Scripta METALLURGICA Vol. 18, pp. 363-366, 1984 P e r g a m o n Press Ltd.

P r i n t e d in the U.S.A. All r i g h t s r e s e r v e d

DEFORMATION BEHAVIOR OF SHAPE MEMORYT i - N i ALLOY CRYSTALS

T. S a b u r i , M. Yoshida and S. Nenno

Department o f M a t e r i a l s S c i e n c e and E n g i n e e r i n g
F a c u l t y o f E n g i n e e r i n g , Osaka U n i v e r s i t y
Yamadaoka, S u i t a , Osaka 565, J a p a n

(Received November 25, 1983)

Introduction
The shape memory e f f e c t i s c l o s e l y r e l a t e d t o a t h e r m o e l a s t i c m a r t e n s i t i c t r a n s f o r m a t i o n
and t h e shape memory s t r a i n ( t h e s t r a i n which i s r e c o v e r a b l e on h e a t i n g ) i s b r o u g h t about by
r e o r i e n t a t i o n o f t h e m a r t e n s i t e v a r i a n t s on s t r e s s i n g . The r e o r i e n t a t i o n changes a s e l f -
accommodation s t r u c t u r e o f t h e m a r t e n s i t e v a r i a n t s i n t o .a s i n g l e c r y s t a l s t a t e o f t h e m a r t e n s i t e
t h a t i s o r i e n t e d most f a v o r a b l y w i t h r e s p e c t t o t h e s t r e s s . Thus t h e c h a r a c t e r i s t i c s h a p e -
change between t h e p a r e n t and t h e m a r t e n s i t e c r y s t a l s d e t e r m i n e s t h e l i m i t o f t h e r e c o v e r a b l e
strain.
A g e o m e t r i c t r e a t m e n t o f t h e s h a p e - c h a n g e i n a n e a r e q u i a t o m i c T i - N i a l l o y ( 1 ) , b a s e d on
t h e p a r e n t - m a r t e n s i t e l a t t i c e c o r r e s p o n d e n c e and t h e l a t t i c e p a r a m e t e r s o f t h e two p h a s e s ( 2 ) ,
p r e d i c t s t h a t t h e r e c o v e r a b l e s t r a i n o f t h e Ti-Ni a l l o y i s s i g n i f i c a n t l y o r i e n t a t i o n d e p e n d e n t .
The p r e d i c t e d o r i e n t a t i o n dependence i s c h a r a c t e r i z e d by s m a l l r e c o v e r a b l e elongations(--3%) in
d i r e c t i o n s c l o s e t o [001] and l a r g e r e c o v e r a b l e e l o n g a t i o n s ( 8 ~ 1 0 % ) i n d i r e c t i o n s c l o s e t o
[011] and [111].
We have little experimental information about deformation behavior of single crystals of
the near equiatomic Ti-Ni alloys, although we have a large stock of information about the
polycrystalline alloys (3-18). The orientation dependence of the recoverable strain appears
to be of basic importance in improving the mechanical properties of the polycrystalline Ti-Ni
alloys. Thus the present investigation was undertaken to examine experimentally the orienta-
tion dependence of the deformation behavior in the Ti-Ni alloys by tensile tests on single
crystal specimens.
Regarding pseudoelasticit~ the results of the tensile tests on the single crystals were
compared with those of the polycrystalline specimens with different grain sizes.
Experimental Procedure
A Ti-S0.Sat.%Ni (nominal composition) alloy was prepared by vacuum melting in a graphite
crucible. By cooling the molten alloy slowly in the crucible, very coarse grains were
obtained in the ingot. Single crystal specimens for tensile tests were prepared from the
large grains of the ingot. Fine grain (50~m in diameter) polycrystal specimens were prepared
by hot-rolling a part of the ingot at 800°C into a sheet 0.gmm thick. Beside these, specimens
of intermediate grain size (Imm in diameter) were prepared from a relatively fine-grained
part of the ingot. All these specimens were annealed in evacuated capsules at 800°C for
5.6ks and quenched into iced water. Then they were aged at 500°C for 3.6ks and quenched again.
After the heat treatment, specimens were polished mechanically to remove the oxidized surface
layer and then they were electropolished to remove the strained surface layer in an electro-
lyte of acetic acid (95%) and perchloric acid (7%). The final size of the specimens was
typically ix0.4x20rmn. Orientations of the single crystal specimens were determined by the
Laue back-reflection technique. Tensile tests were performed at a cross-head speed of
8.Sx10-3w~/s, the gage length being 10mm. The tests at temperatures between -100°C and 0°C
were carried out in a methyl-alcohol bath cooled by liquid nitrogen. A water bath was used
for the tests at temperatures above 0°C. Optical microscope observation was made on the stress-
induced martensite and the habit-plane indices were determined by two-surface trace analysis.
Results and Discussion
(I) Deformation behavior
Figure 1 shows a series of tensile stress-strain curves at temperatures between -70°C

