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TRANSFORMATION BEHAVIOR OF Ti50Ni47Fe3 ALLOY :I. INCOMMENSURATE AND
COMMENSURATE PHASES
C. Hwang, M. Meichle, M. Salamon, C. Wayman
To cite this version:
C. Hwang, M. Meichle, M. Salamon, C. Wayman. TRANSFORMATION BEHAVIOR OF
Ti50Ni47Fe3 ALLOY :I. INCOMMENSURATE AND COMMENSURATE PHASES. Journal de
Physique Colloques, 1982, 43 (C4), pp.C4-231-C4-236. �10.1051/jphyscol:1982430�. �jpa-00222144�
JOURNAL DE PHYSIQUE
CoZZoque C4, suppte'ment au n o 22, Tome 43, dicembre 2982 page C 4 - 2 3 1
TRANSFORMATION BEHAVIOR OF T i N i Fe ALLOY:
5 0 4 7 3
I, INCOMMENSURATE AND COMMENSURATE PHASES
C.M. H w a n g , M. M e i c h l e , M.B. Salamon and C.M. Wayman University of IZZinois, Urbana, IZZinois 61801, U. S . A.
( A c c e p t e d 9 A u g u s t 1982)
Abstract.- The t r a n s f o r m a t i o n b e h a v i o r o f TiNiFe a l l o y s o f nominal c o m p o s i t i o n T i Ni Fe has been s t u d i e d by t r a n s m i s s i o n e l e c t r o n microscopy and
di?!ra:iioi, and e l e c t r i c a l r e s i s t a n c e measurements, between room temperature and -19h°C. Based on t h e p r e s e n t r e s u l t s and complementary n e u t r o n and x-ray d i f f r a c t i o n data, charge d e n s i t y wave (CDW) phenomena and a s s o c i a t e d phase t r a n s i t i o n s were found t o be i n v o l v e d i n t h e " p r e m a r t e n s i t i c " b e h a v i o r o f t h e Ti50Ni47Fe3 a l l o y s . The c r y s t a l s t r u c t u r e o f t h e h i g h temperature p a r e n t phase was c o n f i r m e d t o be t h e CsCl(B2) s t r u c t u r e . Upon c o o l i n g below room temperature, 1/3(110) and 1/3(111) super1 a t t i c e r e f l e c t i o n s appeared,
c o i n c i d e n t w i t h t h e o n s e t o f an e l e c t r i c a l r e s i s t a n c e anomaly (increase). The
"1/3" s u p e r l a t t i c e r e f l e c t i o n s were observed t o i n t e n s i f y w i t h d e c r e a s i n g temperature, and c l o s e i n s p e c t i o n showed t h a t such r e f l e c t i o n s d e v i a t e s l i g h t l y f r o m t h e e x a c t 1/3 p o s i t i o n s r e l a t i v e t o t h e p a r e n t CsCl s t r u c t u r e , s u g g e s t i n g t h e f o r m a t i o n o f an incommensurate s u p e r l a t t i c e o v e r a 12OC temperature range. The appearance o f t h e "113" s u p e r l a t t i c e r e f l e c t i o n s i s i n t e r p r e t e d t o be a s s o c i a t e d w i t h t h e f o r m a t i o n o f CDW's. A second
" p r e r n a r t e n s i t i c ' e f f e c t was found t o o c c u r a p p r o x i m a t e l y 12OC below t h e onset o f t h e i n i t i a l "normal-to-incommendurate" t r a n s i t i o n . T h i s subsequent phase change i n v o l v e s a s t r u c t u r a l t r a n s i t i o n from a " d i s t o r t e d " CsCl p a r e n t t o a rhombohedral product, d u r i n g which t h e "113" s u p e r l a t t i c e r e f l e c t i o n s a r e s h i f t e d t o p r e c i s e 1/3 p o s i t i o n s . The rhombohedral d i s t o r t i o n i s e f f e c t e d by a homogeneous expansion a l o n g <Ill> d i r e c t i o n s , a l l o w i n g t h e l a t t i c e and CDW1s t o l o c k - i n and become commensurate.
