HAL Id: jpa-00226573
https://hal.archives-ouvertes.fr/jpa-00226573
Submitted on 1 Jan 1987
HAL is a multi-disciplinary open access archive for the deposit and dissemination of sci- entific research documents, whether they are pub- lished or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers.
L’archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d’enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.
STUDIES ON EARLY AND LATE STAGES OF FORMATION OF δ’ PHASES IN Al-Li ALLOYS BY
NEUTRON SMALL ANGLE SCATTERING
S. Fujikawa, M. Furusaka, M. Sakauchi, K. Hirano
To cite this version:
S. Fujikawa, M. Furusaka, M. Sakauchi, K. Hirano. STUDIES ON EARLY AND LATE STAGES OF FORMATION OF δ’ PHASES IN Al-Li ALLOYS BY NEUTRON SMALL ANGLE SCATTERING.
Journal de Physique Colloques, 1987, 48 (C3), pp.C3-365-C3-372. �10.1051/jphyscol:1987342�. �jpa-
00226573�
JOURNAL DE PHYSIQUE
Colloque C3, supplkment au n09, Tome 48, septembre 1987
STUDIES ON EARLY AND LATE STAGES OF FORMATION OF 6 ' PHASES IN A1-Li ALLOYS BY NEUTRON SMALL ANGLE SCATTERING
S. FUJIKAWA
,
M. FURUSAKA",
M. SAKAUCHI and K. HIRANOTohoku
University, Departmento f
Materials Science, J-Sendai 980, Japan" ~ o h o k u
University, Physics Department, J-Sendai 980, JapanA b s t r a c t
The phase s e p a r a t i o n process i n A1-9.5 and 11.4 a t . % L i a l l o y s a ed a t 423 K has been s t u d i e d o v e r a wide q ( = ( h s i n ~ ) / i ) range ( 0 . 0 6 r q r 6 nm-1) w i t h tRe p u l s e d c o l d n e u t r o n s m a l l a n q l e s c a t t e r i n q i n s t r u m e n t a t N a t i o n a l L a b o r a t o r v f o r Hiqh Enerqv Physics. A t v e r y e a r l y s t a e- c a t t e r j n g f u n c t i o n p t t h e h i g h
$
s i d eii
n o t o i i y p r o p o r t i o n a l t o q-2, q-4 an!4-6.
b u t i t obeys n o n - ~ n t e g e r p we 0 g . The power changes c o n t i n u o u s l y from q-1.5 o r q-2-t.o q - 6 - i n v e r y s h o r t t i m e . A t t h e l a t e s t a g e , t h e s c a t t e r i n g f u n c t i o n c o n s i s t s o f q-4and qadependences. The v e r y i n t e r e s t i n g r e s u l t s can n o t be s a t i s f a c t o r i l y e x p l a i n e d by t h e e x i s t i n g t h e o r i e s . The phase s e p a r a t i o n a t t h e v e r y e a r l y s t a g e t a k e s p l a c e by t h e s p i n o d a l mechanism, b u t some d e v i a t i o n s a r e observed f r o m t h e l i n e a r s p i n o d a l t h e o r y . A t t h e l a t e stage, t h e dynamic s c a l i n g l a w proposed by Furukawa and L e b o w i t z d e s c r i b e s w e l l t h ee x p e r i m e n t a l r e s u l t s .
