopy (WDS) attached to a atmosphere condition exhibits the presence of all the
JEOL JXA 8230 electron probe microanalyzer (EPMA). peaks of retained austenite (marked by arrows),
In order to confirm the morphology of the retained whereas, water quenching (WQ) or air cooling gives
austenite in the sample, electron backscattered diffraction rise to very small first austenite peak only. This behavior
(EBSD) and JEOL JEM-2200FS transmission electron is attributed to the longer duration for carbon diffusion,
microscope (TEM) were used. The samples for TEM at relatively higher temperature, during slow cooling.[33]
measurements were prepared by mechanical grinding to The hardness values are about 238, 255 and 326 HV for
thickness ranging from 60 to 80 lm followed by twin jet salt bath furnace atmosphere-cooled, air-cooled, and
polishing, with 10 pct perchloric acid and 90 pct WQ-treated samples, respectively. The low hardness in
methanol solution, at about – 30 C. slow cooled sample is attributed to the higher amount of

METALLURGICAL AND MATERIALS TRANSACTIONS A

 partitioning. The retained austenite peaks have not been
observed in Q&P-treated samples of Alloy-2
(Figure 4(c)), at any of the QTs. However, QT of
290 C depicts a small lift at first austenite peak
position, as marked by the arrow. The absence of
retained austenite in Alloy-2 is due to tempering
reaction dominating over carbon partitioning to austen-
ite. Hence, the Alloy-2 did not respond to nonisothermal
partitioning process. The XRD investigation by Ghali
et al.[46] showed that with an increase in boron content,
the martensite phase became more ordered and
restricted the migration of carbon atoms from marten-
site to austenite. Also, the precipitation of boron carbide
at grain boundaries consumes some amount of car-
bon.[47] Öhlund et al.[48] have demonstrated that TiC
precipitates at the martensite lath boundaries during the
tempering reaction. In addition, Ti is a cementite
stabilizer. Therefore, the presence of Ti and B in Alloy-2
might have affected the kinetics of carbon partitioning
to austenite.
The variation of hardness and retained austenite
content with QTs for the investigated alloys are given in
Table II. Alloy-1 depicts retained austenite for most of
the QTs. However, the experimentally determined
retained austenite content is incommensurate with the
predicted value. This observation is consistent with the
recent findings.[2,9,11,12] This deviation is due to the
model assumptions and the fact that Ms temperature
was calculated empirically. The maximum amount of
retained austenite is achieved at QT of 250 C, which
corresponds to the lowest hardness value. The observed
variation in hardness with QTs is attributed to different
retained austenite content, carbide formation due to
tempering as well as formation of secondary martensite,
if any. The carbon content in experimentally observed
retained austenite was calculated using Eq. [1] and was
found to be about 1.34, 1.24, 1.27 and 1.34 wt pct at
QTs of 170 C, 210 C, 250 C, and 290 C, respec-
tively. The Alloy-2 does not show any retained austen-
ite, and hence, the variation in hardness with QTs is due
to the tempering of martensite and formation of
secondary martensite, if any. In general, the hardness
value decreases with the increase in QT, which is a
typical behavior of tempered martensite.[43] The hard-
Fig. 4—XRD profiles of (a) Alloy-1 quenched to 250 C followed by ness of Alloy-1 and Alloy-2 in as-quenched condition
carbon partitioning in different cooling mediums. Salt bath furnace are 430 and 495 HV, respectively. Due to the presence of
atmosphere-treated samples after quenching to different QTs for (b)
Alloy-1 and (c) Alloy-2. fully martensitic microstructure in the as-quenched
condition, these values are higher than that of the
Q&P-treated samples.
retained austenite as well as self-tempering. Based on
these findings, salt bath furnace atmosphere was chosen
B. Microstructures
for carbon partitioning after quenching to different
temperatures between Ms and Mf. 1. SEM analysis
The XRD results of Q&P-treated sample of Alloy-1 The microstructures of Alloy-1, obtained after differ-
(Figure 4(b)) confirm the presence of retained austenite ent heat treatments, are shown in Figure 5. The WQ
for QTs of 170 C, 210 C, 250 C, and 290 C. How- sample shows lath-type martensitic microstructure
ever, QTs close to Ms (such as 330 C and 370 C) do (Figure 5(a)). The microstructures after Q&P treatment
not stabilize any austenite despite relatively enhanced at QTs of 370 C, 250 C, and 170 C are depicted in
partitioning kinetics at these temperatures. The possible Figures 5(b) through (d), respectively. The QT close to
reason for this behavior could be the fact that large Ms (i.e., 370 C) does not show any feature of retained
initial austenite fraction after quenching might result austenite. The reason for such behavior is already
in insufficient carbon enrichment in austenite after discussed in Section IV–A. However, the intermediate

