Various stages in stressstrain curve of TiAlNb alloys undergoing SIMT

Archana G. Paradkar a, , S.V. Kamat a , A.K. Gogia b , B.P. Kashyap c

Defence Metallurgical Research Laboratory, Hyderabad 500058, AP, India Project Ofce (Materials), Kaveri Engine Programme, Hyderabad 500058, AP, India c Indian Institute of Technology, Department of Metallurgical Engineering and Material Science, Mumbai 400076, Maharashtra State, India
b a

Abstract TiAlNb alloys in the present range of composition were found to exhibit a typical four-stage behaviour observed in alloys undergoing stressinduced martensitic transformation (SIMT) in as well as 2 heat-treated condition. Intermittent unloadingreloading during tensile test was used to measure the apparent modulus at regular strain intervals. This coupled with the observation of microstructure of the samples from tensile tests interrupted at each of the four stages was used to identify the operative mechanism of each stage.
Keywords: TiAlNb alloys; Apparent modulus; Stress-induced martensitic transformation (SIMT)

1. Introduction Stress-induced martensitic (SIM) transformations in steels and shape memory alloys are studied extensively [14]. Alloy undergoing SIM transformation exhibits a typical stress-plateau in the tensile stressstrain curve (Fig. 1). The curve delineates four distinct stages and the numbers in Fig. 1 denote these stages during deformation. Several investigations [1,514] have been carried out to clarify the nature of each stage in NiTi and the results of these studies are summarized in the following. Stage 1 is the initial linear elastic region. In this stage, the parent phase undergoes an elastic deformation [5,6]. Stage 2 or stress plateau region corresponds to stress-induced transformation of metastable parent phase to martensite or reorientation of martensite present in initial microstructure [1,5,7]. In case the reorientation of martensite is responsible for deformation strain, the stress plateau is at, but, when stress-induced martensite contributes to deformation strain, this stage is reported to exhibit gradual increase in stress with increase in strain [8] resulting in a rising stress plateau. The mechanism of the deformation in stage 3 is not well established. Some authors [1,9] have suggested that the defor-

mation in stage 3 is an elastic deformation of the martensite phase formed in stage 2. Similar observations are also reported by Vaidyanathan et al. [6]. However, transmission electron microscopy observations by Melton and Mercier [10] revealed an intersecting array of martensite laths in some part and dislocations in another part in a specimen deformed into stage 3. However, their observation is limited to a small region of stage 3. Miyazaki et al. [11], on the other hand, reported that in NiTi alloy, this stage corresponds to the mixed processes of elastic deformation of stress-induced martensite formed in stage 2 and reorientation of martensite in combination with the further stress-induced transformation of the parent phase. Mohamed and Washburn [1] made an electron microscopy observation of specimens elongated by 8% and found heavy irregularity of martensite boundaries. Thus, they suggested that slip occurred at the stage 4 in NiTi alloy. Michel [12] and Tadaki and Wayman [13] also made the electron microscopy observation of heavily cold-rolled (30%) specimens, which roughly corresponded to stage 4 in tensile tests. They both found high density of dislocations and the segmentation of martensites. These results are clear evidence to show that slip occurs in stage 4. Stage 4 denes the plastic deformation of oriented martensite or martensite and retained parent phase, if any, depending upon the initial microstructure. Similar four-stage stressstrain curves are also reported in CuAINi single crystals in specic orientations [14]. While the rst two stages are similar to those seen

293 Table 2 Solutionising temperatures for various alloys S/N % 2 Solution treatment temperature ( C) Ti15Al12Nb 1 2 3 4 0 10 20 40 970 920 880 840 Ti15Al8Nb 1010 965 926 886 Ti18Al8Nb 1080 1026 985 941

Fig. 1. Typical stressstrain curve for an alloy undergoing SIM (numbers denote various stages during tensile testing).

