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Materials Science & Engineering A 677 (2016) 505514

Contents lists available at ScienceDirect

Materials Science & Engineering A


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

Analysis of the mechanical behavior of a 0.3C-1.6Si-3.5Mn (wt%)


quenching and partitioning steel
Farideh HajyAkbary a,b,n, Jilt Sietsma b, Goro Miyamoto c, Naoya Kamikawa d,
Roumen H. Petrov e, Tadashi Furuhara c, Maria J. Santomia b
a
Materials innovation institute (M2i), Delft, The Netherlands
b
MSE Department of Materials Science and Engineering, TU Delft, Delft, The Netherlands
c
Institute for Materials Research, Tohoku University, Sendai, Japan
d
Intelligent Machines and System Engineering, Hirosaki University, Hirosaki, Japan
e
Department of Materials Science and Engineering, Ghent University, Ghent, Belgium

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

Article history: A 0.3C-1.6Si-3.5Mn (wt%) steel was subjected to different Q&P treatments, leading to different combi-
Received 15 June 2016 nations of initial martensite, bainite, secondary martensite, and retained austenite. In this study, initial
Received in revised form martensite refers to the martensite formed during the initial quenching step and then subjected to an
20 September 2016
isothermal treatment at 400 C; secondary martensite refers to martensite formed during quenching
Accepted 21 September 2016
Available online 22 September 2016
from 400 C to room temperature. The yield strength of each constituent phase was determined by
applying physical models to the data obtained from detailed microstructural characterization. The yield
Keywords: strength (uncertainty of 5%) of the Q&P microstructures was calculated by using a composite law to
Quenching and partitioning steels account for the contribution of each constituent phase. The dependence of the yield strength on the
Yield strength
microstructural features of the Q&P microstructures was revealed by using the approach developed in
Strengthening mechanism
this work. For example, initial martensite (which has a high yield strength and is the dominant phase in
Dislocation density
Martensite the microstructures) had the greatest effect on the yield strength of the Q&P microstructures. Further-
more, the phase fraction and dislocation density of this phase increased with decreasing quenching
temperature, leading to an increase in the yield strength of the material.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction microstructures. The yield strength of each phase is controlled by the


type of crystal and the defects in the crystal [4]. Knowledge of these
During the "Quenching and Partitioning" (Q&P) process, initial defects (for example, dislocations, precipitates, solute atoms, and
martensite is formed by rapidly quenching an austenitic micro- grain boundaries) is crucial for determining the yield strength of a
structure to temperatures lower than the martensite-start tempera- phase. However, owing to the complex assembly of phases in Q&P
ture (Ms). This is followed by an isothermal treatment, where carbon steels, quantitative analysis of the strengthening contribution asso-
is partitioned from supersaturated martensite to austenite, and nal ciated with each phase is challenging. Therefore, most studies have
quenching [1]. Secondary martensite may form during nal focused on the qualitative relation between the phase fraction and
quenching, if some austenite regions are insufciently stabilized. the mechanical properties of the material [5,6].
Furthermore, isothermal martensite [2] or bainitic ferrite [3] may In this study, the strengthening contributions from disloca-
form during the isothermal holding step. Accordingly, Q&P micro- tions, grain boundaries, precipitate, and solute atoms are ac-
structures are composed of initial martensite (M1), isothermal mar- counted in calculating the yield strength of the constituent phases
tensite, bainite, secondary martensite (M2), and retained austenite comprising the Q&P microstructures of a 0.3C-1.6Si-3.5Mn (wt%)
(RA). Knowledge of the yield strength of each constituent phase and steel. These contributions are determined by applying a composite
the respective contribution to the overall yield strength of the ma- law, with the aim of identifying the key microstructural para-
terial is essential for tailoring the yield strength of the Q&P meters that determine the yield strength of the Q&P steels.

n
Corresponding author.
E-mail addresses: f.hajyakbary@tudelft.nl (F. HajyAkbary), 2. Theoretical calculation of the yield strength
j.sietsma@tudelft.nl (J. Sietsma), mmiyamoto@imr.tohoku.ac.jp (G. Miyamoto),
kamikawa@hirosaki-u.ac.jp (N. Kamikawa), roumen.petrov@ugent.be (R.H. Petrov),
furuhara@imr.tohoku.ac.jp (T. Furuhara), The yield strength of the Q&P microstructures can be calculated
m.j.santomianavarro@tudelft.nl (M.J. Santomia). by considering the contribution of each constituent phase. This

http://dx.doi.org/10.1016/j.msea.2016.09.087
0921-5093/& 2016 Elsevier B.V. All rights reserved.
506 F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514