METALLURGICAL AND MATERIALS TRANSACTIONS A

QT (i.e., 250 C) and lower QT (i.e., 170 C) samples exact nature of these films has been discussed later in the
reveal thin films as well as blocky areas (white features) EBSD and TEM results.
in the microstructure. As observed in XRD analysis Figure 6 shows the scanning electron micrographs of
(Table II), QT of 250 C leads to the maximum amount the Alloy-2. Similar to Alloy-1, the WQ sample shows
of retained austenite in Alloy-1, which is also evident a fully martensitic microstructure (see Figure 6(a)).
from the microstructural analysis (Figure 5(c)). The Figures 6(b) through (d) illustrate the microstructural
magnified view of the highlighted part of Figure 5(c) is development after Q&P treatment at 370 C, 250 C,
presented in the inset. The EDS analysis across the thin and 170 C temperatures, respectively. The microstruc-
white region shows a jump in carbon concentration. The tures at all the QTs depict the presence of fine carbides

Table II. Retained Austenite (RA) Content and Hardness with QTs for Investigated Alloys

Alloy-1 Alloy-2

Hardness Predicted Experimental Percent C Hardness Predicted Experimental

QT (C) (HV) Percent RA Percent RA in RA (HV) Percent RA Percent RA
RT (WQ) 430.0 ± 5.2 — — — 495.0 ± 3.1 — —
170 337.0 ± 4.2 6.0 5.6 1.34 478.5 ± 6.2 8.6 ND
210 354.8 ± 6.3 9.3 2.6 1.24 473.0 ± 4.9 13.4 ND
250 238.6 ± 3.8 4.1 7.8 1.27 409.4 ± 4.2 5.2 ND
290 254.8 ± 7.6 1.7 6.6 1.34 364.4 ± 4.8 2.5 ND
330 311.5 ± 8.0 1.2 ND — 398.0 ± 1.8 1.8 ND
370 235.6 ± 2.9 1.0 ND — 320.7 ± 5.0 1.7 ND
RT room temperature, ND not detected.

Fig. 5—Scanning electron micrograph of Alloy-1 under (a) WQ condition; Q&P-treated condition at (b) 370 C; and (c) 250 C (inset showing
magnified view of the marked area and carbon concentration analyzed using EDS) and (d) 170 C.

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 6—Scanning electron micrograph of Alloy-2 under (a) WQ condition; Q&P-treated condition at (b) 370 C; (c) 250 C, and (d) 170 C.

Fig. 7—EPMA analysis of Alloy-1 Q&P-treated at 250 C. (a) secondary electron image and (b) carbon distribution map.

(white areas in the microstructures), which is due to Figure 7(b) represents the carbon distribution map
tempering reaction dominating over carbon partitioning analyzed using WDS at step size and dwell time of
to austenite. This, in turn, reduces the available carbon 0.16 lm and 150 ms, respectively. In this figure, two
for austenite stabilization. Likewise, the amount of distinct morphologies of the high-carbon regions can be
precipitates decreases with lowering of QT. observed. The area to the left of PAGB appears to be
decorated with thin-film-like microstructure, whereas,
2. EPMA analysis that on the right shows mostly blocky morphology.
EPMA-WDS analysis was carried out to understand These features are further substantiated by EBSD and
the carbon distribution in the sample from Alloy-1, TEM analysis.
Q&P-treated at QT of 250 C. Figure 7(a) shows the Elemental distribution map for the sample of Alloy-2,
secondary electron (SE) image, where the presence of Q&P-treated at 250 C, is depicted in Figure 8. The
prior austenite grain boundary (PAGB) is indicated. microstructure contains fine precipitates (white in color)

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 8—EPMA analysis of Alloy-2 Q&P-treated at 250 C. (a) secondary electron image and (b) carbon distribution map.

Fig. 9—EBSD analysis for Alloy-1 Q&P-treated at 250 C. (a) secondary electron image; (b) corresponding inverse pole figure (IPF) of austenite
phase; (c) image quality (IQ) map of high-magnification scan; and (d) corresponding IPF of austenite phase.

within the grain interiors (see Figure 8(a)). The carbon 3. EBSD analysis
distribution map in Figure 8(b) indicates that these are EBSD micrographs of Alloy-1, Q&P-treated at
the regions of high-carbon concentration. However, the 250 C, are shown in Figure 9. The inverse pole fig-
composition of individual precipitates cannot be con- ure (IPF) map for austenite phase, corresponding to
firmed due to the limited resolution of the EPMA. Figure 9(a), is depicted in Figure 9(b). This confirms the

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 10—EBSD Analysis for Alloy-2 Q&P-treated sample at 250 C. (a) secondary electron image and (b) corresponding phase map for
austenite.

