The Twin and Twin System in FCT L1 0 -MnNi Phase in an Equiatomic Mn-Ni Alloy
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1 Materials Transactions, Vol. 48, No. 10 (2007) pp to 2550 Special Issue on Advances in Electron Microscopy for Materials Characterization #2007 The Japan Institute of Metals The Twin and Twin System in FCT L1 0 MnNi Phase in an Equiatomic MnNi Alloy YoonUk Heo and HuChul Lee Department of Materials Science and Engineering, Seoul National University, Seoul , Korea This study examined the twinning mechanism and operating twin system of a face centered tetragonal (FCT) L1 0 MnNi phase in an equiatomic MnNi alloy using detailed TEM analysis (electron diffraction, high resolution imaging, and HAADF (Zcontrast) imaging techniques) of the structure of the twins formed during the (B2, bcc) to (L1 0, fct) phase transformation. In addition to the welldocumented f111g1=6h112š deformation twinning system in L1 0 crystals, f111g1=6h211š type pseudotwin systems were also observed. The Zcontrast image of the twins showed that no atomic shuffling occurred during twinning in the MnNi phase and atomic order was maintained in the f111g1=6h112š type truetwins. in hijkš, i and j are interchangeable in the tetragonal system but k is not. [doi: /matertrans.md200782] (Received May 9, 2007; Accepted June 25, 2007; Published September 12, 2007) Keywords: twin, L1 0 crystal, MnNi, transmission electron microscopy, atomic shuffle 1. Introduction The twinning systems of a L1 0 crystal are similar to that of a fcc crystal, which was reported to be f111g1=6h112i. 1) However, there is limited dislocation movement in a L1 0 ordered phase compared with that in fcc crystals due to the atomic ordering and poor symmetry of the tetragonal crystal structure. 2,3) Therefore, the twinning system of the L1 0 ordered phase is also limited compared with that of the fcc structure. Many studies have on the twin systems of L1 0 ordered phase been carried out. 4 13) These studies can be categorized in two groups. The first is the formation of twins during mechanical deformation. 4 10) The other is the twinning system during the phase transformation of a disordered phase to an ordered L1 0 crystal. 11,12) In both groups, it was reported that the possible twinning system of the L1 0 structure is a f111g1=6h112š type true twin. 4,7,9,10) The f111g1=6h211š type pseudotwin system can change the crystal structure of L1 0 to L1 1 if there is no atomic shuffling. 4,7,8) It was concluded that a pseudotwin system is difficult to occur in a L1 0 crystal because this would increase the total energy of the system. 4,7) Atomic shuffling is also an important factor in the twinning of the ordered phase. Many reports state that twinning along with atomic shuffling occurs in the ordered phase. 6,7) Therefore, the structure of the twins in the ordered phase was considered to be same as that of the matrix, even though twinning in the ordered crystal could alter the symmetry and structure of the crystal. 13) In this study, the twinning systems of the L1 0 MnNi phase were examined using TEM techniques, and atomic ordering in the twins was confirmed by HAADF imaging using Cscorrected STEM. 2. Experimental 2.1 Alloy preparation and heat treatment A MnNi alloy with a composition of 51.3%Mn48.7%Ni was prepared by vacuum induction melting using electrolytic nickel, and electrolytic manganese. The ingot was homogenized at 950 C for 24 hours in an argon atmosphere, and furnace cooled to 800 C at a rate of 6 C/min. The ingot was then annealed at this temperature for 24 hours, and furnace cooled to room temperature. 2.2 Microscopic observation Specimens, 11:5 mm in thickness, were cut using a low speed diamond saw. These specimens were electrochemically thinned to a 100 mm in thickness, and 3 mm discs were then punched out from these sheets. The specimens for transmission electron microscopy (TEM) were prepared using an electropolishing method in a solution of 10% perchloric acid + 90% methanol followed by ionmilling in a Gatan PIPS. The thin foils were observed on a JEOL JEM 3000F or in FEI TEHCNAI F20 microscope. To investigate the arrangement of Mn and Ni atoms in the matrix and twins, a high angle annular dark field (HAADF) image was obtained using a JEM2100F microscope equipped with a STEM Cscorrector. 3. Results 3.1 Crystal structure of MnNi phase Figure 1 shows the crystal structure and atomic arrangement in the L1 0 MnNi phase. The phase has a face centered tetragonal structure with the lattice parameter of the caxis being 6% shorter than that of the aaxis. Mn atoms lie in the basal (001) plane and Ni atoms lie in the (002) plane. The Mn and Ni columns are arranged separately in h110š beam directions ([110], ½110Š). However, in the h011š beam directions ([011], ½011Š, [101], ½101Š), Mn and Ni atoms occupy alternate layers. In Fig. 2 shows the diffraction pattern of the phase in the [110] beam and [011] beam orientations. In the [110] zone, the angle between the g111 and g111 vector was 73.8 and ordered spots such as g110 and g001 can also be observed due to the independent arrangement of the Mn and Ni columns. However, in the [011] beam direction, no ordered spots could be observed due to the alternating occupancy of Mn and Ni atoms. The angle between the g111and g111vectors is 68.8.