calculation is performed on the basis of a composite law, which is considered as the effective grain sizes that control the yield
given as follows: strength of bainite and martensite, respectively. The grain
i
boundary strengthening of each phase (gb ) is determined from the
yc = yif i ,
(1) Hall-Petch equation:
i
KHP
where yc , yi , i
and f are the yield strength of the Q&P micro- i
gb = ,
i
structure, yield strength of phase i ( i M1, bainite, M2, and RA), dgb (8)
and volume fraction of the phase, respectively. i
where is the effective grain size of martensite or bainite. A Hall-
dgb
Petch slope, KHP , of 210 MPa mm has been reported for both
2.1. Yield strength of martensite and bainite
bainite and martensite [13].
The summation of the strengthening components can be cal-
2.1.3. Precipitate strengthening
culated as follows [7]: i
The contribution from precipitate strengthening, pcpt (MPa), is
2 2 expressed as [14]:
yi = ( ) + ( )
i
A
i
B (2)
i i
where i denotes M1, bainite or M2; A and B are associated with i 0. 538Gb f pcpt dpcpt
pcpt = ln 2b ,
the forest dislocations and the particles, respectively, and are de- i
dpcpt
(9)
ned as follows:
i i
where dpcpt : average diameter of the precipitates, f pcpt : volume
Ai = 0 + ssi + gb
i
fraction of precipitates, G : shear modulus (G 76 GPa for lath
Bi = pcpt
i
+ i (3) structure with high dislocation density [14]), and b: length of the
Burgers vector.
where 0 : lattice friction stress of pure bcc Fe, ssi : solid solution
i i
strengthening, gb : grain boundary strengthening, pcpt : precipitate 2.1.4. Dislocation strengthening
strengthening, and i : dislocation strengthening. In some studies, The contribution of dislocations to the yield strength of phase i ,
precipitate strengthening is considered the same as that resulting i , can be approximated by the Taylor equation:
from obstacles (i.e., particles) and therefore its contribution is
added to Ai [8]. However, in this study, by considering that mobile i = MGb i , (10)
dislocations are unable to distinguish between precipitates and i
where : geometrical constant, M : Taylor factor, and : dislocation
forest dislocations, the contribution from precipitate strengthen-
density in phase i . Here, M 2.73 [15] and 0.25 [16].
ing is added to the contribution from dislocation strengthening.

2.1.1. Solid solution strengthening 2.2. Retained austenite


The solid solution strengthening of each phase ( ssi ) consists of
contributions from both interstitial carbon atoms and substitu- Owing to the high Si concentration, cementite formation in
tional atoms: austenite is prevented during isothermal holding at 400 C. Fur-
thermore, RA has a low dislocation density and therefore, solid
ssi = Ci + st , (4) solution hardening and grain boundary strengthening are con-
sidered the main factors that determine the yield strength of RA.
where Ci
and st are the solid solution strengthening from carbon
The yield strength (MPa) of RA ( yRA ) is determined from the fol-
atoms and substitutional atoms, respectively. Non-partitioning of
lowing empirical relation [17]:
the substitutional elements is assumed during the formation of
bainite and martensite and, hence, these elements have with the
same concentration in both phases. The solid solution strength-
(
yRA=15. 4 4. 4 + 23XCRA +1. 3XSiRA +0. 24XCr
RA RA
+0. 94XMo +32XNRA )
0. 46
ening from carbon, in MPa, is determined as follows [9]: + ,
dRA (11)
1/2
Ci =1720 XCi ( ) , (5) where X jRA and dRA are the concentration (wt%) of element j ( j C,
Si, Cr, Mo, N) in RA and the grain size (mm) of RA, respectively. This
where XCi
(wt%) is the concentration of solute carbon in phase i .
For carbon concentrations higher than 0.2 wt%, Eq. (5) over- equation is typically used for steels with alloying concentrations of
estimates ci and, in this case, XCi (wt%) is determined from [10]: up to 26 wt% [17].

1/3
Ci =1170 XCi ( ) , (6)
3. Experimental procedure
where XCi is in wt% and Ci is in MPa. The solid solution
strengthening from substitutional atoms, in MPa, is given as fol- Cylindrical 10 mm (length)  3.5 mm (diameter) specimens
lows [11]: were machined parallel to the hot-rolling direction of 0.3C-1.6Si-
3.5Mn (wt%) steel sheets. The specimens were austenitized at
st =83XSi +32XMn 31X Cr +39X Cu , (7)
900 C for 180 s, and then quenched to 25 C, 180 C, 200 C, and
where Xj is the concentration (wt%) of element j ( j Si, Mn, Cr, 220 C at a cooling rate of 20 C s  1. Afterwards, the specimens
and Cu). This equation has been used for steels with alloying were isothermally treated at 400 C for 0 s, 5 s, 10 s, 50 s, 100 s, and
concentrations of 45 wt% [11]. 200 s and subsequently quenched to room temperature in a Bhr
DIL 805 A/D dilatometer. The resulting specimens were designated
2.1.2. Grain boundary strengthening as QTxxx-y, where xxx-y denotes a specimen quenched to xxx C and
The bainite plate size [12] and martensite block size [13] are isothermally treated at 400 C for y seconds. A QT260-5 specimen
F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514 507

