Bainite Transformation During Continuous Cooling: Analysis of Dilatation Data

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Bainite Transformation During Continuous Cooling:

Analysis of Dilatation Data


RAVI RANJAN and SHIV BRAT SINGH

A new approach based on iteration is presented to extract the amount and composition of
bainitic ferrite and austenite from the dilatation curve. The carbon concentration of bainitic
ferrite estimated from the dilatation curve was found to be higher than the solubility of carbon
in a-ferrite that is in paraequilibrium with c-austenite, and it agreed well with the corresponding
value estimated from X-ray diffraction (XRD). A slightly better fit between the experimental
and calculated dilatation curves was obtained with body-centered-tetragonal than with
body-centered-cubic (bcc) bainitic ferrite. These results suggest that the austenite to bainitic
ferrite transformation occurs through a displacive mechanism.

https://doi.org/10.1007/s11661-017-4419-9
Ó The Minerals, Metals & Materials Society and ASM International 2017

I. INTRODUCTION In general, bainite shares many features, e.g., carbon


supersaturation, morphology, and crystallographic fea-
EVER since the discovery of bainite in steels, there tures, with martensite.[1,2,4,11,12,20] Therefore, it is often
has been an intense debate on the mechanism of its difficult to distinguish bainitic ferrite from martensite
transformation.[1,2] However, the displacive approach and quantify their relative fractions in a multiphase
has been shown to be quite appropriate and the theory microstructure through conventional microscopy.
of transformation under this framework has advanced Dilatometry can be a useful technique in such cases to
sufficiently; the quantitative theory is used extensively to detect the presence of bainite and martensite as these
design new grades of steels, such as TRIP-aided steels, transformations usually occur in different temperature
bainitic steels, and nanobainitic steels, with an encour- ranges. A dilatometer records the change in length of a
aging combination of properties.[1–10] material for a given thermal treatment. Therefore, the
Like other phases, the ability of bainite to affect the recorded data include the contribution from the thermal
final combination of properties offered by a steel effect and associated phase transformation, if any. In
depends on its volume fraction, composition, and size. general, the formation of a phase with bcc or bct crystal
There are some experimental results that indicate that structure from face-centered-cubic (fcc) austenitic phase
the carbon concentration in bainitic ferrite is higher than leads to an expansion, which is clearly reflected in the
that dictated by transformation under paraequilibrium dilatation curve. The expansion observed is propor-
condition.[11,12] At first, the measured high carbon tional to the amount of phase formed from austenite.
concentration in bainitic ferrite was attributed to carbon However, in general, this qualitative relationship alone
atoms trapped at dislocations generated as a result of is not sufficient to extract the quantitative details of the
the transformation.[10,13–15] However, recent experimen- phases involved such as their amount and the compo-
tal results obtained using three-dimensional atom probe sition. Therefore, a method is presented in this work to
studies indicate that excess carbon, over and above the extract these details from the experimental dilatation
solubility limit in body-centered-cubic (bcc) ferrite (in curve for the transformation of austenite to bainitic
equilibrium with austenite), remains in solid solution in ferrite during continuous cooling. This method was
bainitic ferrite.[11,12] Higher solid solubility of carbon in applied assuming that bainitic ferrite has (i) very small
bainitic ferrite has been attributed to a change in crystal amount of carbon or (ii) higher carbon with bcc or bct
structure from bcc to body-centered-tetragonal structure, and the results obtained in these two cases
(bct).[16–19] were compared to obtain an insight into the nature of
bainite transformation.