I n t r o d u c t i o n
I t i s w e l l known t h a t t h e m e t a s t a b l e A13Li ( 6 ' ) phases i n A1-Li a l l o y s a r e r a p i d l y formed and t h e y t e n d t o be s h e r i c a l because o f t h e s m a l l coherency s t r a i n . However, i t i s s t i l l u n c e r t a i n whether 6 ' phases a r e formed b y s p i n o d a l decomposition, by n u c l e a t i o n and growth, o r by t r a n s f o r m a t i o n o f o t h e r m e t a s t a b l e phases i n
c o n t r o v e r s y . G e n e r a l l y , i t i s d i f f i c u l t t o i n v e s t i g a t e q u a n t i t a t i v e l y t h e mechanism o f t h e e a r l y s t a g e o f f o r m a t i o n o f 6 ' phases u s i n g u s u a l methods such as a n e l e c t r o n microscopy, c a l o r i m e t r y and r e s i s t i v i t y measurement. n a d d i t i o n , t h e l a t e s t a g e has been o f t e n s t u d i e d by X-ray s m a l l a n g l e s c a t t e r i n g f l ),(2), b u t i t i s n o t easy t o s t u d y t h e e a r l y s t a g e by t h e method. On t h e o t h e r hand, n e u t r o n s m a l l a n g l e
s c a t t e r i n g i s v e r y u s e f u l f o r t h e s t u d y o f t h e e a r l y s t a g e because o f t h e l a r g e d i f f e r e n c e between n e u t r o n s c a t t e r i n g l e n g t h b ~ 1 and b ~ i . Recently, t h e k i n e t i c s o f phase s e p a r a t i o n o f quenched a l l been o f t e n i s t i a t e d by t h e dyanamical s c a l i n g l a w proposed by Furukawa
?Y?,?n
and ~ebowitzi'F'7.?
t i s v e r y i n t e r e s t i n g t o s t u d y by n e u t r o n s m a l l a n g l e s c a t t e r i n g whether t h e dynamic s c a l i n g l a w h o l d s t o t h e l a t e s t a g e o f f o r m a t i o n o f 6 ' phases o r n o t .I n t h e p r e s e n t work, we g i v e t h e r e s u l t s c o n c e r n i n g t h e t i m e e v o l u t i o n o f t h e s c a t t e r i n g i n t e n s i t y from t h e v e r y e a r l y s t a g e t o t h e l a t e s t a g e o f t h e phase s e p a r a t i o n i n A1-Li a l l o y s u s i n g a s m a l l a n g l e n e u t r o n i n s t r u m e n t . The r e s u l t s were a n a l y z e d f r o m t h e v i e w p o i n t of power l a w o f s c a t t e r i n g f u n c t i o n , t h e s p i n o d a l t h e o r y and t h e dynamic s c a l i n g law.
Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1987342
JOURNAL DE PHYSIQUE
Experimental procedures
The c a s t i n g o t s o f A1-Li a l l o y s c o n t a i n i n g 2.65 mass% (9.5 a t . % ) and 3.24 mass%
(11.4 a t . % ) L i were r e p e a t e d l y h o t r o l l e d and f i n a l l y c o l d r o l l e d t o 2 mm i n t h i c k n e s s . The p l a t e was c u t i n t o s m a l l specimens w i t h t h e s i z e o f 2 x 1 0 x 30 mm f o r t h e s c a t t e r i n g e x p e r i m e n t . These a l l o y s c o n t a i n e d 0.09 mass% Fe, 0.03 mass% S i
,
3 ppm Na, 20 ppm Ca and <1 ppm Na as i m p u r i t i e s . The s c a t t e r i n x p e r i m e n t s were c a r r i e d o u t u s i n g t h e s m a l l a n g l e n e u t r o n s c a t t e r i n g i n s t r u m e n t 1 6 y i n s t a l l e d a t t h e p u l s e d c o l d n e u t r o n s o u r c e a t t h e N a t i o n a l L a b o r a t o r y f o r High Energy Physics (KEK).
The s a m p l e - t o - d e t e c t o r d i s t a n c e was s e l e c t e d t be 1 m f o r t h e e a r l y - t i m e e v o l u t i o n e x p e r i m e n t t o c o v e r t h e q r a n g e o f O..?<q<6 nm-?, 5 m f o r t h e l a t e - t i m e e v o l u t i o n e x p e r i m e n t t o c o v e r 0.06<q<l nm-1. a w i d e range o f wave l e n g t h ( ~ = 0 . 3 % 1 .l nm) o f i n c i d e n t n e u t r o n spectrum was u t i l i z e d t o c o v e r t h e s e wide q ranges. The s c a t t e r i n g d a t a were c o r r e c t e d f o r background, t r a n s m i s s i o n and d e t e c t o r s e n s i t i v i t y as d e s c r i b e d i n e l sewhere(6).