2 The Twin and Twin System in FCT L1 0 MnNi Phase in an Equiatomic MnNi Alloy 2547 Fig. 2 The diffraction patterns of MnNi in the [110] and [011] beam directions. Fig. 1 The crystal structure and atomic arrangement of FCT L1 0 MnNi. 3.2 Electron microscopy of L1 0 MnNi twin Highresolution (HR) image and diffraction analysis (1) In the [110] beam direction Figure 3 shows the bright field (BF), high resolution (HR) micrographs and selected area diffraction (SAD) pattern of the twin in the MnNi phase observed in the [110] beam direction. Ordered spots could be found in the Fast Fourier Transform (FFT) of the phase contrast image and the SAD pattern in Fig. 3(c). The angle between the adjacent ð111þ and ð111þ plane was approximately 74, which is identical to that of the phase at the h110š zones. However, the angle between the g111 T and g111 was approximately 72, which is different from that of the matrix. This means that the twin plane in this type of twin is not a mirror plane. (2) In the [011] beam direction Figure 4 shows another type of twin and SADP in the [011] beam direction. The ordered spot could not be found in the FFT and SADP at this orientation. The angle between the g111 and g111 vectors was approximately 68, which is the same as the type of h011š zones in the phase. In the case of the twin observed in the [011] direction, the angle between the g111 and g111 T vector was approximately 70, which is also different from that of the phase. Fig. 3 Twins of the MnNi phase observed in the [110] beam direction BF image, HR image, (c) SAD Pattern from, and (d) lay diagram of (c).
3 2548 Y.U. Heo and H.C. Lee T T T T 111 (c) (d) Fig. 4 Twins of MnNi at the [011] beam direction, HR image and SADP of and (d) lay diagram of (c). Twin θmatrix (c) Fig. 5 HAADF HR image and filtered image of the matrix and twin observed in the [110] beam direction and (c) the intensity profiles of the marked lines (a d).
4 The Twin and Twin System in FCT L1 0 MnNi Phase in an Equiatomic MnNi Alloy 2549 Fig. 6 The atomic arrangement in the [110] orientation. Fig. 7 Twinning shear angle,, as a function of the c=a ratio in a FCT crystal Zcontrast image analysis Figure 5 shows a STEM HAADF HR image and the intensity profiles of the Mn and Ni columns at the matrix and twin in the [110] beam direction. In the [110] beam direction, Mn and Ni atoms were separated in alternating (002) planes. Although the difference in the atomic number between Mn and Ni atoms is small, the difference in scattering intensity will increase with increasing thickness of the thin foil. The Ni columns in the [110] zone are brighter than that of the Mn columns. Figure 5 shows stronger Ni columns and weaker Mn columns in the twin and matrix. The intensity profiles of lines a and c in Fig. 5(c) was > However, the intensity of lines b and d ranged from to This suggests that lines a and c are Ni columns and lines b and d are Mn columns. This difference in brightness could be noticed more easily in the filtered image of Fig. 5. Figure 6 shows the atomic arrangement in the [110] orientation. This confirms that the Zcontrast image in Fig. 5 matches that of Fig Discussion 4.1 The shear angle of fct L1 0 MnNi phase In the diffraction patterns shown in Fig. 3 and Fig. 4, the angle between the adjacent {111} type planes in the twin were different from that of the matrix. This difference can be understood by calculating the shear angle in the twin. Figure 7 shows the twinning shear angle,, in the fct structure. The final equation in Fig. 7 shows the shear angle to be a function of the tetragonal aspect ratio (c=a). If the aspect ratio is 1, as is the case of a fcc crystal, the shear angle would be The shear angle was found to be in the case of the phase. Therefore, twin plane in the phase cannot be the mirror plane. 4.2 The twin system of L1 0 MnNi phase Figure 8 shows the Thompson s tetrahedral in the FCT MnNi. In the fct phase, the Burgers vectors of the 1=6h211Š type Shockley partial dislocations are longer than that of the 1=6h112Š type Burgers vectors. Moreover, when the f111g1=6h211š twin system is present, the crystal structure can change to a L1 1 structure. 