J. Mater. Sci. Technol., 2010, 26(2), 181-186.

Grain Size Eect on the Martensite Formation in a High-Manganese TWIP Steel by the Rietveld Method
G. Dini1) , A. Najazadeh1) , S.M. Monir-Vaghe1) and R. Ueji2)
1) Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran 2) Department of Advanced Materials Science, Faculty of Engineering, Kagawa University, 2217-20, Hayashi-cho, Takamatsu, Kagawa, 761-0396, Japan
[Manuscript received January 5, 2009, in revised form July 6, 2009]

The aim of the present work was to study the eect of austenite grain size (AGS) on the martensite formation in a high-manganese twinning-induced plasticity (TWIP) steel. The results of a quantitative microstructural characterization of the steel by the whole X-ray pattern tting Rietveld software, materials analysis using diraction (MAUD), indicated that the volume fraction of bcc -martensite increases with increasing AGS. However, the value of the stacking fault probability (Psf ) does not show a large variation for samples with dierent values of AGS under water-quenching conditions. KEY WORDS: Austenite grain size; Martensite formation; TWIP steel; Stacking fault probability

1. Introduction Recently, Fe-Mn-C-Al-Si alloys have attracted immense interest from metallurgists and materials scientists on account of their industrial importance, where superior mechanical properties, such as high work-hardening rate, high ductility and strength, are required[1,2] . High manganese steels containing 1530 wt pct Mn along with Si, Al and C exhibit high strength and exceptional plasticity due to the formation of extensive twins under mechanical load (twinning-induced plasticity, TWIP eect) or multiple martensitic transformations, such as fcc (austenite)hcp (hcpmartensite)bcc (bcc-martensite) (transformationinduced plasticity, TRIP eect)[35] . For twinning to occur, it is generally accepted that the stacking fault energy (SFE) of the steel must be in the range 18 mJ/m2 <SFE<35 mJ/m2 . If the SFE is lower, twinning is replaced by martensitic transformations. If the SFE is higher, dislocation glide is the only mech Corresponding author. Ph.D.; Tel.: +98 311 3915741; Fax: +98 311 3912751; Email address: gh dini@ma.iut.ac.ir (G. Dini).

anism contributing to deformation[6] . The stability of austenite in these steels is a phenomenon of the utmost importance in alloy design. Sato et al.[7] reported two dierent paths, fcc bcc and fcc hcp bcc , of martensitic transformation that depend on the chemical composition, the test temperature, and the amount of strain imparted to the material. The formation of martensite can be either thermally induced or stress induced. During cooling, binary austenitic Fe-Mn steels transform partially to hcp - and bcc -martensite within a restricted composition range[3] . It is believed that planar faults (stacking and twin faults) play an important role in the formation of martensite in Fe-Mn-Si-Al TWIP steels. It is well known that the fcc hcp phase transformation takes place through the introduction of stacking faults on every alternate layer of the {111} planes of austenite (fcc)[8] . bcc -martensite forms at the intersection of dierent hcp variants or directly from the austenite phase. It has been reported that the deformation twins and stacking faults act as nucleation sites for bcc -martensite formation[9,10] . In addition to the cooling rate and the crystallo-

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graphic defects, the austenite grain size (AGS) is also one of the parameters that controls the stability of austenite, as the martensite formation can be prohibited by a high number of barriers in the structure, such as grain boundaries. In this work, the eect of AGS on the formation of martensite in a TWIP steel and its correlation with the stacking fault within the microstructure were studied. The microstructure of the dierent phases has been characterized by analyzing the whole X-ray diraction (XRD) patterns via the Rietveld software, materials analysis using diraction (MAUD)[11] , which has its origin in the pioneering work by Rietveld[12] . In some recent studies, MAUD has been applied to characterize the microstructure of dierent phases[1315] . 2. Experimental The alloy we used was melted in an induction furnace protected by argon gas and cast into a rectangular ingot, which was 250 mm120 mm60 mm in size. The chemical composition of the alloy is given in Table 1. A 14 mm thick plate was cut from the ingot,
Table 1 Chemical composition of the prepared steel (wt pct) C 0.32 Mn 36.06 Al 2.62 Si 3.21 S 0.005 Fe Bal.

homogenized in an air furnace at 1200 C for 2 h and then air-cooled. The plate was rolled through a cold rolling mill, which turned it into a sheet with a thickness of 0.5 mm. From this sheet, the specimens used for XRD tests and microstructural observations were prepared. The specimens were annealed at 850 C for 5, 15, 30 and 60 min and then water quenched. In the rest of this paper, the specimens will be referred to as 5MW, 15MW, 30MW and 60MW, respectively. The microstructure was characterized by optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy(TEM). XRD data were collected between 30 and 100 (2) at room temperature using a diractometer with a Cu target and monochromator, a step size of 0.05 , and a counting time of 1 s. 3. Methods of Analysis The Rietveld method mostly consists of modeling a large portion of the experimental XRD pattern with an analytical function to explain the proles, whose intensities are directly related to the structure of each investigated phase[12] . In the present work, we chose Rietveld s software MAUD to t exactly the entire XRD patterns for microstructural characterization of the constituent phases (austenite and martensite), including the calculation of crystallographic defects during the

