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To cite this article: G. A. Thomas & J. G. Speer (2014) Interface migration during
partitioning of Q&P steel, Materials Science and Technology, 30:9, 998-1007, DOI:
10.1179/1743284714Y.0000000546
Download by: [Indian Institute of Technology Madras] Date: 23 June 2017, At: 02:36
Interface migration during partitioning of Q&P
steel
G. A. Thomas* and J. G. Speer
The quenching and partitioning (Q&P) process for heat treatment of steel has previously been
shown yield to good combinations of strength and ductility owing to the presence of martensite
and austenite. Interface mobility has been discussed in previous literature, mostly related to local
driving forces. The present work considers the migration of the martensite/austenite interface in
two steels (containing CMnSiMo or CNiSiMo). Experimental data show clear evidence of interface
migration in the CMnSiMo steel during partitioning treatments at temperatures between 200 and
400uC for times ranging from 30 to 1000 s; conversely, the interface in the CNiSiMo steel was
stationary during the same partitioning treatments. The different behaviours observed are
considered in the context of differences in interface mobility and driving forces, and it appears
that interface crystallography differences could influence the partitioning behaviour of Q&P steels.
Keywords: Quenched and partitioned steel, Q&P, Interface migration, Martensite, Austenite, Orientation relationships
This paper is part of a special issue on Adventures in the Physical Metallurgy of Steels
martensite and later towards the austenite (i.e. austenite X-ray diffraction (XRD) was used to measure the
growth followed by martensite growth). retained austenite fraction and estimate the carbon
The movement of the martensite/austenite interface in content of austenite before and after the partitioning
the direction of martensite is perhaps consistent with treatments. XRD was performed at room temperature
classically observed ‘reversion’ (the literature is not clear with nickel filtered copper radiation using a Phillips X-
whether ‘reversion’ refers only austenite growth by shear pert diffractometer operating at 45 kV and 40 mA and
mechanisms or if interface migrations by diffusional equipped with an X’celerator detector with a 1u slit.
processes are also included12–14,30–37). Martensite reversion Samples were prepared by grinding to remove surface
to austenite has been reported to occur by growth of oxides with 60, 120, 240, 300, 400 and 600 grit silicon
existing austenite or by nucleation of new austenite and carbide papers. The grinding step introduces work into
subsequent growth; in which the former would result in the sample that might alter the XRD measurement; to
reversed austenite of the same orientation as the parent avoid the detrimental effects of grinding, the samples
austenite10 and the latter might cause austenite to be were chemically thinned for approximately 15 min in a
formed with orientations that are different than the parent water cooled container of 10 parts water, 10 parts 30%
austenite from which martensite formed.10,11 Growth of hydrogen peroxide and 1 part hydrofluoric acid.
austenite might occur by an athermal shear mechanism Samples were scanned through a 2h range from 40 to
(i.e. martensitic ‘reverse’ transformation) or by a thermally 105u over a total scan time of about 21 min. Filtered
activated diffusional mechanisms (i.e. short range diffusion copper radiation was used and four austenite peaks
across the martensite/austenite interface).12 The dominant ({111}, {200}, {220} and {311}) and four ferrite/
mechanism depends on the temperature and the heating martensite peaks ({110}, {200}, {211}, {220}) were
rate; where high heating rates are reportedly associated quantified and the austenite fraction was estimated using
with shear transformations11,12 and low heating rates are the SAE method.19 The carbon content of the as
c
typically associated with thermally activated diffusion quenched austenite (Cquenched ) was assumed to be that
mechanisms.12,13 In either case, the reversed austenite of the bulk alloy. The carbon content of austenite after
c
typically has a high density of defects14 (although austenite partitioning treatments (Cpartitioined ) was calculated from
formed by shear mechanisms may have a higher defect the change in lattice parameter relative to the as
density as compared to that formed by diffusional quenched condition according to the equation20–22
growth12). It has been hypothesised that the reversed
c c ac {aco
austenite is more stabile than the parent austenite (i.e. Cpartitioined ~Cquenched z : (1)
resistant to transformation back to martensite) due to 0 00453
hindering of martensitic growth by the recovered sub-grain where ac is the lattice parameter of austenite after the
structure of the reversed austenite.10,12 partitioning treatment and aco is the lattice parameter of
Diffusional interface migration is reported to occur by austenite in the as quenched condition. Unless otherwise
one of two mechanisms. The first is a step or ledge noted, all data were collected from unique samples
mechanism15 which occurs for coherent and semicoher- which were each subjected to partitioning treatments for
ent interfaces with relatively low index orientation the times and temperatures indicated.