S o l u t i o n t r e a t m e n t was c a r r i e d o u t a t 773 K f o r A1-9.5 a t . % L i a l l o y and a t 823 K f o r A1-11.4 a t . % L i a l l o y i n an a r g o n atmosphere. The specimens were water-quenched and aged a t 423 K i n a n o i l b a t h i n t h e r a n g e o f a g e i n g t i m e between 60 s and 6.06 x 105 s. One measurement was c a r r i e d o u t a t room t e m p e r a t u r e u s i n g 3 o r 4 specimens w h i c h were h e a t t r e a t e d s i m u l t a n e o u s l y . A t s h o r t e r a g e i n g t i m e t h a n 7.2 x 104 s t h e specimens were r e p l a c e d i n an o i l b a t h a t 423 K a f t e r measurements were made, w h i l e a t l o n g e r a g e i n g t i m e t h a n 1.05 x
l o 5
s each specimen was used t o o b t a i n o n l y one datum p o i n t . The a g e i n g t e m p e r a t u r 423 K was s e l e c t e d f r o m t h e f o l l o w i n g reason.A c c o r d i n g t he c a l o r i m e t r i c study?7) and n e u t r o n h i g h - r e s o l u t i o n powder
d i f f r a c t i o n y 8 j on t h e p r e c i p i t a t i o n process i n A l - L i a l l o y s , t h e 6 ' phases a r e m a i n l y formed i n t h e m a t r i x a t 423 K.
R e s u l t s and d i s c u s s i o n
F i g . 1 and F i g . 2 show t h e change o f s c a t t e r i n g i n t e n s i t y a t t h e e a r l y s t a g e o f phase s e p a r a t i o n a t 423 K i n A1-9.5 and 11.4 a t . % i
t
a l l o y s , r e s p e c t i v e l y . Here, t h e i n c r e a s e o f i n t e n s i t y a t s m a l l q r e g i o n (q<0.4 nm- ) i s a t t r i b u t e d t o a s m a l l amount o f l a r g e p r e c i p i t a t e s on g r a i n b o u n d a r i e s . F i g . 3 shows t i m e e v o l u t i o n o f t h e maxi- mum p o s i t i o n qmax and t h e maximum i n t e n s i t y Imax Obtained f r o m t h e r e s u l t s shown i n F i g . 1 and F i g . 2. The q u a l i t a t i v e f e a t u r e s a r e as f o l l o w s : ( 1 ) The maximum p o s i t i o n i n A1-9.5 a t . % L i a l l o y i s s h i f t e d s l o w l y towards s m a l l e r q w i t h a g e i n g t i m e : ( 2 ) The maximum p o s i t i o n i n A1-11.4 a t . % L i a l l o y i s s h i f t e d s l o w l y towards l a r g e r q w i t h a g e i n g t i m e and t a k e s t h e b r o a d maximum; ( 3 ) The maximum i n t e n s i t y i n A1-11.4 a t . % L i a l l o y i s l a r g e r t h a n t h a t i n A1-9.5 a t . % L i a l l o y . I n A1-11.4 a t . % L i a l l o y , a c l e a r peak i s observed even f o r as-quenched s t a t e , i n d i c a t i n g t h a t t h e phase s e p a r a t i o n o c c u r s v r y r a p i d l y ;e
( 4 ) Crossover e f f e c t s p r e d i c t e d by t h e Cahn's s p i n o d a l t h e o r y ( 9 a r e n o t c l e a r l y observed and r a t h e r t h e h i g h q t a i l appears t o merge t o g e t h e r . F i g . 4 shows t h e t y p i c a l r e s u l t s o f t h e l a t e - t i m e e v o l u t i o n o f s c a t t e r i n g i n t e n s i t y , showing t h a t t h e maximum p o s i t i o n and t h e maximum i n t e n s i t y much d i f f e r f r o m t h o s e a t e a r l y stage. F i g . 5 shows t h e Log-Log p l o t o f t h e t i m e e v o l u t i o n o f t h e maximum p o s i t i o n and t h e max~,mum i n t e n s i t y . B o t h parameters obey t h e power law,% x i t ) he a g e i n g t i m e exceeding a b o u t 3.6 x 10 s.