was used to investigate the microstructural properties of marten- 4. Results


site. The volume fractions (uncertainty of 70.02 [3]) of initial
martensite ( f M1), bainite ( f B ), and secondary martensite ( f M2 ) were 4.1. Volume fraction and carbon concentration of the constituent
calculated by applying the lever rule to the dilatometry data ob- phases
tained during the initial quenching, isothermal holding, and nal
Fig. 1 shows that three dilatations occur after the austenitization
quenching steps, respectively. Electron backscatter diffraction
step of the QT220-200 specimen. The rst dilatation starts at 288 C,
(EBSD) measurements were performed via orientation imaging
i.e., the Ms temperature of the steel, and continues until the
microscopy (OIM) on a FEI Nova 600 Nanolab dual-beam (focused quenching temperature (220 C) is reached. The second and third
ion beam) FEG-SEM. The QT260-5 specimen was subjected to in- dilatations occur during isothermal holding and nal quenching,
place EBSD and SEM analysis. During this process, EBSD analysis which are associated with the formation of bainitic ferrite and sec-
was performed, the carbon contamination on the surface of the ondary martensite, respectively. Although the rst and third dilata-
specimen was subsequently removed (via ne polishing), and SEM tions occur in all specimens, the second dilatation occurs only in
analysis was then conducted. Post-processing analysis of EBSD data specimens quenched to 220 C and isothermally treated at 400 C for
having a condence index of 40.2 was performed by using the 10 s, 50 s, 100 s, and 200 s.
TSLs software. Selected specimens were observed with a trans- The QT25-0 (directly quenched) specimen consists of marten-
mission electron microscope (TEM; Philips CM300) operated at site and carbides (see Fig. 2a). Furthermore, as in the case of the
QT180-5 specimen (see Fig. 2b), the microstructures of the QT180,
300 kV; details of this examination are provided elsewhere [3].
QT200, and QT220 specimens consist of an internally etched phase
Atom probe measurements were carried out at Tohoku Uni-
with carbide precipitates (M1), a blocky phase (M2), and thin lms
versity, using a LEAP 4000HR (CAMECA Co.) in voltage-pulse
of RA. The occurrence of carbide in the as-quenched specimen
mode. The experiments were performed at an average detection
indicates that the carbides in M1 resulted from the auto tempering
rate of 1% and a pulse fraction, pulse rate, and base temperature of of martensite during the initial quenching step [3].
20%, 200,000 Hz, and 80 K, respectively.
Three series of X-ray diffraction (XRD) measurements were 4.1.1. Initial martensite
performed; (a) a continuous-scan to determine the volume frac- Austenite peaks were absent from the XRD spectra of the QT25
tion of RA ( f RA ) and the carbon concentration of RA ( XCRA ). The f RA specimens and therefore these specimens were assumed to be
and XCRA values were calculated by using the method described in fully martensitic with carbide precipitation. Regarding the occur-
[18]. (b) Stop-scan XRD analysis to estimate the dislocation density rence of carbide in martensite, the volume fraction of martensite
of martensite. (c) In-situ XRD analysis to investigate the me- was determined by subtracting the volume fraction of carbide
chanically induced martensite during tensile deformation. This from unity: the results are shown in Table 2. Based on the large
fraction of carbide in these specimens, it was assumed that most of
analysis was performed on at tensile specimens having a gauge
the carbon precipitated as carbide and the concentration of solid-
length and cross section of 3 mm and 0.8  0.8 mm2, respectively.
solution carbon is 0.05 wt%.
The measured integral area of the peaks was corrected because the
The volume fraction of M1 ( f M1) in the QT180, QT200, and
XRD beam irradiated an area of 4  3 mm2, which is larger than QT220 specimens (see Table 2) was determined from dilatometry
the at surface of the tensile specimen. This correction was per- data. Several 3D-APT measurements were performed on the
Am
formed by using the relation Ac = sin
, where is the Bragg angle; QT180-5 and QT180-200 specimens in order to determine the
Am and Ac are the measured and the corrected area, respectively carbon concentration of the solid solution in M1 ( XCM1). These
[19]. Details of the XRD tests are provided in Table 1. specimens do not contain bainitic ferrite (next subsection) and M1
In order to determine the tensile properties of the Q&P mi- is the only low-carbon phase. Therefore, regions with a carbon
crostructures, tensile specimens having a gauge length and cross concentration lower than the average carbon concentration of the
section of 3 mm and 0.8  0.8 mm2, respectively, were prepared steel were considered M1. Fig. 3 shows two carbon maps, which
reveal the M1 in the QT180-5 and QT180-200 specimens. The
from specimens treated in the dilatometer. The specimens quen-
carbon concentration of both specimens was measured along the
ched to 180 C, 200 C and 220 C were tested by using a AG-
axis of the cylinders. A loss of Fe ions during the 3D-APT
100kNX plus tensile test machine, where the tensile elongation is
measured by a charge-coupled device (CCD) camera. Tensile test-
ing of the specimens quenched to room temperature was per-
formed on a Deben Microtest machine, where the strain is de-
termined from the crosshead displacement. The inuence of the
machine compliance on the strain was corrected in accordance
with a previous study [20]. Moreover, the tensile tests were all
performed at an initial strain rate of 2  10  3 s  1.