I n t r o d u c t i o n . - Equiatomic T i N i
,
one o f t h e f i r s t known shape memory a l l o y s ( I ) , has been t h e s u b j e c t o f i n t e n s i v e i n v e s t i g a t i o n f o r t h e p a s t t w e n t y years. I t i s known t h a t TiNi undergoes a m a r t e n s i t e t r a n s f o r m a t i o n s l i g h t l y above roorn temperature.The rnartensi t e t r a n s f o r m a t i o n i n T i N i e x h i b i t s p r e m o n i t o r y o r " p r e m a r t e n s i t i c "
phenomena immediately above t h e m a r t e n s i t e s t a r t (M ) temperature, such as an e l e c t r i c a l r e s i s t i v i t y anomaly (2-7), s t r e a k s i n e l k t r o n d i f f r a c t i o n p a t t e r n s (2,3,6,8,9), and "1/3" s p o t s seen i n b o t h x-ray and e l e c t r o n d i f f r a c t i o n p a t t e r n s (6,lO). Other anomalies i n p h y s i c a l o r mechanical p r o p e r t i e s have a l s o been
reported, such as decreases i n sound v e l o c i t y (3,11), e l a s t i c modulus (12), i n t e r n a l f r i c t i o n peaks (12,13), s p e c i f i c heat peak (14,15), etc. The n a t u r e o f t h e s e
" p r e m a r t e n s i t i c " phenomena has l o n g been an enigma.
I t was observed t h a t s u b s t i t u t i n g 3% Fe f o r Ni i n T i N i can suppress t h e Ms temperature more s t r o n g l y t h a n t h e p r e 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 temperature
(T ) ( l h ) , t h u s s e p a r a t i n g t h e temperature range o f t h e p r e r n a r t e n s i t i c
t r % n s f o r m a t i o n from t h a t o f t h e 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 , t h e r e b y r e v e a l i n g a d i s t i n c t premartensi t i c phase. Thus, t h e Ti50Ni47Fe a1 l o y i s i d e a l f o r s t u d y i n g t h e p r e r n a r t e n s i t i c phenomena w i t h o u t " i n t e r f e r e n c e "
gram
t h e m a r t e n s i t i ct r a n s f o r m a t i o n .
We have undertaken a study o f t h e t r a n s f o r m a t i o n b e h a v i o r i n T i Ni Fe e s p e c i a l l y t h e n a t u r e o f t h e p r e m a r t e n s i t i c phenomena, by means o f e78cttTca3'
Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1982430
super1 a t t i c e r e f l e c t i o n s were a1 so seen. T y p i c a l s e l e c t e d a r e a d i f f r a c t i o n (SAD) p a t t e r n s o f t h e " p r e m a r t e n s i t i c " phase showing t h e 1/3(110) s u p e r l a t t i c e r e f l e c t i o n s i n [100IR7 and [111IR2 zones a r e shown i n Fig. 2. The "1/3" s u p e r l a t t i c e
Fig. 2: T y p i c a l e l e c t r o n d i f f r a c t i o n p a t t e r n s o f t h e p r e m a r t e n s i t i c phase o f t h e TiS0Ni 47Fe3 a1 l o y showing 1 / 3 (110) s u p e r l a t t i c e r e f l e c t i o n s . ( a ) and ( b )
correspond t o and [llllg2 zones, r e s p e c t i v e l y .
F i g . 3: E l e c t r o n d i f f r a c t i o n p a t t e r n s showing t e m p e r a t u r e dependence of 113 (110) s u p e r l a t t i c e r e f l e c t i o n s i n t h e [1113 zone. The s u p e r i a t t i c e
r e f 1 e c t i 0% appeared around O°C and i n t e n s i f i e d w i t h d e c r e a s i n g
temperature. ( a ) 4OC, ( b ) O°C, and ( c ) -4OC.
r e f l e c t i o n s were observed t o i n t e n s i f y w i t h d e c r e a s i n g temperatures, as shown i n F i g . 3. The change o f i n t e n s i t y i s r e v e r s i b l e w i t h t e r r p e r a t u r e and i s obvious between O°C and -10°C b u t n o t s o o b v i o u s a t l o w e r temperatures. The p o s i t i o n s of t h e 1/3(110) s u p e r l a t t i c e r e f l e c t i o n s were examined c l o s e l y by measuring t h e spacing between them. The r e s u l t s o f such measurements showed t h a t t h e 1/3(110) r e f l e c t i o n s
C4-234 JOURNAL DE PHYSIQUE
d e v i a t e d s l i g h t l y f r o m t h e e x a c t 1/3 p o s i t i o n r e l a t i v e t o t h e p a r e n t CsCl s t r u c t u r e over a 12OC temperature range. More q u a n t i t a t i v e measurements on t h e i n t e n s i t i e s and p o s i t i o n s o f t h e s u p e r l a t t i c e r e f l e c t i o n s u s i n g n e u t r o n o r x - r a y d i f f r a c t i o n gave p a r a l l e l r e s u l t s .