Fig. 11—TEM analysis of Alloy-1 Q&P-treated at 250 C. (a) brightfield micrograph; (b) darkfield micrograph showing the presence of thin films
between martensitic laths; and (c) selected area diffraction (SAD) pattern from the same region confirming the presence of both austenite and
carbides.

Table III. Mechanical Properties of Alloy-1 and Alloy-2 under Water-Quenched and Q&P-Treated Conditions at 250 °C

Alloy-1 Alloy-2

Mechanical Properties Water Quench Q&P at 250 C Water Quench Q&P at 250 C
2
Charpy impact toughness at RT (J/cm ) 52.0 ± 6.0 89.0 ± 10.0 30.0 ± 2.0 38.0 ± 6.0
Abrasive wear volume loss (mm3) 278.0 ± 9.0 350.0 ± 17.0 265.0 ± 4.0 248.0 ± 4.0
UTS (MPa) 1257.0 ± 17.0 652.0 ± 10.0 1524.0 ± 4.0 940.0 ± 11.0
YS (MPa) 989.0 ± 21.0 466.0 ± 4.0 1187.0 ± 31.0 704.0 ± 18.0
Percent total elongation 11.7 ± 1.5 26.3 ± 1.6 13.4 ± 0.5 17.7 ± 1.6

presence of block type retained austenite, as marked in and (d) show the corresponding image quality and IPF
green color. It is observed that the retained austenite is phase map of austenite, respectively. These austenite films
uniformly distributed throughout the microstructure are shown in green color in Figure 9(d). Like blocky-type
and has a definite orientation relationship with the austenite, thin films also possess a single orientation
grain. The thin-film-type features inside the encircled within a grain. The black regions in Figures 9(b) and (d)
part in Figure 9(a) are not indexed as retained austenite, correspond to martensite.
possibly because of limited instrumental resolution at As discussed earlier, the Q&P-treated sample from
such low magnification.[7] At higher magnification, these Alloy-2 does not reveal any retained austenite, when
thin films are indexed as retained austenite. Figures 9(c) investigated by XRD. In order to reconfirm this fact, the

METALLURGICAL AND MATERIALS TRANSACTIONS A

 phase map, as marked by arrows. However, the amount
of austenite is not enough for detection by XRD and
therefore, austenite peaks were not detected in XRD
(Figure 4(c)).

4. TEM analysis
Figure 11 shows the transmission electron micro-
graph of Alloy-1, Q&P-treated at 250 C. The bright-
field and darkfield images from the same region
(Figures 11(a) and 11(b), respectively) reveal the pres-
ence of thin-film-like features between martensitic laths.
The darkfield image was taken using the ð20 2Þ diffrac-
tion spot of the austenite phase. The corresponding
SAD pattern (Figure 11(c)) confirms that these are
austenite films possessing a ð011Þa ð111Þc type K–S
orientation relationship with adjacent martensite.[49]
The diffraction spots belonging to e-carbide of [0001]
zone axis are also present.[50]

C. Mechanical Properties
The mechanical properties are presented in Table III.
The Q&P-treated sample of Alloy-1 shows a high value
of room temperature (RT) charpy impact toughness,
which is attributed to the presence of retained austenite,
low-carbon martensite and carbides. The retained
austenite suppresses the propagation of microcracks
and continuously absorbs dislocations from adjacent
martensite, which in turn leads to the improvement in
ductility and impact toughness.[51,52] However, the
Alloy-1, in WQ condition, shows reduced impact
toughness due to its fully martensitic microstructure.
The Alloy-2 exhibits a lower impact toughness for both
the WQ and the Q&P-treated conditions. This is due to
the higher carbon content compared with Alloy-1 and
the inability of the alloy to respond to the Q&P
treatment.
The abrasive wear volume loss for both the alloys, in
WQ condition, is comparable. This similarity in their
wear resistance is attributed to their fully martensitic
microstructure. However, the Q&P-treated sample from
Alloy-1 shows an increased wear loss, which might be
due to its lower hardness in comparison with the WQ
sample. The Q&P-treated sample of Alloy-2 depicts
lowest wear loss amongst all the treatment conditions.
This is attributed to the presence of hard carbide
particles, as a result of tempering, and TiN
precipitates.[15]
The engineering stress–strain curves for both the
Fig. 12—Tensile results (a) engineering stress–strain plot; (b) alloys are shown in Figure 12(a). The alloys show the
Crussard–Jaoul (C–J) plot for all the alloys; and (c) comparison of highest strength in WQ condition. The lower strength of
work hardening behaviors of Alloy-1 under WQ and Q&P-treated
conditions. the Alloy-1 is attributed to the low-carbon content in
comparison with the Alloy-2. The strength of the
Alloy-1 drops to about half after Q&P treatment due
same sample was scanned through EBSD. Figure 10(a) to the presence of retained austenite, low-carbon
shows the secondary electron image, and the corre- martensite and carbides, and shows a corresponding
sponding phase map for austenite is depicted in increase in elongation.[51,52] The Q&P-treated sample of
Figure 10(b). Red and green colors in Figure 10(b) Alloy-2 also demonstrates a drop in strength along with
elucidate the austenite and martensite phases, respec- an increase in elongation, which is due to its tempered
tively. Small islands of austenite were observed in the microstructure compared with WQ condition.