in NiTi alloy, the deformation modes in stages 3 and 4, in this case, are proved unambiguously to be due to the elastic deformation of a martensite and martensite-to-martensite transformation, i.e. successive stress-induced transformation, respectively [14]. Thus, it is seen that the operative mechanisms during the various stages of stressstrain curve are dependent on the alloy system. SIM in Ti alloys is well reported in literature [1524]. TiAlNb alloys containing 1518 at.% Al and 812 at.% Nb are also reported to undergo SIM in WQ condition [25]. The present investigation is aimed at studying the operative mechanisms during the tensile deformation of TiAlNb alloys undergoing stress-induced transformation for various heat treatments resulting in either fully single-phase microstructure or ( + 2 ) microstructure with different volume fraction of 2 . Three alloys, viz. Ti15Al8Nb, Ti15Al12Nb and Ti18Al8Nb were selected for this purpose. 2. Experimental work Ingots of Ti15Al8Nb, Ti15Al12Nb and Ti18Al8Nb alloys were melted by consumable vacuum arc melting process. The nominal composition of the alloys is listed in Table 1. The transus temperatures of the alloys were found to be 1000, 950 and 1060 C for Ti15Al8Nb, Ti15Al12Nb and Ti18Al8Nb, respectively. The ingots were rst forged in single-phase region and hot rolled at a temperature 100 C below the transus to 14 mm thick plates in several passes. Few samples were solution treated and water-quenched to get single-phase structure. The volume fraction of 2 is varied
Table 1 Nominal composition of the alloys Alloy Ti15Al8Nb Ti15Al12Nb Ti18Al8Nb Al, wt.% (at.%) 8 (14.4) 7.8 (14.5) 10.10 (17.9) Nb, wt.% (at.%) 15.75 (8.23) 21.90 (11.82) 15.9 (8.18)

by heat-treating in 2 region at different temperatures so as to obtain different volume fractions of 2 , viz. 10, 20 and 40% (Table 2) and then water quenched. The tensile samples of 4 mm diameter and 10 mm gage length (parallel to the rolling direction) were machined and stress relieved after machining and pickled so as to avoid masking of the true ow behaviour of the alloy [25]. The tensile tests were carried out using strain gauges on a servo-hydraulic Instron Universal Testing Machine at a crosshead speed of 1 mm/min. A set of specimens in 2 and water-quenched condition for all the three alloys were loaded, unloaded and reloaded several times at regular strain intervals during the tensile deformation with holding time of 2 min after each loading and unloading. The apparent modulus was measured by taking the average of the unloading and reloading stage. Few samples of Ti15Al8Nb alloy, as a representative case, were electropolished and the tensile test was interrupted at each stage for SEM observations. 3. Results and discussions Microstructures of all the alloys in 2 and waterquenched condition are similar and representative micrographs for Ti15Al8Nb in and 2 heat-treated conditions are shown in Figs. 2 and 3, respectively. The microstructure shows single-phase structure (Fig. 2), in water-quenched condition and a two-phase structure in 2 (Fig. 3ac) water-quenched condition, which is conrmed by XRD (Figs. 2b and 3d) to be and + 2 , respectively. TiAlNb alloys in the present range of composition, show typical four-stage behaviour in both and (2 ) water-quenched condition during the tensile test, similar to observations in NiTi alloy [5], and representative curves for Ti15Al8Nb are shown in Fig. 4. In the present case, however, the stress-plateau is slightly rising. This indicates that the transformation strain in the present case is due to the stress-induced transformation of to martensite [8]. In Ti alloys, the elastic modulus of orthorhombic martensite ( ) is signicantly different than that of phase. The phase

O (wt.%) 0.0450 0.0415 0.0450

N (wt.%) 0.0085 0.0100 0.009

Ti Balance Balance Balance

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Fig. 2. (a) Optical micrograph and (b) XRD of the Ti15Al8Nb alloy in water-quenched condition showing phase.

change from bcc to orthorhombic martensite during the deformation would then be reected by a change in the elastic modulus. Thus, the measurement of the apparent modulus can be used as a tool for tracking the SIM transformation in these alloys and hence identifying the various stages in the tensile stressstrain curve. The term apparent modulus is used here as the modulus obtained on unloading and reloading is not the true modulus of mixture since secondary deformation mechanisms such as stress-induced transformation and martensite reorientation are also operative [5]. Representative stressstrain curves for Ti15Al8Nb alloy, tested with intermittent unloadingreloading condition, in and 2 (10% 2 ) heat-treated conditions are shown in Fig. 5. Similar curves are obtained for other alloys in various microstructural conditions. Hysteresis is absent in stage 1. However, beyond this stage, hysteresis is seen and it decreases with increase in strain. The hysteresis seen during unloading and reloading (Fig. 5)

can be attributed to mechanical reversibility of stress-induced martensite or partial reversibility of martensite reorientation [26]. Figs. 68 depict the measured values of the apparent elastic modulus plotted as a function of strain during different stages of tensile deformation for the three alloys. It is seen from these gures that the apparent modulus is high initially (see Table 3) and does not change in stage 1. The modulus starts to decrease as stage 2 commences and attains a stable value (Figs. 68) at the end of stage 2, which is signicantly lower than the corresponding initial modulus values (Table 3). The value does not change subsequently in stages 3 and 4. The microstructures of the specimens during each of the four stages are also examined. Microstructure of the tensile specimen of Ti15Al8Nb alloy interrupted at stage 1 (Fig. 9a) shows that there is no change in the microstructure as a result of loading to stage 1. This coupled with the observation that the elastic modulus does not change in stage 1 indicates that

Fig. 3. SEM micrographs of alloy Ti15Al8Nb in: (a) ( + 10% 2 ) WQ, (b) ( + 20% 2 ) WQ, (c) ( + 40% 2 ) WQ condition and (d) XRD pattern showing presence of 2 and .