363
0 0 3 6 - 9 7 4 8 / 8 4 $3.00 + .00
C o p y r i g h t (c) 1984 P e r g a m o n Press Ltd.
364 DEFORMATION OF Ti-Ni CRYSTALS Vol. 18, No. 4

001 011 FIG. 1

Stress-strain curves of a
Ti-50.5at.%Ni single crystal
specimen. Temperatures shown
in the figure are the test
temperatures. Tensile axis:
_ ,°°I- f / B.

' ,/.
0
,r.~I°° u.J

20!
•-J Or , , II i i
0

Io(J

0 ! 2 3 40 l 2 l 4 | 40 2
STRAIN (%1 STRAIN (,~)

FIG. 2
~ 200 Yield stress (0.5% offset stress)
= versus test temperature curve as
~ obtained from Fig. i.
100

/J
t i | i ii
0 ' -6'0 -4'0 -20 0 6 2'0 i 4'0
Temperature "C
and 40oC for a single crystal specimen whose tensile axis is B in the unit triangle as shown
at the top right of the figure. Tensile stress was applied till the specimen was elongated
by about 4~ and then the stress was removed. The yield stresses (o) obtained from the stress-
s t r a i n c u r v e s were p l o t t e d a g a i n s t t h e t e s t t e m p e r a t u r e s (T) as shown i n F i g . 2. I t i s s e e n
i n t h i s f i g u r e t h a t t h e p l o t has a minimum a t about O°C and i t shows a l i n e a r r e l a t i o n i n t h e
t e m p e r a t u r e r a n g e between 20°C and 4 0 ° C , s a t i s f y i n g t h e C l a u s i u s - C l a p e y r o n r e l a t i o n . The s l o p e
o f t h e l i n e , do/dT, i s found t o be 6.THPa/°C. I t i s t o be n o t e d t h a t t h e r e i s no t e m p e r a t u r e
range where p e r f e c t p s e u d o e l a s t i c i t y b e h a v i o r a p p e a r s . At t e m p e r a t u r e s between 30°C and 40°C,
the strain disappears partly on unloading,but a large part of it remains. This is a signifi-
cant difference from the behavior of polycrystal specimens of the same chemical composition
(of the same ingot). Takei et al. (19) has also observed similar behavior in a Ti-S0.3at.~Ni
alloy single crystal. The residual strain in the single crystals, however, disappears on
heating ahove 70°C, if the strain is small.
In situ observations were made on the stress-induced transformation and reversion on
heating, and the close correlation between the shape memory effect and the martensitic trans-
formation was confirmed. Habit-plane indices were determined to be {4, S, ii I by two-
surface trace analysis.
(2) Orientation dependence of the recoverable strain
In order to examine the orientation dependence of the strain which is recoverable on
heating (the shape memory strain), the following tensile tests were performed on the specimens
with four different orientations (tensile axes) shown in the unit triangle in Fig. 3.
Specimens were strained to a certain point at IO°C (below A~), and after unloading they were
heated above 70°C. When the tensile strain was small, it dzsappeared completely on heating.
Vol. 18, No. 4 DEFORMATION OF Ti-Ni CRYSTALS 365