RAVI RANJAN and SHIV BRAT SINGH are with the Depart- A. Experimental
ment of Metallurgical and Materials Engineering, Indian Institute of
Technology Kharagpur, Kharagpur, 721302, India. Contact e-mail: A typical TRIP-aided steel with a composition (wt
ravi.ranjan.9007@gmail.com pct) of 0.20C-1.6Mn-0.5Si-1.2Al-0.25Mo-0.04Nb was
Manuscript submitted 16 August, 2017. selected for the study.[21] The as-cast material was cut to

METALLURGICAL AND MATERIALS TRANSACTIONS A


appropriate size (100 9 20 9 20 mm3) and soaked for 2 respect to li ; fp and Xp represent the volume fraction and
hours at 1473 K (1200 °C) in a muffle furnace and then mean atomic volume of phase p at any temperature,
forged in the temperature range of 1373 K to 1473 K respectively (p = ab for bainite and c for austenite),
(1100 °C to 1200 °C) giving 50 pct reduction in thick- while fic ð¼ 1Þ and Xic correspond, respectively, to the
ness. Finally, the forged material was air cooled to room volume fraction and mean atomic volume of the
temperature. A cylindrical sample with 4 mm diameter austenite at the beginning of cooling immediately after
and 10 mm length was prepared from the hot-forged the austenitization step.
material using wire electric discharge machining. The The lattice parameter(s) (mp) of a given phase p at any
thermal treatment on the cylindrical sample was per- temperature T can be calculated from
formed in Bähr 805 A/D quenching and deformation  
dilatometer having a resolution of 0.05 lm/0.05 °C. The mp ¼ m0p 1 þ bp ðT  298Þ ½2
sample was heated at 5 K/s to 1323 K (1050 °C) and
soaked for 3 minutes. The sample was then cooled at where m0p is the ambient temperature lattice parameter,
10 K/s to the ambient temperature. The selected cooling bp is the coefficient of linear thermal expansion of phase
rate was sufficient to avoid ferrite and pearlite transfor- p, and mp represents the lattice parameters (ap and cp).
mation during cooling. The continuously cooled sample Further, the mass balance up to the Ms temperature
was cut along the transverse direction in the center, and gives
the cross section was mechanically polished following
the standard procedure and etched with 2 pct nital for Cab fab þ Cc fc ¼ C0 ; fab þ fc ¼ 1 ½3
examination of optical microstructure. In addition, where Cp represents the carbon concentration of phase p
X-ray diffraction (XRD) measurement was performed and C0 ð0:2 wt pctÞ is the overall carbon content of the
to detect the presence of retained austenite in the final steel.
microstructure, if any, and to estimate the lattice The volume fraction of the phases for a given thermal
parameters of the phases present. The XRD measure- treatment can be calculated from the experimental
ment was performed with Co Ka radiation between the dilatation data (relative change in length vs temperature
2h angles of 40 and 130 deg at a step size of 0.02 deg and or time) using Eq. [1] if the mean atomic volume (Xp) is
time per step of 0.5 seconds in Bruker’s D8 Discover known. The mean atomic volume of a phase (Xp)
equipment. depends on its crystal structure and lattice .parameter(s).
3
For fcc austenite, it is given simply by ac 4, where ac is