Table 1
Details of XRD measurements performed for different applications.

Application 2 range Filament Step size Counting


time

Determining f RA and XCRA 30135 Co 0.05 5s


Dislocation density of 40150 Cu 0.02 10 s
martensite
Mechanical stability of 45107 Co 0.05 1s
austenite
Fig. 1. Dilatometry curve of the QT220-200 specimen.
508 F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514

Fig. 3. 3D atom probe tomography map of carbon atoms in the QT180-5 and
QT180-200 specimens.

4.1.2. Bainite
The phase transformation associated with the isothermal holding
of the Q&P process of this steel has previously been investigated [3].
In that work, the fraction of formed phase was perfectly predicted by
the simulation of bainitic-ferrite formation. Therefore, in the present
work, it is assumed that bainitic ferrite is the only phase formed
during isothermal holding. Bainite formation is negligible in the
QT180 and QT200 specimens, but is quite pronounced in the speci-
mens quenched to 220 C. In fact, the fraction of bainite in the QT220
specimens increases with increasing isothermal holding time; the
volume fraction of bainite ( f B ) in these specimens is shown in Ta-
ble 2. Furthermore, owing to the low solubility of carbon in ferrite,
Fig. 2. SEM micrographs of the (a) QT25-0 (as-quenched) and (b) QT180-5 specimens. the carbon concentration of bainite is assumed to be zero.

Table 2
4.1.3. Secondary martensite
Volume fractions of initial martensite, bainite, secondary martensite, retained The volume fraction of M2 ( f M2 ) in the QT180, QT200, and
austenite (uncertainty of measurements: approximately 7 0.02) and carbide QT220 specimens was determined from dilatometry data obtained
(uncertainty: 70.05). during the nal quenching step. In some cases, the summation of
Partitioning time (s)
the calculated phase fractions is greater than unity. Therefore, to
fM f fB fM fRA
1 2 normalize the total fraction to unity, f M2 was calibrated by ap-
QT25 0200 0.95 0.05 0 0 0 plying a multiplication to each phase fraction; the corresponding
QT180 5 0.79 0.02 0 0.04 0.15 results are shown in Table 2. A maximum value of 0.02 (which lies
10 0.79 0.02 0 0.03 0.16 within the range of uncertainty of the measurements) was ob-
50 0.79 0.02 0 0.01 0.18 tained for the difference between the calibrated fraction of M2 and
100 0.79 0.02 0 0.02 0.17
200 0.79 0.02 0 0.02 0.17
the fraction calculated from dilatometry. The carbon concentration
QT200 5 0.74 0.01 0 0.07 0.19 of M2 was determined from the dilatometry data and by applying
10 0.74 0.01 0 0.08 0.18 the method described in [3]. Moreover, the carbon content of M2
50 0.74 0.01 0 0.04 0.22 and other phases ( C i ) can be obtained from: C i = f i XCi , where XCi is
100 0.74 0.01 0 0.03 0.23
the carbon concentration of phase i (i M1, RA, M2, and B). Fig. 4a
200 0.74 0.01 0 0.04 0.22
QT220 5 0.65 0.01 0 0.18 0.17 c show the C M2 of the QT180, QT200, and QT220 specimens, re-
10 0.65 0.01 0.01 0.14 0.2 spectively. M2 has a high carbon concentration, i.e., TEM analysis
50 0.65 0.01 0.03 0.09 0.23 revealed highly deformed twin-containing martensite grains,
100 0.65 0.01 0.04 0.08 0.23
which are considered M2. Fig. 5a shows an example of an M2 grain
200 0.65 0.01 0.05 0.06 0.24
in the QT180-200 specimen. M2 is un-tempered martensite and,
hence, carbide cannot be detected in the TEM micrographs. As
measurements leads to an overestimation of the concentration such, the carbon in M2 is assumed to be in solid solution.
and, hence, the values were corrected by using the method de-
4.1.4. Retained austenite
scribed in [21]. This yielded a value of 0.05 7 0.01 wt% for the
Table 2 lists the f RA of the QT180, QT200, and QT220 specimens.
corrected concentration of solid-solution carbon in M1 of the
The carbon concentration of RA ( XCRA ) in these specimens was
QT180-5 and QT180-200 specimens. SEM micrographs reveal a
determined via XRD analysis. The corresponding C RA are shown in
high fraction of carbides in the QT180, QT200, and QT220 speci-
Fig. 4ac, respectively.
mens. In addition, the carbon partitioning simulations predict that
most of the solid-solution carbon partitions to austenite during the 4.1.5. Carbide
initial stage of isothermal holding [3]. Therefore, a XCM1 of Selected Area Diffraction (SAD) analysis of carbides in the
0.05 70.01 wt% is also assumed for these specimens. QT180-5 and QT180-200 specimens indicates that M1 contains -
F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514 509