-.
aad I m a x ( t )-
t - a.
I t i s no ed t h a t t h e v a l u e s o f a ' and a " change5
F i g . 6 shows t h e t y p i c a l G u i n i e r p l o t s i n A1-9.5 a t . % L i a l l o y s . F i g . 7 shows t i m e e v o l u t i o n o f G u i n i e r r a d i u s ( R ~ ) p l o t t e d on t h e b a s i s o f t h e t1I3 power l a w . I t i s i n t e r e s t i n g t h a t t h e dependence i s d i v i d e d i n t o two p o r t i o n s .F i g . 8 shows t h e t y p i c a l Log-Log p l o t s o f t h e q dependence o f s c a t t e r i n g i n t e n s i t y a t e a r l y s t a g e i n A1-9.5 a t . % L i a l l o y s . A4 shown i n F i g . 8, t h e s c a t t e r i n g i n t e n s i t y a t h i g h q s i d e obeys t h e f o l l o w i n g e q u a t i o n ,
I ( q ) c q - a ( t ) .
. . . . .. . . . . .. . .
( 11
F i g . 9 shows t h e t i m e e v o l u t i o n o f power a ( t ) i n eq. ( 1 ) a t t h e e a r l y s t a g e o f phase s e p a r a t i o n i n A1-9.5 and 1 1 . 4 a t . % L i a l l o y s . I t i s gound t h a t t h e s c a t t e r i n g f u n c t i o n a r e n o t o n l y p r o p o r t i o n a l t o q-2, q-4 and q- a t h i g h q s i d e o f them, b u t t h e y obey n o n - i n t e g e r fowers o f q. As shown i n F i g . 9, t h e power changes c o n t i n u - o u s l y f r o m q-1.5 o r q- t o q-6 i n v e r y s h o r t t i m e . These v e r y i n t e r e s t i n g r e s u l t s can n o t be now s a t i s f a c t o r i l y e x p l a i n e d by t h e e x i s t i n g t h e o r i e s . The s c a t t e r i n g f u n c t i o n s f o r t h e specimens aged f o r a b o u t 120 s e x h i b i t a q-2 dependence f o r h i g h q values, s u g g e s t i n g t h a t t h e q-2 dependence i s a c h a r a c t e r i s t i c o f t h e e a r l y s t a g e o f phase s e p a r a t i o n . I n t h e A1-11 .4 a t . % L i a l l o y t h e q-2 dependence i s c l e a r l y observed even f o r as-quenched s t a t e , i n d i c a t i n g t h a t t h e e a r l y s t a g e proceeds v e r y r a p i d l y i n con A1-Li a l l o y s . The q-2 dependence o f t h e s c a t t e r i n g f u n c t i o n can be derivedrs0f:TiP9 from t h e k i n e t i c e q u a t i o n o f L a n g e r - B a r - o n - H i l l e r r s
t h e o r y ( 1 2 ) . I t i s found t h a t t h e s c a t t e r i n g f u n c t i o n s i n b o t h a l l o y s aged f o r 600 s obey q-4 dependence, c o r r e s p o n d i n g t o t h e s i t u a t i o n t h a t i n t h i s s t a g e t h e p r e c i p i - t a t e s have d e f i n i t e i n t e r f a c e w i t h t h e m a t r i x . However, t h e q-4 dependence i s r e - p l a c e d by t c a t t e r i n g f u n c t ' w i t h h i g h e r power f o r a g e i n g t i m e t h a n 600 s. I n A1 -Zn a l l o y P P 1