B. Results and Discussion the austenite lattice parameter. The lattice parameter of
The experimental dilatation curve, optical microstruc- austenite at the ambient temperature (a0c ) can be
ture (2 pct nital etched), and XRD pattern of the sample calculated from its composition.[22] Three cases were
cooled at 10 K/s are shown in Figure 1. In Figure 1(a), considered in the present work for bainitic ferrite with
the critical transformation temperatures, i.e., bainite respect to its carbon concentration and crystal structure
start (BS), bainite finish (Bf), and martensite start (Ms) in view of the recent results described earlier.[16–19] In the
(of carbon-enriched austenite remaining untransformed first case (i.e., case 1), the bainitic ferrite was assumed to
after the bainite transformation), are also highlighted. have a negligible amount of carbon with a bcc crystal
These critical temperatures were taken as the points structure and the equation describing the lattice param-
where the dilatation curve deviated from the linear eter of bcc ferrite at the ambient temperature as a
thermal contraction (dashed line in Figure 1(a)) associ- function of its composition was used.[23] The bainitic
ated with the cooling of the sample. The dilatation curve ferrite in the other two cases, 2 and 3, was assumed to
indicates that the final microstructure of the sample contain higher carbon and it was determined from the
consists of a mixture of bainite and martensite with a experimental dilatation data by iteration. In case 2, the
relatively higher amount of the former. However, it was crystal structure of bainitic ferrite was taken to be bcc
difficult to distinguish these two phases from the optical and the equation proposed by Bhadeshia et al.[24] for the
microstructure (Figure 1(b)) and XRD pattern lattice parameter of bcc bainitic ferrite at the ambient
(Figure 1(c)). temperature was used where the effect of carbon is also
Assuming that the volume change associated with the incorporated along with other alloying elements. In case
austenite (c) to bainitic ferrite (ab) transformation is 3, on the other hand, it was assumed that bainitic ferrite
isotropic, it can be shown that the change in length has a bct crystal structure and its lattice parameters aab
accompanying the transformation is related to the mean and cab follow the same equations that describe the
atomic volume (Xp) and the relative amount of the lattice parameters of martensite at the ambient temper-
phases (fp) by ature as a function of its composition.[25,26] In all three
cases, it was assumed that substitutional alloying
i
Dl 1 fab Xab þ fc Xc  fic Xc elements do not partition during the course of austenite
¼ ½1 to bainitic ferrite transformation. The mean atomic
li 3 fic Xic
volume of bainitic ferrite ðXab Þ is given by a2ab cab =2 with
where li is the length of the sample at the beginning of aab ¼ cab for the bcc crystal structure.
cooling immediately after the austenitization step and Dl The first step to extract the phase evolution informa-
is the change in length at any temperature (T) with tion from the experimental dilatation data involved the