Fig. 5. (a) Bright eld TEM image of twins and (b) dark eld TEM micrograph of -
carbide in the QT180-200 specimen.

crystals. The rejection of Si to the surrounding volume is essential


for the growth of cementite nuclei. However, the nucleation and
growth of -carbide are not inuenced by Si [3].
The volume fraction of -carbide (Fe2.2C) can be determined
from the amount of carbon in the precipitates. As such, the carbon
content of M1 was calculated by subtracting the carbon content of
the other phases from the carbon content of the steel (C =0.3 wt%);
i.e.C M1=C C RA C M2 C B . In the case of the QT25 specimens, f RA =0
Fig. 4. Carbon content of phases in the (a) QT180, (b) QT200, and (c) QT220 specimens.
and, hence, C M1=0.3 wt% for these specimens. Fig. 4ac show the
C M1 of the QT180, QT200, and QT220 specimens, respectively. The
carbide [3]. This suggests that negligible cementite formation oc- carbon content of initial martensite (see Fig. 4) includes both
curred during isothermal holding and most of the carbides are - carbon in the precipitates and in solid solution. The amount of
carbides that formed during the initial quenching. Therefore, the carbon in the precipitates was determined by subtracting the
carbides in the Q&P specimens are considered -carbide, indicating amount of solid solution carbon from C M1. Table 2 lists the calcu-
that Si retards the kinetics of cementite formation in steels, but lated volume fractions of -carbide. An average diameter of
has negligible inuence on the kinetics of -carbide formation. The 207 5 nm was obtained for the -carbides, based on dark eld
difference in the inuence of Si on cementite and -carbide for- TEM analysis of the QT180-200 specimen (see example in Fig. 5b)
mation is attributed to the fact that Si is insoluble in cementite and TEM analysis of the other specimens.
510 F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514

Fig. 6. (a) Combined IQ and phase map of the QT260-5 specimen; black boundaries correspond to misorientation higher than 15; green grains and red grains are RA and martensite
(M1 and M2), respectively. (b) Distribution of grain average IQ of BCC grains, (c) SEM micrograph, and (d) combined IQ and phase map of the selected region in Fig. 6a. In Figs. 6b and
6d, yellow and blue denote M2 and M1, respectively. (For interpretation of the references to color in this gure legend, the reader is referred to the web version of this article.)

4.2. Grain size characterization of the phases To determine the actual block size of the grains, the normal direc-
tion of the specimen must be perpendicular to the habit plane of the
Fig. 6a shows a combined grain average Image Quality (GAIQ) grain. Therefore, the measured block size ( dl ) must be corrected using
and phase map of the QT260-5 specimen. In this map, RA grains d = d sin , where d is the actual size [13]; is the angle between the
l l l
and martensite grains (both M1 and M2) are shown in green and normal of the lath habit plane ((0 1 1)M//(1 1 1)A, M: martensite, A:
red, respectively. The RA grains have a blocky morphology. How- austenite) and the normal of the specimen surface. This parameter ( )
ever, thin lms of RA occur between the martensite grains. These can be determined from EBSD analysis and is used, in the present
lms have grain sizes that are smaller than the step size of EBSD
work, to determine the block sizes of M1 and M2 in the QT180-5,
(50 nm) and are therefore undetectable, leading to an under-
QT180-200, and QT220-5 specimens. The block sizes were determined
estimation of the RA fraction [22].
for ve initial austenite grains of each specimen. Sizes of 0.970.1 mm
Tempering of M1 during isothermal holding reduces the carbon
and 0.470.1 mm were obtained, and designated as the block sizes of
concentration and dislocation density of M1 to values lower than
M1 and M2, respectively, in the QT180, QT200, and QT220 specimens. A
those associated with M2. Consequently, M1 and M2 can be clas-
block size of 0.470.1 mm was obtained for martensite in the QT25
sied as regions with high-GAIQ and low-GAIQ, respectively [23].
The GAIQ of martensite in the region shown in Fig. 6a was de- specimens. This value is the average size of grains, in the QT25-5
termined (see Fig. 6b) in order to develop an approach for iden- specimen, which have misorientation higher than 15.
tifying M1 and M2 on the basis of their GAIQ. Subsequently, based Owing to the tempering of M1 during the isothermal annealing
on the SEM micrograph of the selected region in Fig. 6c, the GAIQ step, M1 and bainitic ferrite have low carbon concentration.
of the M1 and M2 grains in Fig. 6b was designated by blue and Therefore these phases exhibit similar contrast in SEM and TEM
yellow, respectively. Fig. 6b conrms that most of the M1 grains images as well as similar GAIQ during EBSD analysis, leading to
have higher GAIQ than M2 grains. However, as shown in Fig. 6b, difculty in distinguishing the phases. A thickness of 0.17 mm is
the GAIQ distributions of M1 and M2 overlap in a narrow region. assumed for the bainite plates in the QT220 specimens. This is the
Fig. 6d shows the corresponding microstructure, where green, thickness of bainitic ferrite plates formed at 400 C in a steel with
blue, and yellow denote the respective RA, M1, and M2 grains. A chemical composition (0.27C-1.98Si-2.18Mn wt%) [24] similar to
comparison of Fig. 6c and d indicates that M1 and M2 can be that of the studied steel. The thickness of bainite plates in silicon-
identied from the GAIQ distributions as grains with high-GAIQ rich steels is determined by the strength of austenite at the
and low-GAIQ, respectively. transformation temperature and the chemical free energy change
F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514 511