A n t i p h a s e - l i k e microdomains (APD's) -15008 i n d i a m e t e r were r e v e a l e d i n dark- f i e l d images u s i n g t h e "1/3" r e f l e c t i o n s . A t y p i c a l example o f t h e APU's i s shown i n Fig. 4. These microdomains a r e s i m i l a r t o a n t i p h a s e domains i n o r d e r e d a l l o y s .
Fig. 4: T y p i c a l example showing a n t i p h a s e domains(AP0's) i n t h e p r e m a r t e n s i t i c phase o f t h e Ti50Ni4 F e j a l l o y . (a) dark f i e l d e l e c t r o n m i c r o g r a p h showing APU's, ( b ) c o r r e s p o n d i n g s e l e c t e d area d i f f r a c t i o n p a t t e r n showing t h e 1/3(110)
s u p e r l a t t i c e r e f l e c t i o n used f o r t h e dark f i e l d imaging, and ( c ) b r i g h t f i e l d image.
However, no APD's a r e seen i n t h e d a r k - f i e l d images t a k e n by u s i n g (100) t y p e s u p e r l a t t i c e r e f l e c t i o n s i n t h e p a r e n t phase as w e l l as i n t h e prernarten!?iic
temperature r e g i o n s . It was n o t e d t h a t APD's a r e teiilperature independent, i .e., t h e domain s i z e and shape do n o t change w i t h t e m p e r a t u r e i n t h e p r e m a r t e n s i t i c regime.
A t about 12°C below T
,
n e e d l e - l i k e microdomains f o r m i n t h e T i 50 47 .3 Ni Fe a l l o y . The t e m p e r a t u r e coPresponding t o t h e f o r m a t i o n o f t h e "needle domains w i l l be c a l l e d Td. A t y p i c a l example o f n e e d l e domains i s shown i n F i g . 5(a). F i g u r e 5 ( b ) i s t h e c o r r e s p o n d i n g SAD p a t t e r n taken from t h e e n c i r c l e d r e g i o n i n F i g . 5(a).( a ) Transmission e l e c t r o n m i c r o g r a p h showing p a r a l 1 e l need1 e domains.
'*:responding s e l e c t e d area d l f f r a c t i on p a t t e r n t a k e n f rorn b o t h t h e need1 e domains and t h e m a t r i x r e g i o n . T h i s d i f f r a c t i o n p a t t e r n i s a superimposed p a t t e r n which c o n s i s t s o f t h e [001] and [201] zones. The i n n e r " s p l i t " s p o t s correspond LO t h e [2O1IH zone. Both t # e [201IH a#d [001lH zones a r e d e r i v e d from a
zone.
The p r e m a r t e n s i t i c s t - u c t u r e o f b i n a r y T i N i was r e p o r t e d t o be rhombohedra1
(2,8). E l e c t r o n d i f f r a c t i o n p a t t e r n s o f t h e rhombohedral s t r u c t u r e o f t h e m a r t e n s i t i c phase i n Au-5Oat.%Cd a r e w e l l - e s t a b l i s h e d (18). A s e r i e s o f SAD p a t t e r n s o f t h e TiS0Ni 7Fe3 a l l o y i n t h e p r e m a r t e n s i t i c s t a t e between Td and Ms was taken. A comparison 04 t h e p r e s e n t r e s u l t s w i t h t h e SAD p a t t e r n s o f t h e
rhombohedral s t r u c t u r e ( l a ) , shows t h a t t h e y a r e i d e n t i c a l i n symmetry. I n
a d d i t i o n , n e u t r o n and x-ray d i f f r a c t i o n (19), as w i l l be d i s c u s s e d l a t e r , show t h a t t h e p r e m a r t e n s i t i c s t r u c t u r e o f T i N i F e between Td and M i s rhombohedral. The SAD p a t t e r n s a r e t h e r e f o r e indexed a c c o r d i n g t o t h e rhombohsdral s t r u c t u r e i n terms o f hexagonal i n d i c e s . The d i f f r a c t i o n p a t t e r n i n F i g . 5(b) i s i n t e r p r e t e d as a superimposed d i f f r a c t i o n p a t t e r n w h i c h c o n s i s t s o f two o r i e n t a t i o n s . The i n n e r
" s p l i t " s p o t s correspond t h e [201IH zone, w h i l e t h e o u t e r " s p l i t " s p o t s correspond t o t h e [OOl] zone. It was proven by d a r k - f i e l d imaging t h a t t h e "needle" domains correspond t! [201IH ( i n n e r s p o t s ) and t h e m a t r i x corresponds t o [ O O l l H ( o u t e r spots). Three v a r i a n t s o f "needle" domains i n a d d i t i o n t o t h e m a t r i x were u s u a l l y seen t o f o r m below T
.