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 1—(a) Experimental dilatation curve, (b) optical microstructure (etchant: 2 pct Nital), and (c) XRD pattern along with the corresponding
fitted pattern using the Reitveld refinement method and the intensity difference between the two.

estimation of linear thermal expansion coefficients of


austenite (c) and bainitic ferrite (ab). The linear thermal
expansion coefficient of austenite was simply obtained
by iteratively fitting the experimental dilatation data in
the linear region above Bs (Figure 1(a)) to Eq. [1] and
taking fab ¼ 0. The objective of the iteration was to
obtain the best-fit value of the linear thermal expansion
coefficient of austenite that gives the best match between
the experimental and calculated dilatation curves, as
reflected by a high correlation coefficient (r2) value close
to 1 in the temperature range above the Bs temperature.
However, the thermal expansion coefficient value of
bainitic ferrite cannot be obtained in the same way since
fab 6¼ 1 at any temperature in the thermal cycle. There-
fore, to obtain this value and the relative amount of
austenite and bainitic ferrite and its carbon concentra-
tion, the dilatation curve starting from the Bs temper-
ature up to the Ms temperature was fitted using Eqs. [1]
and [2] together with the mass balance equation
(Eq. [3]). The appropriate lattice parameter values of
austenite and bainitic ferrite, as discussed previously,
were used together with the linear thermal expansion
coefficient of austenite, as determined earlier. Equa-
tions [1] through [3] were then solved simultaneously
using an iterative procedure to obtain the best possible
match between the experimental and the calculated
dilatation curves, as given by a very high value of the
Fig. 2—Flow chart showing the steps of calculation to extract the
correlation coefficient (r2  1). The carbon concentra- phase evolution information (amount and composition) along with
tion in bainitic ferrite was taken to be constant, while thermal expansion coefficients of the phases from the experimental
austenite was allowed to be enriched with carbon as the dilatation curve.
transformation progressed and the lattice parameters of
both the phases were updated accordingly. It should be of unknown variables in the temperature range below Bs
noted that the entire dilatation curve above the Ms is three, i.e., Cc, fab , and bab , and they can be obtained
temperature was fitted simultaneously with a single set easily from the three equations following the approach
of parameters. A flow chart summarizing the procedure discussed in the previous paragraphs. For cases 2 and 3,
is shown in Figure 2. however, no prior assumption was made with respect to
For case 1, the carbon concentration in bainitic ferrite the carbon concentration of bainitic ferrite. This
was assumed to be negligible. Therefore, Eq. [3] can be increases the number of unknowns to four (i.e., Cab in
simplified to Cc fc  C0 , fab þ fc ¼ 1 so that the number addition to Cc, fab , and bab ) in these two cases, and it is