accompanying the transformation. These factors are both de- concentration of steel leads to a maximum dislocation density of
termined by the chemical composition of the steel. 4.1  1015 m  2; further increases result in the formation of twins and
Average RA grain sizes of 0.4 mm, 0.45 mm, and 0.5 mm were a decrease in the dislocation density [26]. Moreover, the strength-
estimated from EBSD analysis of specimens quenched to 180 C, ening mechanisms are only slightly inuenced by ne internal
200 C, and 220 C, respectively. twinning in plates of martensite [27]. Therefore, the inuence of
twins on the yield strength of M2 is not considered in the current
4.3. Dislocation density of initial martensite, bainite, and secondary study.
martensite The dislocation density of bainitic ferrite ( B (m  2)), which
forms at temperatures of 300650 C, can be determined as fol-
XRD peaks corresponding to M1 and M2 overlap in the QT180 and lows [28]:
QT200 specimens and in the QT220 specimens the peaks of M1, M2, 15845 4100000
and bainite overlap. The volume fractions of M2 and bainite are B = 2 109 exp ,
T T2 (12)
signicantly lower than that of M1 and consequently the full width at
half maximum (FWHM) of the peaks is attributed to the dislocation where T is the isothermal holding temperature in K. An isothermal
density of M1. In this study, the dislocation density was calculated holding temperature of 400 C yields a dislocation density of
from the peak broadening by using the method described in [25]. 4  1015 m  2, which is similar to the dislocation density of initial
Fig. 7a shows the dislocation density of martensite in the QT25 martensite. However, bainite has a very low carbon and therefore the
specimens and M1 in the QT180, QT200, and QT220 specimens as a dislocation density of bainitic ferrite should be lower than that of M1.
function of the quenching temperature. As the gure shows, the This conict may be resolved by considering that the austenite, which
dislocation density of martensite decreases with increasing quench- gives rise to bainitic ferrite, has a higher carbon concentration than the
ing temperature or increasing isothermal holding time. austenite that gives rise to initial martensite. This is due to the fact that
Martensite in the QT25-0 specimen and M2 in the QT180, QT200, kinetics of carbon partitioning is faster than that of bainitic ferrite
and QT220 specimens were formed by quenching to room tem- formation and, hence, austenite receives carbon prior to bainite for-
perature. These phases were not isothermally treated. Therefore, the mation [3]. Accordingly, austenite that gives rise to bainitic ferrite is
dislocation density of M2 is considered equal to that of martensite in harder than the austenite, which gives rise to initial martensite. The
the QT25-0 (directly quenched) specimen, although the carbon calculated dislocation density of bainitic ferrite is therefore consistent
concentration of the former is higher than that of the latter. This with the fact that the bainitic ferrite is almost carbon-free.
assumption is based on the fact that increasing the carbon
4.4. Yield strength of the microstructures

Fig. 7b shows the 0.2% offset yield strength of the specimens as


a function of the quenching temperature. As the gure shows, the
yield strength decreases with increasing quenching temperature
while increasing the quenching temperature from 25 C to 180 C
have a signicant effect on the strength. However, the yield
strength is insensitive to the isothermal process associated with
each quenching temperature.

4.5. Mechanical stability of retained austenite

The mechanical stability of RA was determined by measuring


the volume fraction of RA during microtensile testing of the
QT180-5 and QT180-200 specimens (see Fig. 8). Prior to yielding,
the volume fraction of RA decreases by 0.03, which is considered
negligible in the current study.