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Fig. 4. Tensile stressstrain curves in and 2 water-quenched condition: (a) 1040 C/1 h/WQ, (b) 965 C/1 h/WQ, (c) 926 C/1 h/WQ and (d) 886 C/1 h/WQ for Ti15Al8Nb alloy. Table 3 Initial modulus of the alloys from curves Alloy Ti15Al12Nb Ti15Al8Nb Ti18Al8Nb 10% 2 74.68 78.89 90.68 20% 2 79.81 83.45 96.54 40% 2 89.04 92.96 104.06

Fig. 5. Intermittent loading unloading curves in: (a) WQ condition and (b) 2 heat-treated condition (10% 2 ) for Ti15Al8Nb alloy.

Fig. 6. Variation of apparent modulus of elasticity vs. engineering strain for Ti15Al12Nb alloy in various heat-treated conditions.

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Fig. 7. Variation of apparent modulus of elasticity with engineering strain for Ti15Al8Nb alloy in various heat-treated conditions.

this stage corresponds to elastic deformation of the starting microstructure. The stress-induced martensite in Ti alloys is known to have orthorhombic structure [27]. A representative micrograph (Fig. 9b) of the Ti15Al8Nb alloy in heat-treated condition, in the beginning of stage 2, shows a small volume fraction of

orthorhombic martensite ( ) needles along with retained . The microstructure at the end of stage 2 shows a considerably higher volume fraction of needles along with some retained . There is no signicant change in the microstructure in stage 3 (Fig. 9c). The point to note is that no slip lines are observed in the micrograph either in stage 2 or 3. However, the micrograph

Fig. 8. Variation of apparent modulus of elasticity with engineering strain for Ti18Al8Nb alloy in various heat-treated conditions.

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Fig. 9. SEM micrographs of electro-polished tensile sample interrupted at various stages: (a) elastic region in stage 1, (b) at the beginning of stage 2 showing SIMT of to , (c) in stage 3 showing absence of slip lines and (d) beginning of stage 4 showing slip lines for Ti15Al8Nb alloy in treated condition.

(Fig. 9d) in stage 4 clearly indicates the presence of slip lines. The observation of the apparent modulus variation with strain as well as the microstructure in the different stages conrmed that the behaviour is similar in 2 heat-treated specimens. The only difference is the presence of 2 in addition to . Stress-induced produced at the beginning of stage 2 in 2

Fig. 10. Similar stages are observed for alloy in 2 heat-treated condition. Microstructure shows the presence of an additional phase primary 2 . SEM micrographs of electro-polished tensile sample interrupted at the beginning of stage 2 showing SIMT of to are seen for (20% 2 + ).

Fig. 11. XRD of Ti15Al8Nb alloy after deformation in: (a) WQ and (b) 2 WQ condition.