By gradually increasing the tensile strain, the test was repeated until an appreciable amount
of strain remained even after heating above 70°C. In this way the recoverable strain was
obtained. For example, when a specimen with the A orientation (close to [001]) was strained
by 4% and then unloaded, there remained a strain of 3%, and on heating it was recovered
completely. When the tensile strain was increased to 5%, the residual strain after unloading
was 3.7%, as can be seen in the curve A in Fig. 3. On heating, 3.1% was recovered as
indicated by an arrow (~---~ under the stress-strain curve, but ~.6% remained. In this way
we found the recoverable strain in the A orientation to be 3.1%. Similarly the recoverable
tensile strain was found to be 8.0% for the B orientation, I0.1% for the C orientation and
10.6% for the D orientation*.
The observed anisotropy in the recoverable strain agrees well with the prediction (1),
which is shown in Fig. 4. The predicted values for the A, B, C, and D orientations are 3.0%,
8.8%, 9.1%, and 10.5% respectively.
Thus far we have made clear experimentally that the orientation dependence in the shape
memory strain is significant in Ti-Ni alloy crystals. This knowledge ought to be quite
important in improving the shape memory capacity in polycrystalline Ti-Ni alloys. If we can
develop a texture in a material, we will be able to improve the memory capacity in a certain
direction. For example, a wire having a fiber axis in the range from [~ii] to [011] of the
stereographic triangle, should give a large recoverable elongation in the length direction.
(3) Grain size effect
As have been already mentioned in the preceeding section, single crystal specimens of the
Ti-50.Sat.%Ni alloy do not behave pseudoelastically at any temperature. Polycrystal
specimens (grain size: 50~m) of the same alloy, on the other hand, show complete pseudo-
elasticity above Af (30°C). Figure 5 illustrates the test results at 40°C for three
different cases; (a) grain size: 50~m, (b) grain size: lmm, and (c) single crystal. It is
clearly seen in the figure that the pseudoelasticity becomes pronounced as the grain size
decreases. The result indicates that the reduction in grain size is very effective in
improving the pseudoelasticity and that the role of the grain boundaries is important in the
pseudoelasticity of Ti-Ni alloys. Further investigations are needed for more details.
References
(i) T. Saburi and S. Nenno, Proc. International Conference on Solid-Solid Phase Trans-
formations, edited by H. I. Aaronson, D. E. Laughlin, R. F. Sekerka and C. M. Wayman,
by The Metallurgical Society of AIME, p. 1455 (1981).
(2) K. Otsuka, T. Sawamura and K. Shimizu, Phys. Stat. Sol. (a) 5, 457 (1971).
(3) A. G. Rozner and R. J. Wasilewski, J. Inst. Metals 94, 169 (1966).
(4) R. J. Wasilewski, Met. Trans. 2, 2973 (1971).
(5) J. Perkins, Scripta Met. 8, 1469 (1974).
(6) H. A. Mohamed and J. Washburn, J. Materials Science 12, 469 (1977).
(7) K. N. Melton and O. Mercier, Met. Trans. 9A, 1487 (1978).
(8) K. N. Melton and O. Mercier, Acta Met. 27, 137 (1979).
(9) T. Honma, Proc. Joint U.S./Japan Seminar on Mechanical Behavior of Metals and Alloys,
Troy, U. S. A., p. 72 (1979).
(i0) J. N. Kachin, V. E. Gjunter, V. P. Sivokha and A. S. Savvinov, Proc. International
Conference on Martensitic Transformations (ICOMAT-79), p.474 (1979).
(ll) H. C. Ling and R. Kaplow, Met. Trans. IIA, 77 (1980).
(12) K. N. Melton and O. Mercier, Acta Met. 29, 393 (1981).
(13) H. C. Ling and R. Kaplow, Materials Sci. Eng. 51, 193 (1981).
(14) H. C. Ling and R. Kaplow, Met. Trans. 12A, 2101 (1981).
(15) S. Miyazaki, K. Otsuka and Y. Suzuki, Scripta Met. 15, 287 (1981).
(16) S. Miyazaki, T. Imai, K. Otsuka and Y. Suzuki, Scripa Met. 15, 853 (1981).
(17) S. Miyazaki, Y. Ohmi, K. Otsuka and Y. Suzuki, Proc. International Conference on
Martensitic Transformations in Belgium (ICOMAT-82), Supplement to Journal de Physique
43-C4, 255 (1982).
(18) T. Saburi, T. Tatsumi and S. Nenno, Proc. International Conference on Martensitic Trans-
formations in Belgium (ICOMAT-82), Supplement to Journal de Physique 43-C4, 261 (1982).
(19) F. Takei, T. Miura, S. Miyazaki, S. Kimura, K. Otsuka and Y. Suzuki, Scripta Met. 17,
987 (1983).
(20) S. Kimura, S. Miyazaki, K. Otsuka and Y. Suzuki, Abstracts of Fall Meeting of Japan
Institute of Metals, p. 362 (1983).

*Kimura,et al. made similar experiments and found essentially the same orientation dependence
recently (20).
366 DEFORMATION OF T i - N i CRYSTALS Vol. 18, No. 4

zll A

ill
eei el i
I,

FIG. 4
STRAIN. (%)
The predicted orientation dependence of the
recoverable strain (i). The contour lines
FIG. 3
join orientations which give the same value
Orientation dependence of the recoverable of the strain (%). The figure is drawn for
strain. Deformed at IO°C and heated above the parent-martensite correspondence that
IO°C. is the most favorable for a tensile stress
along a direction in the stereographlc
triangle 001-OII-TII.

.(a} ~ Tested

"If 3
ir i i i I i i L

FIG. 5

Grain size effect on pseudoelasticity in

ZOO TI-50.5at.%Ni alloy. Tensile axis of the
single crystal in (c): orientation B in
Fig. 3.
Jorein size: I mm
e ~ i i i L 1
~ e'

'"tl /,i.,,..
.V,, /..*?""
"L~_3_J 4 s e ;
STRAIN 1%1