METALLURGICAL AND MATERIALS TRANSACTIONS A

 The work hardening behavior of ferritic, pearlitic, Q&P-treated sample could sustain work hardening up
martensitic, tempered martensitic, and dual-phase steels to a larger strain compared with WQ sample.
(in the present case, it is martensite and austenite) can be
distinguished by differential Crussard–Jaoul (C–J) anal-
D. Fractography
ysis,[53,54] which is based on the following equations:
The fracture and worn surfaces of charpy impact- and
r ¼ r0 þ k  en ½2 wear-tested samples, respectively, were examined under
SEM to determine the prevalent fracture and wear
dr mechanisms in Alloy-1. Figure 13 depicts the frac-
ln ¼ lnðk  nÞ þ ðn  1Þ  ln e; ½3 tograph of the charpy tests performed on sample of
de
Alloy-1. As shown in Figure 13(a), fracture surface of
where the slope of the lnðdr=deÞ vs ln e plot yields WQ-treated sample of Alloy-1 is dominated by dimples
(n  1), and the value of work hardening exponent (n) is of different sizes. This indicates involvement of ductile
calculated as (slope + 1). mode of fracture and hence, results in good impact
Figure 12(b) represents the C-J plots for both the toughness value of 52 J/cm2. Figure 13(b) shows the
alloys from YS to UTS. It can be seen that both the fracture surface of the Alloy-1, Q&P-treated at 250 C.
alloys in WQ condition, with fully martensitic The presence of fine and uniformly distributed dimples,
microstructure, depict a very similar trend. The tem- compared with WQ sample, indicates the activation of a
pered microstructure of the Q&P-treated sample from large number of nucleating sites for microvoids, which
Alloy-2 reveals a higher slope (i.e., less negative) than in turn signifies higher plastic deformation.[55] An
that obtained for the martensitic microstructure. The enlarged image of the marked area, shown in the inset,
Q&P-treated sample from Alloy-1 depicts a still higher indicates the involvement of shear-type deformation. All
slope indicating higher work hardening, which might be these observations justify a high impact toughness value
due to the presence of both the retained austenite and of 89 J/cm2 for Q&P-treated sample of Alloy-1. The
the low-carbon martensite. Figure 12(c) differentiates macroscopic images (in the inset of both the figures)
the behavior of Alloy-1 under WQ (full martensite) and depict the flat fracture surface for WQ sample, while
Q&P (low-carbon martensite, retained austenite and showing a rough surface (due to higher deformation
carbides)-treated conditions. The work hardening expo- prior to fracture) for Q&P-treated sample.
nent (slope + 1) and the transition strain, correspond- Figure 14 depicts the worn surfaces of Alloy-1 after
ing to different stages, are also indicated in the figure. abrasion testing. The macroscopic examination (in the
The Q&P-treated sample exhibits three different stages inset of both the images) of worn surface illustrates wear
of work hardening. The presence of retained austenite, scars of rectangular shape with uniform depth, confirm-
along with low-carbon martensite and carbides, led to ing the proper alignment during wear testing. The
positive work hardening values at all the stages. It starts scanning electron micrograph in Figure 14(a) corre-
decreasing with the increasing strain, which is associated sponds to WQ condition, i.e., fully martensitic
with the start of yielding of hard phase, i.e., martensite microstructure. The formation of scratches or grooves
and strain-induced transformation of retained austenite. parallel to wear track is indicative of plowing mecha-
The WQ sample from Alloy-1 demonstrates two differ- nism of material removal.[2] Figure 14(b) shows the
ent work hardening stages. The negative work harden- worn surface of the Q&P-treated sample of Alloy-1. The
ing value at both the stages is due to the presence of microstructure exhibits very rough surface, pointing
hard martensite in the microstructure.[54] Also, the toward a local fracture causing formation of microchips

Fig. 13—Macroscopic (inset) and microscopic views of the fracture surface of Alloy-1 samples tested for charpy impact toughness at room
temperature for (a) WQ and (b) Q&P-treated at 250 C (inset showing magnified image from the marked area).