4,7,8) This will increase the total energy of the system. This type of twin system was barely observed in the L1 0 system. Fig. 8 Thompson s tetrahedra in the MnNi (FCT) structure. Table 1 Allowed Twin systems in an MnNi (L1 0 ) structure at a specific beam direction Beam direction [110] [011] [101] Twin plane Shockley partial dislocation Distance of Shockley partial dislocation vector Twin system (111) 1/6[112] Short (111) 1/6[112] (111) 1/6[112] Short (111) 1/6[112] (111) 1/6[211] Long (111) 1/6[211] (111) 1/6[211] Long (111) 1/6[211] (111) 1/6[121] Long (111) 1/6[121] (111) 1/6[121] Long (111) 1/6[121] However, in addition to the ð111þ 1=6½112Š type truetwin system, the ð111þ 1=6½211Š type pseudotwin system was found in the phase, as shown in Figs. 3 and 4. The diffraction pattern in the [101] beam orientation was identical to that of the [011] zone in the fct phase. The twin in the [101] zone was also a pseudotwin and is identical to that of the [011] zone. It can be concluded that the ð111þ 1=6½121Š and ð111þ 1=6½121Š twin systems in the [101] zone as well as the ð111þ 1=6½211Š type pseudotwin system in the [011] zone are possible. Table 1 shows all possible twin systems in the L1 0 MnNi phase. In addition to the f111g1=6h112š truetwin systems, the f111g1=6h211š pseudotwin systems were also allowed in
5 2550 Y.U. Heo and H.C. Lee the L1 0 MnNi phase. This is in contrast to previous reports on the L1 0 twin system. 4,7 10) 4.3 Atomic shuffling in the twin of L1 0 MnNi phase It was suggested that twins in the ordered phase were accompanied by atomic shuffling. 6,7) However, there is a report showing that no atomic shuffling is required in the L1 0 truetwin system but no clear evidence was provided. 4) The Zcontrast image in Fig. 5 shows the ordering of Mn and Ni atoms in the weaker Mn and stronger Ni columns in the matrix as well as in the twin. This ordering did not disappear in the twin. This is clear evidence that there is no atomic shuffling in the ð111þ1=6½112š truetwin system. It was not possible to confirm the atomic shuffling in the pseudotwin system because the ordering could not be observed in the [011] and [101] beam orientations. 5. Conclusion The twin system in the L1 0 MnNi phase was examined using TEM. In contrast to previous reports on L1 0 twin systems, it was confirmed that the L1 0 phase has f111g1=6h211š pseudotwin systems as well as f111g1=6h112š truetwin systems. The SAD patterns also confirmed that the twin plane is not a mirror plane in both the truetwinning and pseudotwinning systems. This was attributed to the variation in the shear angle with respect to the aspect ratio (c=a). The Zcontrast image analysis revealed that a pure twinning shear occurred without atomic shuffling during the operation of the f111g 1=6h112Š type truetwin systems. Acknowledgement The authors wish to thank Dr. Tetsuo Oikawa, Dr. Hideyuki Takahashi, Mr. Eiji Okunish, and Mr. Tomoaki Mukai for their support of the experimental work with Cscorrected STEM at the JEOL technical center. REFERENCES 1) R. E. ReedHill: Physical Metallurgy Principles, 3nd, PWS Publ. Com., Boston, ) D. Shechtman, M. J. Blackburn and H. A. Lipsitt: Metall. Trans. 5 (1974) ) T. Kawabata and O. Izumi: Scripta Metall. 21 (1987) ) Y. Q. Gao and S. H. Whang: Scripta Metall. 31 (1994) ) A. S. Murthy and E. Goo: Acta Metal. Mater. 41 (1993) ) J. W. Christian and D. E. Laughlin: Acta Metal. 36 (1988) ) M. H. Yoo, C. L. Fu and J. K. Lee: J. Phys. III 1 (1991) ) Z. Jin and G. T. Gray III: J. Mater. Sci. 33 (1998) ) J. G. Wang, L. C. Zhang, G. L. Chen and H. Q. Ye: Mater. Sci. and Eng. A252 (1998) ) S. H. Whang, Q. Feng and Y.Q. Gao: Acta mater. 46 (1998) ) Q. F. Xiao, E. Bruck, Z. D. Zhang, F. R. de Boer and K. H. J. Buschow: J. All. Comp. 364 (2004) ) I. Baele, G. V. Tendeloo and S. Amelinckx: Acta Metall. 35 (1987) ) J. W. Cahn: Acta Metall. 25 (1977)
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