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 3—Experimental and calculated dilatation curves for (a) case 1, (b) case 2, and (c) case 3, and (d), (e), and (f) corresponding extracted phase
evolution data, i.e., volume percentage of bainitic ferrite and austenite and carbon concentration (at. pct) in austenite, as a function of tempera-
ture.

METALLURGICAL AND MATERIALS TRANSACTIONS A


Table I. Data Obtained Iteratively from the Experimental Dilatation Curve

Carbon Concentration Linear Thermal


Amount At Pct Expansion Coefficient
(Pct) [Wt Pct] (9 105 K)

Type ab c ab c ab c
Case 1 98 2 negligible 45.445 1.631 2.338
(Figures 3(a) and (d)) [9.110]
Case 2 97 3 0.811 4.070 1.512 2.369
(Figures 3(b) and (e)) [0.179] [0.890]
Case 3 97 3 0.811 4.070 1.507 2.423
(Figures 3(c) and (f)) [0.179] [0.890]

not possible to get a unique set of solutions through the carbon concentration in the untransformed austenite
approach discussed previously. Therefore, in cases 2 and was taken as 4.070 at. pct (0.890 wt pct) for the iteration,
3, the experimentally measured MS temperature of the as stated earlier. The corresponding carbon concentra-
austenite left untransformed after the bainite transfor- tion in bainitic ferrite in cases 2 and 3 obtained from
mation was used as additional data during the iteration. iteration was 0.811 at. pct (0.179 wt pct), which is close
The measured MS temperature of 385 K (112 °C) to the carbon concentration of 0.909 at. pct (0.2 wt pct)
(Figure 1(a)) corresponds to 4.070 at pct (0.890 wt pct) of the steel or the parent austenite (c), which transforms
carbon in austenite, according to the equation proposed to bainite during cooling. The results clearly indicate
by Andrews.[27] that the carbon concentration of bainitic ferrite is higher
The results of the analysis are summarized in Figure 3 than the solubility of carbon in a-ferrite that is in
and Table I. The experimental and calculated dilatation paraequilibrium with c-austenite. To confirm this, the
curves for the three cases are shown in Figures 3(a) bainitic ferrite lattice parameter was estimated using the
through (c). The corresponding extracted phase evolu- Rietveld method from the XRD pattern using X’Pert
tion data, i.e., volume percentages of austenite and High Score Plus (Figure 1(c)), and its corresponding
bainitic ferrite and carbon concentration (at. pct) in carbon concentration was obtained using the equation
austenite, are presented in Figures 3(d) through (f). In proposed by Bhadeshia et al.[24] The difference between
addition, the critical transformation temperatures are the calculated and experimental intensity of the XRD
highlighted in Figure 3. pattern shown in Figure 1(c) suggests a good match is
Table I indicates that the linear thermal expansion obtained between the two. A lattice parameter value of
coefficient values for the three cases are nearly the same 2.8733 Å was estimated for the bainitic ferrite. This
for a given phase. Moreover, in general, a good match is value corresponds to a carbon concentration of 0.898 at.
obtained between the calculated best-fit curve obtained pct (0.198 wt pct) and agrees well with the carbon
through iteration and the experimental dilatation curve concentration value of 0.811 at. pct (0.179 wt pct) in the
in cases 2 and 3 (Figures 3(b) and (c)), with case 3 being bainitic ferrite obtained from the dilatation data. The
the best; the fit is relatively poor in case 1 (Figure 3(a)). results, thus, indicate that the austenite to bainitic ferrite
Moreover, the highlighted critical temperatures in case 3 transformation proceeds through a displacive mecha-
(Figure 3(c)) are close to the corresponding values nism. Since the best fit to the experimental dilatation
obtained by the simple tangent method (Figure 1(a)). curve was obtained in case 3, the values of the critical
The calculated amount of the austenite remaining transformation temperatures (Bs and Bf), the thermal
untransformed up to Ms was around 2 pct in case 1 expansion coefficients, and the amount and composition
and around 3 pct in cases 2 and 3 (Figures 3(d) through of the phases corresponding to this case represent the
(f) and Table I). More significantly, the results in actual material and transformation characteristics.
Figure 3(d) and Table I reveal that the estimated carbon
concentration of the untransformed austenite is 45.445
at. pct (9.11 wt pct) in case 1, which is unrealistically II. SUMMARY AND CONCLUSIONS
high (the maximum solubility being 2.1 wt pct[28]).
Moreover, the calculated best-fit dilatation curve begins A procedure involving iteration has been presented to
to deviate from the experimental one well above the Ms extract the phase evolution information, i.e., amount
temperature (Figure 3(a)). It was impossible to fit the and composition of the phases (bainitic ferrite and
entire dilatation curve with this assumption. These austenite), from the experimental dilatation curve for
inconsistencies lead to the conclusion that the underly- the transformation of austenite to bainitic ferrite during
ing assumption of very low carbon bainitic ferrite for continuous cooling. The carbon concentration of
case 1 is not correct. Cases 2 and 3 give a better bainitic ferrite estimated by this method agreed well
description of the experimental results. The small with the corresponding value estimated from the XRD
deviation between the calculated and the experimental analysis, and it was found to be higher than the
curves (Figures 3(b) and (c)) below Ms is simply because solubility of carbon in a-ferrite that is in paraequilib-
the data below Ms were not fitted. For cases 2 and 3, the rium with c-austenite. Bainitic ferrite with bct crystal