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 14—Macroscopic (inset) and microscopic views of the worn surfaces of Alloy-1 under (a) WQ condition and (b) Q&P-treated at 250 C.

as well as spalling through fragmentation mechanism of austenite was not observed on the worn surfaces, indicating
wear.[2] The XRD scan on worn surface did not show the occurrence of TRIP effect during wear. A further
any peak of retained austenite. Hence, it can be optimization of retained austenite morphology and distri-
concluded that retained austenite is mechanically unsta- bution may alter its stability.[3,4] This may provide a better
ble and therefore, transforms to hard martensite during product in terms of abrasion resistance, impact toughness,
wear indicating the occurrence of TRIP effect. and strength. In contrast, the Ti- and B-containing alloy
The foregoing results clearly indicate that austenite (Alloy-2), after Q&P treatment, depicted higher abrasion
retention is possible by nonisothermal carbon partitioning resistance but was limited by lower impact toughness. This
during slow cooling, akin to that observed for a hot-rolled is attributed to the fact that the hardness of tempered
coil. Therefore, this process can significantly improve the martensitic microstructure in Alloy-2 remained high com-
economics, associated particularly with quenching and pared with the Q&P-treated Alloy-1.
tempering or isothermal partitioning process. So far as the Another important aspect that needs consideration is
compositional design of steel is concerned, low-Si (0.5 wt that the present investigation did not involve any hot
pct) V microalloyed steel results in austenite stabilization deformation prior to quenching from 1200 C. However,
along with self-tempering during nonisothermal partition- industrially accepted practice is to quench from tempera-
ing. However, microalloying with Ti and B in a similar tures typically in the range of 900 C to 950 C after finish
alloy (with increased carbon and Mn) led to tempered rolling. Hence, the presently investigated alloys have large
martensitic microstructure with an insignificant amount of prior austenite grains, in comparison to that generally
retained austenite during nonisothermal partitioning. This obtained after hot rolling. In addition, considering the
could be due to several reasons such as (i) ordering of prediction of Thermo-Calc at 1200 C (Figure 1(b)), Ti
martensite phase due to B,[46] (ii) precipitation of boron carbonitride will be fully stable, whereas V carbonitride
carbides at grain boundaries,[47] and (iii) TiC precipitation will dissolve and V will go into solid solution. During
at the martensite lath boundaries during the tempering quenching from 1200 C, therefore, V carbonitride is not
reaction.[48] For V-containing alloy (Alloy-1), the experi- expected to precipitate. However, in the industrial pro-
mentally found retained austenite amount differ slightly cessing, it is likely to precipitate during deformation at the
from the predicted values. This is due to the fact that the temperatures below ~ 1000 C (Figure 1(a)). Hence, the
prediction is based on certain assumptions[45] and Ms is incorporation of hot-rolling deformation prior to quench-
calculated using empirical equation.[35] The presence of ing will definitely result in grain refinement, which may
retained austenite and carbides led to reduced hardness of alter the kinetics of transformation and precipitation
steel in comparison with fully martensitic microstructure. hardening.[11] This can further enhance the mechanical
Both the alloys, under water-quenched condition, resulted properties; particularly, the abrasion resistance, impact
in higher strength and abrasion resistance but were limited toughness and strength for the similar composition and
by low impact toughness and work hardening due to fully heat-treatment conditions.[56]
martensitic microstructure. However, the Q&P treatment
of V-containing alloy engendered better impact toughness
and work hardening at the expense of its strength and a
slight decrease in abrasion resistance. The decrease in V. CONCLUSIONS
strength and abrasion resistance is attributed mainly to the
presence of retained austenite and carbides in the Two different alloys with low-Si content were pro-
microstructure. The purpose of having retained austenite cessed through (i) quenching and nonisothermal parti-
in tempered martensitic matrix for improved impact tioning (Q&P) and (ii) direct water quenching (WQ) to
toughness and good abrasion resistance due to TRIP effect room temperature. The major findings of this study are
is fulfilled. It has already been mentioned that retained as follows:

METALLURGICAL AND MATERIALS TRANSACTIONS A

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