austenite-to-martensite transformation. A diraction pattern was simulated from a series of structural parameters, microstructural parameters, peak shape and width and background parameters. All the variable parameters were rened by choosing an iterative least square procedure through a minimization of the residual parameter. Parameters, such as the 2 correction, peakasymmetry, and peak-broadening parameters (U , V , W ), that are instrumental to the Si standard sample and also assumed to have no size and strain broadening, were used as the tting parameters in the software according to the method described by Lutterotti et al.[16] . The correction of the preferred orientation has been carried out using the arbitrary texture correction method. This kind of texture correction is not a model and, as such, cannot be interpreted in terms of physically understandable parameters of texture. The correction simply consists of assigning arbitrary intensity values to the peaks so that they are in agreement with our observations[17] . The volume fraction of each phase was calculated by determining the weight fraction and the density of each phase. The stacking fault probability (Psf ), which indirectly represents the number of Shockley partial dislocations within the austenite microstructure, was derived using the X-ray Rietveld renement according to the Warren s theory for fault analysis[18] . This was performed in the MAUD software according to the method described by Lutterotti et al.[16] . According to the Warren s formulae, three dierent types of planer defect can be found in an fcc structure as follows: two deformation (stacking) faults, the intrinsic ( ) and the extrinsic ( ) probabilities, and twin fault probability (). And therefore the stacking fault probability (Psf ==( ) and the twining probability (Ptw =) in austenite phase can be calculated. The results of all these analyses, with regard to the microstructural information, are shown in Table 2. However, throughout the entire analyses, the values of Ptw in the austenite phase of all samples were negligible, and hence, these values are not presented in this table. The accuracy of t and reliability of the structural as well as microstructural parameters were calculated by the numerical criteria of t parameter known as goodness of t (GoF). The values obtained from the analysis are also shown in Table 2. 4. Results and Discussion 4.1 Eect of cold-rolling strain on austenite stability The microstructure of the as-homogenized sample shows more or less equiaxial grains that contain some annealing twins (Fig. 1) with an average grain size of about 1130 m (as measured by the linear-intercept method). XRD pattern indicated that the prepared steel contained only a single austenite phase (Fig. 2)

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Table 2 Sample microstructure results in the as-water quenched condition Sample No. GoF 5MW 15MW 30MW 60MW 1.14 1.18 1.20 1.18 Austenite Volume fraction Lattice parameter/nm 103 Psf of martensite/% 0.36384 10.11 0 0.36346 12.33 6 0.36364 11.21 9 0.36380 11.60 15

Fig. 1 Optical micrograph of the as-homogenized prepared steel

Fig. 3 XRD pattern of the as-cold-rolled steel (reduction in thickness of 97%)

Fig. 2 XRD pattern of the as-homogenized steel

in the as-homogenized steel. Figure 3 shows the XRD pattern for the as-coldrolled sample. After severe deformation (reduction in thickness of 97%), there exists only fcc in the sample, and thus, no phase transformation occurs. In contrast, as can be seen in Fig. 4, the evolution of twin volume fraction with the strain increases obviously. The occurrence of deformation twins were conrmed by the TEM bright eld micrograph and selected area diraction pattern (Fig. 5(c) and (d), respectively). At a cold rolling strain of =0.10, the twin volume fraction is more than 60% (Fig. 4(a)). Generally, only one twinning system is active at low to moderate strains in each crystal. The generated twins develop throughout the whole grain and are blocked by the grain boundaries. Starting from a given strain (for example =1.05), a second system is operated in some areas, which leads to a grid pattern, as shown in

Fig. 4(b) and (c) and in Fig. 5 in detail. At large strains, it is dicult to observe the deformation twins in the grains because of the formation of shear bands (Fig. 4(d)). As mentioned in section 1, the governing microstructural parameter that determines the phase stability of the austenite is the SFE. Based on the chemical composition (Table 1) of the steel, we estimated the SFE by thermodynamic calculations. According to thermodynamic models developed by Grssel et al.[19] (for the Fe-Mn-C-Si-Al system) and a Allain et al.[6] (for the Fe-Mn-C system), the SFE of prepared steel is about 67.5 and 32 mJ/m2 , respectively. Obviously, the value of 67.5 mJ/m2 cannot explain the behavior of steel during cold deformation and the formation of a high volume of twins (see Fig. 4). Note that Grssel et al. developed a model a for manganese steels containing a Mn of 15% to 30% (in mass fraction). Therefore, the error in the SFE estimation may be related to this limitation. Also, the SFE calculation of Allain et al. was developed for the Fe-Mn-C system, and the eects of Si and Al additions on the SFE were not considered. However, the estimated value of the SFE by this model is in good agreement with the behavior of steel during the cold rolling. In summary, the results of the microstructure observations and XRD investigations prove that the cold-rolled samples (with a chemical composition given in Table 1) can be classied as part of the TWIP steel category. 4.2 Eect of grain size on austenite stability Figure 6 shows the change in the AGS of the prepared steel with the annealing time. It is observed

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Fig. 4 Optical micrograph of the prepared steel at dierent true strain levels: (a) 0.10, (b) 0.39, (c) 1.05, (d) 1.22

Fig. 5 Deformation twins in the prepared TWIP steel at true strain of 1.05, (a) and (b) the low and high magnication SEM micrographs, respectively, (c) TEM bright eld micrograph and (d) selected area diraction pattern of twinned area

that the AGS of the TWIP steel varied in a range of 4.423.7 m by changing the annealing time from 5 to 60 min.