relationships and habit planes; this mechanism usually EBSD was used to characterise the microstructures
displays start–stop growth behaviour due to the before and after partitioning, to identify phases (auste-
necessity of critical nucleation events.15–17 The second nite and ferrite/martensite) present in the microstruc-
is the massive transformation which involves continuous ture, observe the morphology of austenite and provide
or stepwise growth. The structure (e.g. coherency) of the orientation information useful for understanding micro-
martensite/austenite interface may partially govern the structural evolution. EBSD analyses were performed
mobility of the interface. Ma and Pond18 have modelled using a JEOL-7000F FESEM. Samples were polished
martensite/austenite and suggest that the interface is with 6, 3 and 1 mm diamond slurries. The final step
semicoherent and can migrate by glissile motion of before EBSD data collection involved vibratory polish-
transformation dislocations at the interface. The present ing using 0?05 mm colloidal silica. The samples were
work aimed to understand the role of interface structure tilted 70u (with respect to horizontal) towards the
on interface mobility. camera used to collect EBSD patterns. Owing to the
tilting of the sample, the working distance (approxi-
Procedure mately 15 mm) varied with position; therefore, dynamic
focus control was used to focus the entire image during
Two steels were studied in this work, containing 0?31C– data collection. The accelerating voltage was 20 kV. The
13?95Ni–1?91Si–0?24Mo (wt-%) or 0?27C–8?31Mn– step size for EBSD data collection was 50 nm using a
1?94Si–0?25Mo (wt-%); the steels were designated as hexagonal grid pattern. EDAX-TSL OIM Data
‘14Ni steel’ and ‘8Mn steel’ respectively, due to the Collection 5?1 software was used to collect and index
elevated nickel or manganese levels. The steels were the Kikuchi band patterns and TSL OIM Data Analysis
laboratory cast and hot rolled to 2?54 mm thickness. 5?1 software was used to analyse the results obtained
Salt pots were used to heat treat the material according from EBSD. Post-processing cleaning routines were not
to the Q&P heat treatment process. The samples were employed (unless otherwise noted).
austenitised at 875uC for 300 s and the quenched into
water to room temperature. Some samples were left in
this as quenched condition for examination. Other
Results
samples were reheated to 200, 300 or 400uC and held The austenite fractions and austenite carbon content
for 30, 60, 100 or 1000 s. This is referred to as the estimated from XRD are shown for both steels in Fig. 1
partitioning step. After the partitioning step, the samples as a function of partitioning time (Pt). As seen Fig. 1a,
were quenched in water to room temperature. relative to the as quenched condition (i.e. Pt50 s), the
1 XRD results as a function of partitioning time. a, c Austenite fractions for 8Mn and 14Ni steel respectively. b, d
Austenite carbon contents for 8Mn and 14Ni steel respectively. With exception of the closed symbols in a, all data
were collected from unique samples subjected to partitioning treatments for the times and temperatures indicated. The
closed symbols in a were collected from a single sample that was heat-treated cumulatively for the indicated time at
400uC
austenite fractions of the 8Mn steel increased signifi- partitioning time. The increase in austenite fraction
cantly with increasing partitioning time after partition- must be the result of either growth of existing austenite
ing at 200, 300 or 400uC. The higher partitioning or nucleation of new austenite and subsequent growth.
temperatures resulted in a greater increase in the The austenite fractions measured from the 14Ni steel
austenite fraction for the partitioning times examined. were essentially stabile with partitioning times up to
To verify that the increase in austenite fraction observed 1000 s for partitioning temperatures of 200, 300 or
was a real effect and not an artefact of the experimental 400uC, as shown in Fig. 1c. In this regard, the behaviour
method, a single sample was subjected to a cumulative of the 14Ni steel was in contrast to the 8Mn steel, but
partitioning treatment in which the austenite fraction consistent with assumptions made with respect to
was measured by XRD and then the same sample was constrained carbon equilibrium (CCE).1 The austenite
heated to the partitioning temperature (PT) for the carbon content estimated from XRD are shown in
prescribed amount of time and then cooled to room Fig. 1) and d as a function of partitioning time. The
temperature for XRD analysis, and then reheated to the austenite carbon concentrations increased in both steels
partitioning temperature and so on. The results are after partitioning treatments at 300uC or higher, and the
shown as closed symbols in Fig. 1a. This procedure led effect was apparently more pronounced in the 14Ni
to a similar increase in austenite fractions with steel. However, it should be noted that the austenite
a 8Mn steel 875uCzWQ (as quenched); b 8Mn steel 875uCzWQz400uC, 30 s; c 8Mn steel 875uCzWQz400uC, 60 s;
d 8Mn steel 875uCzWQz400uC, 100 s; e 8Mn steel 875uCzWQz400uC, 1000 s; f legend
3 EBSD image qualityzphase maps of 8Mn steel: a as quenched; then partitioned at 400uC for b 30 s, c 60 s, d 100 s,
e 1000 s; f legend
Figure 6 shows inverse pole figure maps that are sometimes exhibit alternating variants. This morphology
representative of the martensite observed in each steel. has been termed ‘ladder martensite’ due to the appear-
As shown in Fig. 6a, the martensite in the 8Mn steel ance of alternating layers of twin related a9-martensite.