The disappearance o f "needle" domains upon h e a t i n g shows some thermal hystersqs, i.e., "needle" domains c o m p l e t e l y d i s a p p e a r above T.
Amore d e t a i l e d a n a l y s i s o f t h e "needle" domains shows t h a t t h e y can be i d e n t ' i l f i e d a s t w i n s w i t h a {110} t w i n n i n g plane.
The p o s i t i o n s o f 1/3(110) t y p e s u p e r l a t t i c e r e f l e c t i o n s o f t h e p r e m a r t e n s i t i c phase below T were examined c l o s e l y . W i t h i n t h e acsuracy o f measurements, t h e s p a c i n g betwegn s u p e r l a t t i c e r e f l e c t i o n s a l o n g <110> a r e t h e same, i.e., t h e 1/3(110) r e f l e c t i o n s a r e a t e x a c t 1 / 3 p o s i t i o n s o f t h e <110> r e c i p r o c a l l a t t i c e v e c t o r . X-ray d i f f r a c t i o n (19) a1 so showed t h a t t h e "1/3" super1 a t t i c e r e f l e c t i o n s s h i f t t o e x a c t 113 p o s i t i o n s a t T and remain commensurate w i t h t h e Bragg
r e f l e c t i o n s o f t h e rhombohedral s e r u c t u r e i n t h e p r e m a r t e n s i t i c s t a t e . Td v a l u e s a r e -lZ°C and -4g°C f o r Ti50Ni47Fe3 and Ti50.1Ni46.7Fe3.2 r e s p e c t i v e l y .
D i s c u s s i o n and Conclusions.- Two phase t r a n s f o r m a t i o n s r a t h e r t h a n one a r e found t o be a s s o c i a t e d w i t h t h e p r e m a r t e n s i t i c b e h a v i o r i n t h e Ti50Ni4 Fe3 a l l o y . A t T
,
t h e f o r m a t i o n o f "1/3" t y p e s u p e r l a t t i c e r e f l e c t i o n s i s c o i n c l d e n z w ~ t h t h e s t a r t8f
t h ee l e c t r i c a l r e s i s t a n c e anomaly ( i n c r e a s e ) on c o o l ing. The APD's formed
s i m u l t a n e o u s l y when t h e c r y s t a l developed "1/3" s u p e r l a t t i c e r e f l e c t i o n s . A t a s t i l l l o w e r temperature, Td, n e e d l e - l i k e domains were seen t o form. Anomalies i n t h e temperature d e r i v a t i v e o f t h e e l e c t r i c a l r e s i s t i v i t y vs. t e m p e r a t u r e c u r v e and s p e c i f i c h e a t peak a p p e a r i n g around Td were a l s o observed (19). The m i c r o s t r u c t u r e change as w e l l as p h y s i c a l p r o p e r t y anomalies a t T i n d i c a t e t h a t a second p o s s i b l e
" p r e 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 occurs a t a l o w e r t e m p e r a t u r e t h a n t h a t o f t h e f i r s t . The t r a n s f o r m a t i o n temperatures a r e T
-
OOC, Td-
-12OC and T-
-41°C and Td-
-4g0c f o r t h e Ti50Ni47Fe3 and t h e Ti50.1Ni46.7Fe3.2 a1 l o y s , r e s p e @ t i v e l y .The p o s i t i o n s o f t h e 1/3(110) s u p e r l a t t i c e r e f l e c t i o n s were found n o t a t e x a c t 1/3 p o s i t i o n s between two fundamental r e f l e c t i o n s . Neutron d i f f r a c t i o n experiments (20) showed q u a n t i t a t i v e l y t h a t t h e 1/3(110) r e f l e c t i o n s a r e d i s p l a c e d s l i g h t l y toward t h e n e a r e s t fundamental r e f l e c t i o n s by about 0.45% a t t h e onset. The s i g n i f i c a n c e o f t h i s f i n d i n g i s t h a t i t proves t h e f o r m a t i o n o f a 1/3(1-d ) ( 1 1 0 ) incommensurate s u p e r l a t t i c e w i t h d
-