The XRD patterns of the samples under the water quenching conditions with dierent grain sizes (Fig. 7) were subjected to a Rietveld analysis, using the

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Fig. 6 Variation of austenite grain size with annealing time in prepared steel

Fig. 8 Variation of the volume fraction of martensite with the austenite grain size

bcc -

Fig. 7 XRD patterns of water quenched samples: (a) 5MW, (b) 15MW, (c) 30MW, (d) 60MW

Fig. 9 Variation of the stacking fault probability with the austenite grain size

MAUD as described in section 3, to characterize the microstructure and to study the eect of the AGS on the evolution of the microstructure after annealing and subsequent water quenching. The coexistence of austenite and bcc -martensite in the samples can be conrmed from their XRD patterns. The respective results are shown in Table 2. The accuracy of the result is indicated by the value of the quality factor of the tting. The GoF values are close to 1 (Table 2), signifying the accuracy of the tting. The volume fractions of bcc -martensite as a function of the AGS are plotted in Fig. 8. It is easily noticeable that the volume fraction of bcc -martensite increases gradually with increasing AGS. However, in the 5MW sample, the results indicated that, after water quenching, only the austenite phase exists in the structure. The eect of the parent phase grain size on the martensitic transformation start temperature (Ms ) has been studied by many researchers[2022] . It is believed that a grain boundary may be considered to be a preferential site for martensitic transformation

because it is an extensive defect. However, in most cases, grain boundaries stabilize and strengthen the parent phase, and, consequently, Ms decreases with decreasing grain size[22] . Therefore, the increase in the volume fraction of bcc -martensite with increasing annealing time may be ascribed to the increase in grain size, which decreases the additional energy barrier that originates from the grain boundary. Additionally, some reasearchers have investigated the eect of the AGS on the SFE. For example, Lee and Choi[23] suggested that, with decreasing austenite grain size (especially below 30 m), the SFE in high Mn steels increases and helps to suppress the martensite transformation. It is worth noting that the SFE (including the AGS eect) was called the apparent SFE by these reasearchers. In this study, however, the grain sizes of all the samples are smaller in comparison to the critical value suggested by Lee and Choi[23] , but the martensite transformation occurred in these samples after water quenching. In contrast, according to Jiang et al.[24] , the SFE is

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dependent on the alloy content and other factors such as temperature, but it is independent on the grain size in Fe-Mn-Si alloys. Also, Olson and Cohen[8] found that, in the Fe-based alloys with a low SFE, a perfect dislocation in the fcc matrix can be easily dissociated into two Shockley partial dislocations, forming a stacking fault. The four or ve layers of stacking faults within the austenite act as favorable nucleation sites for the martensite formation. Therefore, the phase transformations consume the stacking faults, which results in low values of Psf in the austenite. Also, the larger the austenite grain, the higher the probability of nding a nucleation site of martensite formed by the overlapping of stacking faults, resulting in the increase in Ms temperature. On the other hand, the AGS may be a geometric barrier to the dissociation of dislocations in Fe-high Mn alloys with low SFE (and stacking faults with large width) when the AGS is smaller than the equilibrium width of the stacking faults. As mentioned previously, as a result of the austenite to bcc -martensite transformation, a large number of stacking faults may be consumed, which leads to a decrease in the stacking fault probability of TWIP steel with low SFE. Therefore, by increasing the volume fraction of martensite, stacking fault consumption increases. Furthermore, the grain size could represent a geometric barrier against the dissociation of perfect dislocations if the grain size is smaller than the equilibrium width of the stacking faults. Thus, by increasing the ASG, for example with annealing time, the stacking faults and, hence, Psf increase just before water quenching. Therefore, it is expected that the values of Psf in the samples after water quenching are almost the same. The variations of the Psf parameter in the austenite microstructure are shown in Fig. 9. The results conrm this assumption because the value of Psf does not show a large variation for the samples with dierent grain sizes. In contrast, the volume fraction of martensite increases with increasing AGS (Fig. 8). 5. Conclusions (1) The prepared steel (with chemical composition of Fe-36.06Mn-0.32C-3.21Si-2.62Al) can be classied in the TWIP steel category. (2) The AGS of the samples increases from 4.4 to 23.7 m with increasing annealing time from 5 to 60 min at 850 C. (3) The whole X-ray pattern tting Rietveld software (MAUD) adequately ts the X-ray patterns for

both of the phases (austenite and martensite) of the samples in the water quenching condition. (4) The volume fraction of bcc -martensite increases gradually with increasing AGS. However, the value of stacking fault probability (Psf ) does not show a large variation for samples with dierent AGSs.
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