METALLURGICAL AND MATERIALS TRANSACTIONS A


structure was found to give slightly better fit of the Kramer, S. Mahajan, and P. Veyssière, eds., Elsevier, Oxford,
calculated dilatation curve to the experimental dilata- 2002, pp. 1–7.
9. H.K.D.H. Bhadeshia: Material Science Forum, Trans Tech
tion curve than with bcc structure. The results suggest Publications, Aedermannsdorf, 2005, pp. 63–74.
that austenite to bainitic ferrite transformation takes 10. F.G. Caballero and H.K.D.H. Bhadeshia: Curr. Opin. Solid State
places by a displacive mechanism. Mater. Sci., 2004, vol. 8, pp. 251–57.
11. F.G. Caballero, M.K. Miller, C. Garcia-Mateo, and J. Cornide: J.
Alloys Compd., 2013, vol. 577 (Suppl. 1), pp. S626–S30.
12. F.G. Caballero, M.K. Miller, C. Garcia-Mateo, J. Cornide, and
M.J. Santofimia: Scripta Mater., 2012, vol. 67, pp. 846–49.
13. F.G. Caballero, M.K. Miller, S.S. Babu, and C. Garcia-Mateo:
ACKNOWLEDGMENTS Acta Mater., 2007, vol. 55, pp. 381–90.
14. C. Garcia-Mateo, M. Peet, F.G. Caballero, and H.K.D.H.
The authors gratefully acknowledge the Head of the Bhadeshia: Mater. Sci. Technol., 2004, vol. 20, pp. 814–18.
Department of Metallurgical and Materials Engineer- 15. M. Peet, S.S. Babu, M.K. Miller, and H.K.D.H. Bhadeshia:
ing, Indian Institute of Technology (Kharagpur, In- Scripta Mater., 2004, vol. 50, pp. 1277–81.
dia), for providing the laboratory facility. The authors 16. J.H. Jang, H.K.D.H. Bhadeshia, and D.-W. Suh: Scripta Mater.,
also thank the Ministry of Steel and Department of 2013, vol. 68, pp. 195–98.
17. C.N. Hulme-Smith, I. Lonardelli, A.C. Dippel, and H.K.D.H.
Science and Technology, Government of India, for the Bhadeshia: Scripta Mater., 2013, vol. 69, pp. 409–12.
partial financial support. 18. C. Garcia-Mateo, J.A. Jimenez, H.W. Yen, M.K. Miller, L.
Morales-Rivas, M. Kuntz, S.P. Ringer, J.R. Yang, and F.G.
Caballero: Acta Mater., 2015, vol. 91, pp. 162–73.
19. C.N. Hulme-Smith, M.J. Peet, I. Lonardelli, A.C. Dippel, and
REFERENCES H.K.D.H. Bhadeshia: Mater. Sci. Technol., 2015, vol. 31,
1. L.C.D. Fielding: Mater. Sci. Technol., 2013, vol. 29, pp. 383–99. pp. 254–56.
2. S.B. Singh: in Phase Transformations in Steels: Fundamentals and 20. H.K.D.H. Bhadeshia: Bainite in Steels: Transformations,
Diffusion-Controlled Transformations, E. Pereloma and D.V. Microstructure and Properties, IOM Communications, London,
Edmonds, eds., Woodhead Publishing Limited, Cambridge, 2012. 2001.
3. H.K.D.H. Bhadeshia: Mater. Sci. Eng. A, 1999, vol. 273, 21. R. Ranjan, H. Beladi, S.B. Singh, and D.P. Hodgson: Metall.
pp. 58–66. Mater. Trans. A, 2015, vol. 46A, pp. 3232–47.
4. H.K.D.H. Bhadeshia and R.W.K. Honeycombe: Steels: 22. D.J. Dyson and B. Holmes: J. Iron Steel Inst., 1970, vol. 208,
Microstructure and Properties, Butterworth-Heinemann, Elsevier, pp. 469–74.
Oxford, 2006. 23. W.C. Leslie: Metall. Trans., 1972, vol. 3, pp. 5–26.
5. H.K.D.H. Bhadeshia and D.V. Edmonds: Acta Metall., 1980, 24. H.K.D.H. Bhadeshia, S.A. David, J.M. Vitek, and R.W. Reed:
vol. 28, pp. 1265–73. Mater. Sci. Technol., 1991, vol. 7, pp. 686–98.
6. H.K.D.H. Bhadeshia: Proc. Royal Soc. Lond. A, 2010, https:// 25. L. Cheng, A. Böttger, T.H. de Keijser, and E.J. Mittemeijer:
doi.org/10.1098/rspa.2009.0407. Scripta Metall. Mater., 1990, vol. 24, pp. 509–14.
7. F.G. Caballero, H.K.D.H. Bhadeshia, K.J.A. Mawella, D.G. 26. R. Ranjan, and S.B. Singh: Department of Metallurgical and
Jones, and P. Brown: Mater. Sci. Technol., 2002, vol. 18, Materials Engineering, Indian Institute of Technology, Kharag-
pp. 279–84. pur, India, unpublished research, 2016.
8. H.K.D.H. Bhadeshia: in Encyclopedia of Materials: Science and 27. K.W. Andrews: J. Iron Steel Inst., 1965, vol. 203, pp. 721–27.
Technology, 2nd ed., R.W. Cahn, M.C. Flemings, B. Ilschner, E.J. 28. J. Chipman: Metall. Trans., 1972, vol. 3, pp. 55–64.

METALLURGICAL AND MATERIALS TRANSACTIONS A

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