0.0045. The appearance o f an incomaensurate s u p e r l a t t i c e i s s t r o n g evidence t h i t a f e r m i - s u r f a c e d r i v e n phenomena, such as t h e f o r m a t i o n o f a charge d e n s i t y wave (21) occurs i n t h e p r e m a r t e n s i t i c s t a t e o f t h e TiNiFe a l l o y s . The f o r m a t i o n o f t h e s u p e r l a t t i c e r e f l e c t i o n s i s due t o t h e CDW s u p e r s t r u c t u r e s f o r m i n g on t h e p a r e n t c u b i c s t r u c t u r e . However, t h e CDW f o r m a t i o n s h o u l d i m p l y atomic displacement o r a l a t t i c e d i s t o r t i o n . The f a c t t h a t t h e i n t e n s i t y o f t h e 1/3(1-d ) (110) s u p e r l a t t i c e r e f l e c t i o n s i n c r e a s e s c o n t i n u o u s l y from z e r o on c o o l i n g i m p t i e s a c o n t i n u o u s change o f o r d e r parameter w h i c h i s an i n d i c a t i o n o f a second o r d e r normal-to-incommensurate phase t r a n s i t i o n . 1/3(111) t y p e s u p e r l a t t i c e r e f l e c t i o n s were a l s o found i n t h e [ l l O ] zone e l e c t r o n d i f f r a c t i o n p a t t e r n s . X-ray d i f f r a c t i o n (19) showed q u a n t % ? a t i v e l y t h e incommensurate n a t u r e o f t h e s e 1/3(1-d ) (111) s u p e r l a t t i c e r e f l e c t i o n s w i t h d2-
0.012 a t t h e onset. The n a t u r e o f t h e f i r s t p r e m a r t e n s i t i c phaset r a n s f o r m a t i o n i s t h e r e f o r e a second o r d e r normal-to-incommensurate t r a n s i t i o n w i t h t h e f o r m a t i o n o f two p o s s i b l e CDW's. The APD's a p p e a r i n g i n t h e incommensurate s t a t e o f t h e TiNiFe a1 1 oy, a r e s u g g e s t i v e o f discommensuration-type domains (22),
C 4 - 2 3 6 JOURNAL DE PHYSIQUE
although, anomalously, t h e APD s i z e i s temperature independent.
A system i n an incommensurate s t a t e can l o w e r i t s t o t a l energy by f u r t h e r t r a n s f o r m i n g t o a commensurate s t a t e , t h e so c a l l e d "lwcked i n " s t a t e . F o r t h e T i Ni Fe a l l o y , t h e 1/3(110) t y p e s u p e r l a t t i c e r e f l e c t i o n s i n t h e e l e c t r o n
,
di?!ra?iio; p a t t e r n s were found t o become s i t u a t e d a t 1/3 p o s i t i o n s a l o n g <110> a t lower temperatures i n t h e p r e m a r t e n s i t i c region. A f t e r t h e rhombohedral d i s t o r t i o n , 1/3(111) t y p e s u p e r l a t t i c e r e f 1 e c t i o n s were found by x-ray d i f f r a c t i o n (19) t o become commensurate w i t h t h e Bragg r e f l e c t i o n s a t T
.
The 1/3(111) r e f l e c t i o n s remain commensurate w i t h t h e new Bragg peak even thgugh t h e rhombohedral d i s t o r t i o n i s continuous on f u r t h e r c o o l i n g . The h i g h temperature p a r e n t phase has a c u b i c (CsC1) s t r u c t u r e and i t i s an incommensurate phase between T and T.
So t h e second" p r e 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 i n v o l v e s a " d i s t o r t e d " c u b i c P t o a rdombohedral product. The rhombohedral d i s t o r t i o n i s e f f e c t e d by a homogeneous expansion a l o n g
<Ill> d i r e c t i o n s , a l l o w i n g t h e l a t t i c e and COW'S t o l o c k - i n and become
commensurate. T h i s b e h a v i o r i s d i f f e r e n t from t h e l o c k - i n mechanism i n l a y e r e d compounds (21). The h y s t e r e s i s e f f e c t i n t h e appearance and disappearance o f
"needle" domains i n d i c a t e s t h a t t h e l o c k - i n t r a n s i t i o n i s f i r s t order. Therefore, n a t u r e o f t h e second " p r e 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 i n Ti50Ni47Fe3 a l l o y i s a f i r s t o r d e r incommensurate-to-commensurate CDW t r a n s i t i o n and i s a s s o c i a t e d w i t h a
" d i s t o r t e d " c u b i c t o rhombohedral t r a n s f o r m a t i o n .
Acknowledgements.- T h i s work was supported by t h e N a t i o n a l Science Foundation t h r o u g h t h e M a t e r i a l s Research L a b o r a t o r y a t t h e U n i v e r s i t y o f I l l i n o i s , Grant NSF DMR 80-20250-10. The experimental a l l o y was k i n d l y p r o v i d e d by t h e Raychem Corporation, Menlo Park, C a l i f o r n i a .
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