5. Discussion

5.1. Contribution of the strengthening mechanisms in martensite and


bainite

5.1.1. Lattice friction stress


A value of 41 MPa [29] is adopted for the lattice friction stress
( 0 ) in M1, bainite, and M2; 0 of the QT220-200 specimen is
shown in Fig. 9.

5.1.2. Solid solution strengthening


A value of 0.05 wt% was assumed for the concentration of solid-
solution carbon in martensite of the QT25 specimens and M1 of the
QT180, QT200, and QT220 specimens. The solid solution strengthening
by carbon ( C ) was estimated by substituting this value into Eq. (5).
However, the carbon concentration in bainite is assumed to be zero and,
hence, C in bainite is zero. The contribution of C in M2 was calculated
Fig. 7. Effect of the quenching temperature on the (a) dislocation density of mar- by inserting the carbon concentration of M2 into Eq. (6). Fig. 9 shows
tensite and (b) yield strength of the Q&P specimens. the C values of M1 and M2 in the QT220-200 specimen.
512 F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514

lattice parameter (a) of ferrite was determined from XRD analysis of


a
the specimens. Substituting this value into 2 111 , the Burgers vector
in ferrite was yielded a value of 0.248 nm. Fig. 9 shows the strength
contribution of -carbide precipitate in the QT220-200 specimen.

5.1.5. Dislocation strengthening


As Fig. 7a shows, the dislocation density of martensite decreases
with increasing quenching temperature, as reported in a previous
study [30]. In that work, the quenching process was interrupted and
the dislocation density of martensite was measured via in-situ neu-
tron diffraction. The supplementary deformation of martensite and
austenite increases with decreasing quenching temperature and in-
creasing fraction of martensite. This increased deformation leads to
an increase in the hardness of the material and, hence, the shear
stress required for the formation of new martensite crystallites in-
creases. Consequently, the dislocation density of the newly formed
martensite crystallites increases with decreasing quenching tem-
perature [30]. As in previous studies [31,32], the dislocation density
Fig. 8. Effect of the applied stress on the volume fraction of RA in the QT180-5 and
of M1 decreases gradually during the isothermal holding step (see
QT180-200 specimens.
Fig. 7a). The contribution of dislocation strengthening in M1, M2, and
bainite was calculated by inserting the corresponding dislocation
density into Eq. (10). Fig. 9 shows the dislocation strengthening
contribution in M1, M2, and bainite of the QT220-200 specimen.

5.2. Estimation of the yield strength of the constituent phases

The yield strengths of M1, bainite, and M2 in the QT180, QT200,


and QT220 specimens (see Fig. 10ac, respectively) were determined
from Eqs. (2) and (3). Among these phases, M2 has the highest
concentration of solid-solution carbon and dislocation density and, in
turn, the highest yield strength. In addition, strengthening-mechan-
ism contributions in M2 occur at similar levels in all specimens and
therefore the yield strength of this phase varies (17501860 MPa)
only slightly. In contrast, the yield strength of M1 varies from 1340 to
1590 MPa, 12901460 MPa, and 10801200 MPa in the QT180, QT200
and QT220 specimens (see Fig. 10), respectively. Owing to the higher
dislocation density (Fig. 7a), the yield strength of M1 in specimens
quenched to lower temperature is higher than that of M1 in speci-
mens quenched to higher temperature. Fig. 10c indicates that the
Fig. 9. Contribution of the strengthening mechanisms to the yield strength of M1, yield strength (1121 MPa) of bainite in the QT220 specimens is in-
bainite, and M2 in the QT220-200 specimen. dependent of the isothermal holding time. Fig. 10ac show the yield
strength of RA in the QT180, QT200, and QT220 specimens, respec-
Owing to the low diffusivity of substitutional elements at tively, as determined from Eq. (11). As the gures show, RA has the
400 C, the concentration and, consequently, solid solution lowest yield strength (124131 MPa) of all the phases. This yield
strengthening (st ) of these elements in M1, bainite, and M2 are the strength represents the yield strength of RA with blocky morphology.
same for all of the specimens. The st in M1, bainite, and M2 was The dislocation density of interlath RA is higher than that of blocky
calculated by inserting the chemical composition of the steel into austenite and, hence, the yield strength of interlath austenite is
Eq. (7). The st value of the QT220-200 specimen is shown in Fig. 9. higher than that calculated for blocky austenite. However, EBSD
analysis revealed that the RA has mainly blocky morphology and
5.1.3. Grain boundary strengthening interlath RA constitutes a fraction of o0.04. Therefore, the inuence
M1
The contribution of grain boundary strengthening in M1 ( gb ) of RA on the yield strength is accurately determined by using the
M2
values associated with the blocky morphology.
and M2 ( gb ) in the QT180, QT200, and QT200 specimens was es- The yield strength of each specimen is also included in Fig. 10.
timated by inserting the corresponding block sizes (0.9 mm and The specimens have lower yield strengths than M1, bainite, and
0.4 mm, respectively) into Eq. (8). Similarly, the contribution of grain M2, thereby conrming that RA has signicant inuence on the
B
boundary strengthening in bainite ( gb ) was calculated by inserting mechanical properties of these steels.
the thickness of the bainitic ferrite plates (0.17 mm) into Eq. (8).
M1 M2 B
Fig. 9 shows the gb , gb , and gb of the QT220-200 specimen. The 5.3. The yield strength of the Q&P specimens
block size of martensite (0.4 mm) in the specimens quenched to
M
25 C was inserted into Eq. (8), and gb was thereby calculated. The yield strength of each QT25 specimen was determined from
Eqs. (2) and (3) and compared with the measured values (see
5.1.4. Precipitate strengthening Fig. 11a). This gure reveals that the calculated yield strength (as
The contribution of -carbide precipitate strengthening was de- determined from Eq. (2)) of the martensitic structures deviates by 2%,
termined by inserting the volume fraction (see Table 2) and the which is within the experimental uncertainty, from the measured
average diameter (20 nm) of -carbide precipitates into Eq. (9). The value. The yield strength of the QT180, QT200, and QT220 specimens
F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514 513

