• Aucun résultat trouvé

STUDIES ON EARLY AND LATE STAGES OF FORMATION OF δ' PHASES IN Al-Li ALLOYS BY NEUTRON SMALL ANGLE SCATTERING

N/A
N/A
Protected

Academic year: 2021

Partager "STUDIES ON EARLY AND LATE STAGES OF FORMATION OF δ' PHASES IN Al-Li ALLOYS BY NEUTRON SMALL ANGLE SCATTERING"

Copied!
9
0
0

Texte intégral

(1)

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�

(2)

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. HIRANO

Tohoku

University, Department

o f

Materials Science, J-Sendai 980, Japan

" ~ o h o k u

University, Physics Department, J-Sendai 980, Japan

A 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 e

ii

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 e

e 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

(3)

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 " change

5

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 ) .

. . . . .. . . . . .. . .

( 1

1

(4)

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.

(5)

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 alloy

1

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 .

(6)

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 obtained

(7)

C3-370 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 s

n 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 alloy

1

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 .

(8)

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 s

F 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.% 4

U

alloy

j

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.

(9)

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

1

Acknowledgements

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.,

18

( 1 970), 297.

Références

Documents relatifs

Es una tecnología adecuada para la cloración del agua en los sistemas de agua potable, consta de un tanque (250 a 750 L) que contiene el preparado de hipoclorito de

contribution of the spin misalignment to the total magnetic SANS cross section via the study of the individual magnetization Fourier components; it provides important

The typical space scale for small angle neutron scattering (SANS) ranges from nm to 03BCm, whereas with neutron diffraction the pm to nm range is reached.. In

Absolute intensity measurements, and fits of the full scattering curves using models, suggest that these objects are chiral, possibly symmetrical double helices of

LOW CYCLE FATIGUE OF BINARY Al-Li ALLOYS : III-COALESCENCE OF δ’ PRECIPITATES IN FATIGUE : X-RAY LOW ANGLE

To test whether the vesicular pool of Atat1 promotes the acetyl- ation of -tubulin in MTs, we isolated subcellular fractions from newborn mouse cortices and then assessed

Néanmoins, la dualité des acides (Lewis et Bronsted) est un système dispendieux, dont le recyclage est une opération complexe et par conséquent difficilement applicable à

Cette étude se veut transversale dans la mesure où, quand bien même l’alimentation est ici entrevue principalement sous l’angle de la géographie avec l’étude de la trajectoire