f
and Fe-Cr a l l o y l p 8 ) , q-4 dependence i s observed f o r s u f f i c i e n t l y l o n g p e r i o d , T h e r e f o r e , t h e p r e s e n t r e s u l t seems t o b e unus a l . The s c a t t e r i n g u n c t i o n s o f t h e specimens aged f o r a b o u t 3.6 x 103 s obey t h e q-8 dependence. The q'&dependence o f t h e s c a t t e r i n g f u n c t i o n i s t h o r e t i c a l l y p r e d i c t e d by ~ u r u k a w a ( ~ ) * ( ~ ) , i n d i c a t i n g t h a t c l u s t e r s have i n t r i c a t e s u r f a c e . The e x p ~ ~ ~ ~ e n t a l r e s u l t o f
9-
6 dependence has been r e p o r t e d o n l y i n Fe-34 a t . % Cr a l l o y aged f o r l o n g time a t 773 K. F i g . 1 0 shows t h e t y p i c a l r e s u l t o f Log-Log p l o t o f I ( q ) f o r l a e s t a g e The cI-4 dependence appears a g a i n and t h e s c a t t e r i n g f u n c t ' o n c o n s i s t s o f q-' and q-' dependences. U i t h ageing t i m e t h e c o n t r i b u t i o n o f q-4 dependence i n c r e a s e s , c o r r e s p o n d i n g p r o b a b l y t o t h e s i t u a t i o n t h a t t h e f o r m o f 6 ' phases approaches more s p h e r i c a l . Thus, t h e change o f t h e power l a w o f s c a t t e r i n g f u n c t i o n i n A1-Li a l l o y s i s much more c o m p l i c a t e d t h a n t h o r e t i c a l l y exoected. T h e r e f o r e , t h e more d e t a i l e d i n v e s t i g a t i o n i s necessary.0.8 I I
0
0.7-
Al-9.5 atit.% Li alloy -
0.8 I
40 min I
I
F i g . 1 E a r l y - t i m e e v o l u t i o n of s c a t t e r i n r l F i g . 2 Early-time e v o l u t i o n o f
i n t e n s i t y i n A1-9.5 a t . % L i a l l o p a r l e d s c a t t e r i n q i n t e n s i t y i n A1-11.4 a t . % L i
a t 423 K. a l l o y s aged a t 423 K.
C3-368 JOURNAL DE PHYSIQUE
Fig.. 3 Time e v o l u t i o n o f maximum p o s i t i o n and maximum i n t e n s i t y a t e a r l y s t a g e a t 423 K i n A1-9.5 and 11.4 a t . % L i a l l o y s .
F i g . 4 L a t e - t i m e e v o l u t i o n o f s c a t t e r i n g i n t e n s i t y i n A1-11.4 a t . % L i a l l o y s aged a t 423 K.
As shown i n F i 9, t h e s c a t t e r i n g i n t e n s i t y o f t h e specimens aged f o r 600 s a t 423 K shows t h e q-l'dependence. A c c o r d i n g t o t h e s o - c a l l e d P o r o d ' s law, i f t h e s h a r p i n t e r f a c e i s e s t a b l i s h e d between t h e m a t r i x and p r e c i p i t a t e s , f o r l a r g e v a l u e o f q, t h e p r o d u c t q 4 . 1 ( ~ ) approaches c o n s t a n t , such
l i m q 4 . 1 ( q , t ) = constant:...
