Beruflich Dokumente
Kultur Dokumente
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.
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.
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
Table 1
Details of XRD measurements performed for different applications.
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.
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
5. Discussion
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.
6. Conclusions
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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.
opean Unions Seventh Framework Programme (FP7/2007-2013)/ERC [22] G. Thomas, J. Speer, D. Matlock, J. Michael, Application of electron backscatter
grant agreement number 306292, Netherlands Organization for Sci- diffraction techniques to quenched and partitioned steels, Microsc. Microanal.
entic Research (NWO ), and Dutch Foundation of Applied Sciences 17 (2011) 368373.
[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.
92 (2014) 9195.
[24] S.B. Singh, H.K.D.H. Bhadeshia, Estimation of bainite plate-thickness in low-
alloy steels, Mater. Sci. Eng. A 245 (1998) 7279.
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