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of the initial microstructural constituents. The stress-induced martensitic transformation commences in the beginning of stage 2 and whatever transformation has to occur is completed by the end of stage 2. Stage 3 corresponds to the elastic deformation of retained + structure prevailing at the end of stages 2 and 4 corresponds to plastic deformation of this mixture. Thus, the change in apparent modulus with strain can be used as an excellent tool to track the different stages of tensile deformation. The change in apparent modulus with strain can also be used to estimate the volume fraction of martensite ( ) if one knows the modulii of and 2 phases. This method could overcome the limitation of measurement of volume fraction of martensite by optical method which is not only time consuming and tedious but also may not be very accurate due to the uncertainties associated in resolving smaller martensitic laths. 4. Summary The tensile curves for all the three alloys in both, and 2 , solution-treated and water-quenched conditions depict four-stage behaviour. It is established that stage 1 represents the elastic deformation of the phases present in initial structure, stage 2 corresponds to stress-induced transformation of to martensite ( ), stage 3 represents the elastic deformation of all the constituent phases and stage 4 corresponds to the plastic deformation of the constituent phases. Acknowledgements The authors like to thank all the members of Titanium group for melting, members of rolling and forging group for processing and members of SFSG group for characterization of the alloys. Authors thank Dr. Vikas Kumar for his help during the experimentation and for helpful discussions. The authors would like to thank DRDO, India, for providing funding and facilities for carrying out this work. The authors would also like to thank Director DMRL, Hyderabad, for permission to publish this work. References
[1] A. Mohamed, J. Washburn, J. Mater. Sci. 12 (1977) 469. [2] W.C. Leslie, Physical Metallurgy of Steels, Hemisphere Press, McGrawHill, New York, 1981, p. 294. [3] R.C. Garvie, R.H. Hannink, R.T. Pascoe, Nature 258 (1975) 703. [4] M. Young, E. Levine, H. Margolin, Met. Trans. 5A (1974) 1891. [5] Y. Liu, H. Xiang, J. Alloys Compd. 270 (1998) 154. [6] R. Vaidyanathan, M.A.M. Bourke, D.C. Dunand, J. Appl. Phys. 86 (1999) 3020. [7] M. Young, E. Levine, H. Margolin, 5 (1974) 1819. [8] Y. Liu, P.G. McCormick, ISIJ Int. 29 (1989) 417. [9] J. Perkins, Scr. Met. 8 (1974) 1469. [10] K.N. Melton, O. Mercier, Metall. Trans. A 9A (1978) 1487. [11] S. Miyazaki, K. Otsuka, Y. Suzuki, Scr. Metall. 15 (1981) 287. [12] M. Michel, Ph.D. Thesis, Stanford University, 1979. [13] T. Tadaki, C.M. Wayman, Scr. Met. 14 (1980) 911. [14] K. Otsuka, H. Sakamoto, K. Shimizu, Acta Metall. 27 (1979) 585. [15] Y.T. Lee, L. Welsch, Mater. Sci. Eng. A 128A (1990) 77. [16] T.W. Duerig, G.T. Terelinde, J.C. Williams, Metall. Trans. 11A (1980) 1987.

Fig. 12. TEM micrographs of Ti15Al8Nb alloy after deformation in: (a) WQ (1040 C/1 h/WQ) and (b) 2 WQ (925 C/1 h/WQ) conditions, showing presence of .

heat-treated condition for Ti15Al8Nb alloy for ( + 20% 2 ) is shown in Fig. 10. The transformation of retained to orthorhombic martensite ( ) during the tensile deformation is also clearly evident from a representative XRD patterns of the Ti15Al8Nb alloy after deformation as depicted in Fig. 11. All the alloys exhibit presence of an additional phase, i.e. orthorhombic martensite ( ) after deformation. TEM micrographs of all the alloys after deformation, both in and 2 solution treatment and water-quenched conditions, also indicate the presence of an additional phase, orthorhombic martensite ( ) as shown in representative micrograph of the Ti15Al8Nb alloy after deformation (Fig. 12). This further corroborates the results of XRD studies (Fig. 11). The observation of the change in apparent modulus with the strain as well as microstructure at each stage clearly indicates that in the present alloys stage 1 represents elastic deformation

299 [17] T.W. Duerig, J. Albrecht, D. Richter, P. Fischer, Acta Metall. 30 (1982) 2161. [18] T. Grosdidier, C. Roubaud, M.J. Philippe, Y. Combres, Scr. Met. 36 (1997) 21. [19] T. Grosdidier, Y. Combres, E. Gautier, M.J. Philippe, Metall. Trans. A 31A (2000) 1095. [20] H. Sasano, T. Suzuki, Titanium: Sci. and Technology Proc. Fifth Int. Conf. on Titanium, Munich, Germany, 1984, p. 1667. [21] Y.T. Lee, M. Peters, G. Welsch, Metall. Trans. 22A (1991) 709. [22] C. Lei, M.H. Wu, L.Mc.D. Schetky, C. Burstone, in: Pelton, et al. (Eds.), SMST-97, Proc. Second Int. Conf. on Shape Memory and Super Elastic Technologies, Pacic Grove, CA, USA, 1997, p. 503. [23] M.H. Wu, P.A. Russo, J.G. Ferrero, Proc. Int. Conf. Shape Memory Super Elastic Technol., Pacic Grove, CA, 2003, p. 211. [24] R.W. Margevicius, J.D. Cotton, Metall. Trans. 29A (1998) 139. [25] A.G. Paradkar, Ph.D. Thesis, IIT Bombay, India, 2006. [26] T.W. Duerig, R. Zando, in: T.W. Duerig, K.N. Melton, D. Stockel, C. M (Eds.), Engineering Aspects of Shape Memory Alloys, Butterworth Heinemann, London, 1990, p. 369. [27] J.C. Williams, in: R.I. Jaffee, H.M. Burte (Eds.), Titanium: Sci. and Technology Proc. Second Int. Conf. on Titanium, vol. 3, Planum Press, Boston, 1972, p. 1433.