Fig. 11. (a) Comparison of the calculated and the measured yield strength and
(b) contributions of the different phases to the yield strength of the Q&P specimens.

Although M2 has the highest yield strength of the constituent phases,


this phase accounts for a small volume fraction of each micro-
structure and, therefore, contributes only modestly to the yield
strength. Bainite accounts for a small volume fraction of the QT220
specimens and, hence, contributes only slightly to the yield strength.
However, initial martensite has a high yield strength and accounts for
the highest volume fraction of all the phases. Therefore, this phase
has the highest contribution to the yield strength. This indicates that
controlling the strength and fraction of M1 is essential for tailoring
the yield strength of the Q&P microstructures.

6. Conclusions

The dependence of the yield strength on the microstructural


characteristics of Q&P microstructures was investigated and the
following conclusions were drawn, based on the results obtained:
Fig. 10. The yield strength of the constituent phases and the total yield strength of
the (a) QT180, (b) QT200, and (c) QT220 specimens.
 The contribution of the strengthening mechanisms to the yield
is calculated by inserting the volume fraction (Table 2) and yield strength of the constituent phases (initial martensite, secondary
strength (Fig. 10) of each phase into Eq. (1). As Fig. 11a shows, the martensite, bainite, and retained austenite) was determined by
calculated yield strength corresponds closely (5% deviation) to the applying physical models. The accuracy of the model used to
measured yield strength. Fig. 11b shows the contribution of each calculate the yield strength of martensitic and bainitic struc-
phase to the yield strength of the Q&P microstructures. Owing to its tures was determined by comparing the calculated and mea-
low yield strength and the low amount of martensite formed prior to sured yield strength values of tempered martensite specimens.
yielding (Fig. 8), RA has the lowest contribution to the yield strength. The results showed that the model estimates the strength of the
514 F. HajyAkbary et al. / Materials Science & Engineering A 677 (2016) 505514

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Acknowledgments [18] M.J. Santomia, L. Zhao, R.H. Petrov, C. Kwakernaak, W.G. Sloof, J. Sietsma,
Microstructural development during the quenching and partitioning process
in a newly designed low-carbon steel, Acta Mater. 59 (2011) 60596068.
This research was carried out under project number M41.10.11437 [19] A.J. Kolk, Is Retained Austenite Controlling the Mechanical Properties of Q&P
Steels?, (Master thesis)2014, Delft University of Technology, Netherland.
in the framework of the Research Program of the Materials innova-
[20] F. HajyAkbary, M.J. Santomia, J. Sietsma, Elastic strain measurement of
tion institute M2i (www.m2i.nl). The support of Tata Steel RD&T is miniature tensile specimens, Exp. Mech. 54 (2014) 165173.
gratefully acknowledged. M.J. Santomia gratefully acknowledges the [21] G. Miyamoto, K. Shinbo, T. Furuhara, Quantitative measurement of carbon
nancial support of the European Research Council under the Eur- content in FeC binary alloys by atom probe tomography, Scr. Mater. 67 (2012)
9991002.
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grant agreement number 306292, Netherlands Organization for Sci- diffraction techniques to quenched and partitioned steels, Microsc. Microanal.
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[23] M.J. Santomia, L. Zhao, R.H. Petrov, J. Sietsma, Microstructural analysis of
(STW) through Vidi-grant number 12376. martensite constituents in quenching and partitioning steels, Mater. Charact.
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