Qt" ( 2 )
F i g . 11 shows t h e p l o t s o f q 4 . ~ ( q , t ) versus q4 a t t h e v e r y e a r l y s t a g e o f phase s e p a r a t i o n i n AT-9.5 a t . % L i a l l o y s . W i t h a g e i n g t i m k t h e q 4 . 1 ( q , t ) i n c r e a s e s s t e a d i l y . P o r o d ' s l a w i s s a t i s f i e d a f t e r 600 s . The r e s u l t i n d i c a t e s t h a t t h e i n t e r f a c e between 6 ' phases and m a t r i x i s i n i t i a l l y d i f f u s e
"""",
t 1 " " " I """"I " "[
AI-9.5=tPI0 Li alloy1
AI-9.5 at.'/. Li alloy
F i g . 6 T y p i c a l G u i n i e r p l o t s f o r A1-9.5 a t . % L i a l l o y s aged a t 423 K.
Timels
F i g . 5 Time e v o l u t i o n o f qmax. and Imax i n A1-9.5 a t . % L i a l l o y s aged a t 423 K i n Log-Log p l o t .
F i g . 7 Time e v o l u t i o n o f G i n i e r r a d i u s f o r 1 A1-9.5 a t . % L i a l l o y s i n t Y / 3 p l o t .
n w
-
and sharpens up g r a d u a l l y i n t h e e a r l y cource o f .I phase s e p a r a t i o n t i 1 1 600 s. S i m i l a r r e s u l t s
were obtained f o r t h e A1-11.4 a t . % L i a l l o y s . The r e s u l t i s one o f evidences f o r t h e spinodal decomposition i n A1 - L i a1 l o y s
.
Therefore, we apply the 1 in e a r spinodal t h e o r y ( 9 ) 1 q/nm-I 10
t o our r e s u l t s on t h e very e a r l y stage and
e s t i m a t e t h e i n t e r d i f f u s i o n c o e f f i c i e n t
(8)
a t Fig- O f 423 K i n A1-Li a l l o y . According t o t h e theory, s c a t t e r i n g i n t e n s i t y i n A1-9.5 a t . % t h e time-dependent s c a t t e r i n g i n t e n s i t y has a L i a l l o y s i n Log-Log p l o t .form
I ( q , t ) = I(q,O) exp ( 2 R ( q ) . t ) , . . . - ( 3 )
where I(q,O) i s t h e i n i t i a l s c a t t e r i n g i n t e n s i t y and R(q) i s t h e a m p l i f i c a t i o n fac- t o r g i v e n by
where f " i s t h e second d e r i v a t i v e o f t h e Helmholz f r e e energy o f t h e system p e r u n i t volume. 0 i s t h e f r a c t i o n a l change, ( l / a ) / ( a a / a c), o f t h e l a t t i c e parameter o f t h e s o l i d s o l u t i o n , evaluated a t t h e average composition c
.
K i s t h e energy g r a d i e n t c o e f f i c i e n t . If a l i n e a r spinodal process occurs, t h e aaximum p o s i t i o n qm and t h e crossover p o i n t qc should be i n v a r i a n t w i t h ageing time, having a r e l a t i o n s h i p o f qc/qm = 42. I n t h i s case, a p l o t o f ~ ( q ) / ~ ~ , should be a s t r a i g h t l i n e , w i t h an i n - t e r c e p t , -?f(q) and slope, - ( 2 ~ 8 / f ~ ) . J t h e l i n e a r spinodal the0 y i s a p p l i c a b l e ,f F
i t i s p o s s i b l e t o o b t a i n t h e values of and K, p r o y i d e d f " and
n
Y are known. F i g . 12 shows the l o g a r i t h m o f I ( q ) versus time p l o t t e d f o r d i f f e r e n t q values. It i s noteworthy t h a t a l i n e a r r e l a t i o n s h i p i s observed a t v e r y e a r l y stage. The d e v i a t i o n from t h e l i n e a r i t y occurs a t l o n g e r ageing t i m e than 300 o r 600 s. F i g . 13 shows t h e R(q) versus q p l o t as obtained on t h e b a s i s o f eq. (3) by a least-square method.T h i s curve shows a maximum and extends t o t h e negative value o f R(q), having a v a l u e o f R(q) = 0 a t q = q
.