exhibited a morphology that consists of fine laths that This type of martensite morphology has been related to
a 8Mn steel 875uCzWQ (as quenched); b 8Mn steel 875uCzWQz400uC, 30 s; c 8Mn steel 875uCzWQz400uC, 60 s;
d 8Mn steel 875uCzWQz400uC, 100 s; e 8Mn steel 875uCzWQz400uC, 1000 s; f legend
4 Inverse pole figure maps of austenite in 8Mn steel: a as quenched, partitioned at 400uC for b 30 s, c 60 s, d 100 s,
e 1000 s; f legend. Regions that indexed as martensite regions appear black
the formation of e-martensite prior to formation of a9- highlight boundaries between laths that represent 60u
martensite.26 XRD analysis of the 8Mn steel showed rotations about a ,111.a axis which represents a low
evidence of e-martensite, suggesting that e-martensite energy twin boundary. This type of boundary was
may have preceded a9-martensite formation and yielded observed for all of the alternating laths observed in the
this characteristic morphology. In Fig. 6b, yellow lines 8Mn steel. As shown in Fig. 6c, the 14Ni steel did not
a 14Ni steel 875uCzWQ (as quenched); b 14Ni steel 875uCzWQz400uC, 100 s; c legend
5 EBSD image qualityzphase maps of 14Ni steel after a water quenching and b water quenching and partitioning at
400uC for 100 s
exhibit any of the ‘ladder martensite’ structure when The samples shown were partitioned at 400uC for 60 s.
observed via EBSD, rather a more plate-like morphol- The angular tolerance for this analysis was ¡2?5u. The
ogy was observed in which twin orientations were not angular tolerance was chosen to avoid overlap based on
observed. Further, XRD analyses did not reveal any the difference between the KS and NW orientation
evidence of e-martensite in the 14Ni steel suggesting that relations of 5?26u.28,29
a9-martensite may have formed directly from austenite. Table 3 tabulates the total line length of the afore-
Thus, the mechanisms of martensite formation and mentioned boundaries and shows the ratio of boundary
resulting structures of the martensite formed in each of lengths of KS/NW for all of the partitioning conditions
the two steels appear to be quite different. of the 8Mn steel. As seen in the table, the martensite/
Previous literature has reported different orientation austenite interfaces exhibited in the 8Mn steel were
relationships between austenite and martensite. Two predominately of the KS OR (at a ratio of about 2 : 1
commonly cited orientation relationships are the compared to the NW OR). The 14Ni steel featured the
Kurdjumov–Sachs (KS) orientation relationship and opposite behaviour, wherein the predominant OR of the
the Nishiyama–Wassermann (NW) orientation relation- martensite/austenite interfaces was of the NW OR (at a
ship (OR).27 Table 2 shows the description for these ratio of about 2 : 1 compared to the KS OR).
orientation relationships as well as associated axis–angle
pairs (an axis–angle pair describes a rotation about a
common axis necessary to bring two unit cell orienta-
Discussion
tions into coincidence).28 Figure 7 shows greyscale The results of this work have shown that the martensite/
image quality maps of each steel in which austenite is austenite interface in the 8Mn steel migrated during the
highlighted green and martensite/austenite phase bound- partitioning step. This migration was evident as a
aries associated with the KS or NW orientation significant increase in austenite fraction after partition-
relationship are highlighted red or yellow respectively. ing as compared to the as quenched condition. In
contrast, the behaviour of the 14Ni steel during
Table 1 Number of distinct austenite crystals present in partitioning treatments was very different, with of
8Mn steel in 20625 mm area measured by EBSD*
after partitioning at 400uC for times indicated
stabile austenite fractions indicative of a stationary
martensite/austenite interface. While both steels exhib-
Partitioning time/s PT5400uC ited a significant flux of carbon atoms across the
boundary, it is evident that boundary movement was
As quenched 758 prominent in the 8Mn steel but not in the 14Ni steel. On
30 748
60 544
a basic level, the difference in the behaviour of the two
100 482 steels must be the result of (1) differences in the driving
1000 572 force for austenite formation and/or (2) differences in
the mobility of the martensite/austenite interface. It is
*The EBSD data were subjected to a ‘grain dilation’ cleaning
routine to eliminate ‘noise’ from the data. The settings for the
apparent that there was a driving force for interface
grain dilation cleanup routine considered neighbouring pixels migration (e.g. austenite growth) and the interface was
that were indexed with orientations within 5u of each other and mobile at the partitioning temperatures of interest such
required that each grain be at least 2 pixels in size. that the interface could move at an appreciable velocity
7 Representative EBSD. Image quality maps (greyscale) with austenite highlighted in green and martensite/austenite
boundaries that exhibit particular orientation relationships highlighted in red (KS OR) or yellow (NW OR). Samples
were partitioned at 400uC for 60 s
Kurdjumov–Sachs (KS) {1 1 1}c//{1 1 0}a9 ,1 1 0.c//,1 1 1.a9 42.85u ,0.968 0.178 0.178.
Nishiyama–Wassermann (NW) {1 1 1}c//{1 1 0}a9 ,1 1 1.c//,1 1 0.a9 45.98u ,0.976 0.083 0.201.
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