I t shows t h e c h a r a c t e r i s t i c f e a t u r e s o f spinodal decomposi- tion.The r a t i o q /qmcin t h e present work i s about 2, which excleds t h e value o f 42 p r e d i c t e d by l i n g a r theory. F i g . 14 shows t h e R(q)/q 2 versus q p l o t as obtainedC3-370 JOURNAL DE PHYSIQUE
from F i g . 13.The p l o t c o n s i s t s o f a l i n e a r p 2 r t i o n and,a curved p o r t i o n . I f eq. ( 4 ) i s used f o r t h e l i n e a r o r i o n o f the R(q)/q versus2qk p l o t , t h e value o f -i)(q) 1s equal t o 3.17 x 10-21 m4 i f t h e term o f ( 1
+
( 2 n Y/fl')) i s considered,b
i sn e a r l y equal t o -3 x 0-'I i 2 s - l ; which i s we1 1 c o n s i s t e n t w i t h t h e r e c e n t data
(i)
= 5.0 x 10:21 m2s-I a t 425 K) obtained by e l a s t i c r e c o i l d e t e c t i o n a n a l y s i s (14).Thus, from t h e p r e l i m i n a r y a n a l y s i s we have obtained the experimental evidences t h a t t h e phase separation a t v e r y e a r l y stage i n A l - t i a l l o y s takes p l a c e by the spinodal mechanism. This evidence included: ( a ) a l i n e a r time dependence o f Log I ( q ) , ( b ) t h e occurence o f a negative d i f f u s i o n c o e f f i c i e n t and t h e p l a u s i b l e value o f
B,
( c ) t h e e x i s t e n c e o f t h e d i f f u s e i n t e r f a c e , (d) observation o f t h e c h a r a c t e r i s t i c d5pendeye o f t h e a m p l i f i c a t i o n f a c t o r R(q) on q and ( d ) a l i n e a r dependence o f R(q)/q on q.
However, some d e v i a t i o n s f r o m ' t h e l i n e a r spinodal t h e o r y were observed. Such d e ~ i a - t i o n s from l i n e a r i t y are r e f l e c 3 e d i n the2form o f t h e peak s h i f t o f I ( q ) and t h e c u r v a t u r e i n t h e p l o t o f R(q)/q versus q
.
I n a d d i t i o n , qc/qm r a t i o i s higher than J2. Such a n o n - l i n e a r behavior o f t h e s p i n rocess i L i a110 s must be reex- amined on the s t r i c t t h e o r i e s o f F u r u k a ~ a ( ~ f : 1 ~ 7 , LangerPlfl;nd Cookf15).I n order t o compare t h e s c a t t e r i n g s p e c t r a i n t h e present work w i t h theory, we have c a l c u l a t e d t h e normalized s c a l i n g f u n c t i o n F as f o l l o w ,
5
=
initial stage-
1
-
Al-11.4 at.%Li alloy1
AI-9.5al.%Li alloy. I
Fig. 9 Time e v o l u t i o n of power a ( t ) Fig. 10 Late-time e v o l u t i o n o f s c a t t e r i n g o f eq. (1) f o r A1-9.5 and 11.4 i n t e n s i t y i n A1-9.5 a t . % L i a l l o y s aged a t 423 K at.% L i a l l o y s aged a t 423 K. i n Log-Log p l o t .
Fig. 11 V a r i a t i o n of q o . I ( q , t ) a s a
f u n c t i o n q4 a t t h e v e r y e a r l y s t a g e a t
q lnm-'
423 K i n Al-9.5 a t . % L i a l l o y sF i g . 1 3 A m p l i f i c a t i o n f a c t o r R(q) a s a f u n c t i o n o f q i n A1-9.5 a t . % L i a l l o y s aged a t 423 K.
L
Al -9.5 at.% 4U
alloyj
Fig. 12 Time dependence o f Log I ( q , t )
Fig. 1 4 P l o t o f ~ ( q ) / q Z v e r s u s q 2 f o r i n A1-9.5 a t . % L i a l l o y s aged a t
424 K. A]-9.5 a t . % L i a l l o y s aged a t 423
K.
JOURNAL DE PHYSIQUE
where q l b e i n g t h e f i r s t moment o f t h e s c a t t e r i n g f u n c t i o n , d e f i n e d as
Thus, a p l o t o f F ( q / q l ( t ) ) versus q / q l ( t ) f o r t h e samples aged a t same temperature s h o u l d be independent o f a g e i n g t i m e . F i g . 15 shows t h e t y p i c a l r e s u l t s o f s c a l i n g a n a l y s i s f o r l a t e s t a g e i n A1-9.5 and 1 1 . 4 * a t . % L i a l l o y s . I t i s n o t e d t h a t t h e s c a l i n g l a w h o l d s w e l l and independent o f a e i n g t i m e - a n d L i c o n c e n t r a t i o n . I n t h e case t h e s c a t t e r i n g f u n c t i o n c o n s i s a f ~ ) ~ f q-a and q-6 dependences as shown i n F i g . 10.
A t t h e v e r y e a r l y s t a g e ( ~ ( q ) Q, q-
,
a ( t ! < 4 ) , t h e s c a l i n g l a w does n o t h o l d because o f t h e d i f f u s e i n t e r f a c e . The d e t a i l e d r e s u l t s o f a n a l y s i s w i l l be p u b l i s h e d i n e l sewhere.F i g . 15 S c a l i n g f u n c t i o n F(q/ql ( t ) ) a p p l i e d t o t h e l a t e s t a g e i n A1-9.5 a t . % L i a l l o y s aged a t 423 K.
0 0.5 1 1.5 2 2.5
(14
1Acknowledgements
We a r e g r a t e f u l t o Sumitomo L i g h t M e t a l s I n d . L t d . f o r t h e p r e p a r a t i o n o f specimens.
The p r e s e n t work was supported by G r a n t - i n A i d f o r General Research C (No.62550468) from t h e Japanese M i n i s t r y o f Education, Science and C u l t u r e .
References
( 1 ) F. L i v e t and D. Bloch, S c r i p t a Met.,
19
(1985), 1147.( 2 ) S. Spooner, D. B. W i l l i a m s and C. M. Sung, Aluminum-Lithium A l l o y s 111, The I n s t i t u t e o f Metals, London, 1986, p . 329.
( 3 ) H. Furukawa, Phys. Rev. L e t t . , 43 (1979), 136.
( 4 ) H. Furukawa, Adv. Phys., 34 ( 1 9 W ) , 703.
(5) J. Marro, J. Lebowitz a n d m . Kalos, Phys. Rev. L e t t . ,
43
(1979), 282.( 6 ) Y. Ishikawa, M. Furusaka, N. Niimura, M. A r a i and K. Hasegawa, J. Appl
.
Cryst., 1 9 (1986), 229.( 7 ) Takahashi and T. Sato, J. Japan I n s t . L i g h t M e t a l s ,
36
(1986), 207.( 8 ) M. Furusaka and S. Fujikawa, u n p u b l i s h e d work.
(9) For example, J. E. H i l l i a r d , Phase T r a n s f o r m a t i o n , ASM, 1969, 997.
( 1 0 ) M. Furusaka, Y. Ishikawa, S. Yamaguchi and Y. F u j i n o , J. Phys. Soc. Japan, 55 (1986), 2253.
(11 ) Furusaka, Y. I s h i kawa and M. Mera, Phys. Rev. L e t t . , 17 (1985), 2611
.
(12) J. S . Langer, M. Bar-on and H. D. M i l l e r , Phys. Rev., ~ ~ ( 1 9 7 5 ) , 1417.
(13) S. Katano and M. I i i z u m i , Phys. Rev. L e t t . ,
52
(1984), 835.(14) C. Moreau
,
A. A l l o u c h e and E. J. Knystautas, J. Appl. Phys.,3
(1985), 4582.(15) H. E. Cook, Acta Met.,