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THE STUDY OF LONG RANGE FORCES IN EPITAXY SYSTEMS : THE Ag/Si INTERFACE
J. Shirokoff, K. Hui, U. Erb
To cite this version:
J. Shirokoff, K. Hui, U. Erb. THE STUDY OF LONG RANGE FORCES IN EPITAXY SYS- TEMS : THE Ag/Si INTERFACE. Journal de Physique Colloques, 1988, 49 (C5), pp.C5-165-C5-169.
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supplement a u
THE STUDY OF LONG RANGE FORCES IN EPITAXY SYSTEMS : THE Ag/Si INTERFACE
J. SHIROKOFF, K.C. HUI* and U. ERB
Queen's University, Department
of
Metallurgical Engineering, Kingston K7L 3N6, Canada' ~ u e e n ' s University, Physics Department, Kingston K7L 3N6, Canada
A b s t r a c t
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The Ag/SiO / S i i n t e r f a c i a l system is i n v e s t i g a t e d t o observe o r i e n t a t i o n r e l a t i o n s h i E s of low energy. For t h i s purpose t h e o r i e n t a t i o n d i s t r i b u t i o n of s m a l l s i l v e r p a r t i c l e s on (100) s i l i o n s u b s t r a t e s was measured a f t e r a n n e a l i n g a t 700°C. Three o r i e n t a t i o n r e l a t i o n s h i p s r e s u l t i n g i n i n t e r f a c e s of low energy were observed, r e p r e s e n t i n g cusps i n t h e i n t e r f a c i a l energy v e r s u s m i s o r i e n t a t i o n curve. Two of t h e s e p r e f e r r e d o r i e n t a t i o n s a r e o r i e n t a t i o n s f o r which c l o s e packed and second c l o s e packed p l a n e s of t h e s i l v e r phase a r e p a r a l l e l t o t h e s u r f a c e , w h i l e t h e t h i r d o r i e n t a t i o n i s e p i t a x i a l . The e p i t a x i a l o r i e n t a t i o n was found t o occur even when a n amorphous SiO I n t e r l a y e r of a b o u t 180 s e p a r a t e d t h e Ag p a r t i c l e s from t h e S i s u b s t r a t e . ~ h z i n f l u e n c e of l o n g range o r d e r i n g e f f e c t s a r e d i s c u s s e d .I
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INTRODUCTIONThere i s c o n s i d e r a b l e c o n t r o v e r s y i n t h e l i t e r a t u r e r e g a r d i n g e p i t a x i a l growth and i n f o r m a t i o n t r a n s f e r through amorphous i n t e r l a y e r s i.e. t h e o r i e n t e d growth of i n d i c a t o r f i l m s on s i n g l e c r y s t a l l i n e s u b s t r a t e s when an amorphous i n t e r l a y e r s e p a r a t e s t h e overgrowth and s u b s t r a t e 11-211. E p i t a x y was observed on amorphous i n t e r l a y e r s of carbon, selenium, SiO and polymers f o r v a r i o u s m e t a l l n o n - m e t a l and n o n m e t a l / n o n m e t a l systems 11-8, 12-I$/. These r e s u l t s were e x p l a i n e d i n terms of a c t i v e c e n t r e s on t h e non-metal s u r f a c e , which a r e a s s e m b l i e s of p o i n t d e f e c t s w i t h l o n g range i n f l u e n c e g i v i n g r i s e t o overgrowths w i t h t h e same c r y s t a l l o g r a p h i c o r i e n t a t i o n s a s t h e s u b s t r a t e . S i n c e t h e l o n g range f o r c e s e x e r t o r i e n t i n g i n f l u e n c e o v e r l a r g e d i s t a n c e s (up t o 2000
g),
i t was concluded t h a t t h e y are e l e c t r i c a l l y a c t i v e p o i n t d e f e c t a s s e m b l i e s . The o r i e n t e d c r y s t a l l i z a t i o n through amorphous i n t e r l a y e r s , t h e r e f o r e , s u g g e s t s t h a t n e i t h e r t h e microgeometry of t h e s u r f a c e n o r t h e f i t i n l a t t i c e parameters of t h e s u b s t r a t e and overgrowth a r e of importance f o r e p i t a x y i n s u c h systems. Furthermore, i t h a s been proposed by D i s t l e r and coworkers 16-91 t h a t a c e r t a i n p o l a r i z a t i o n s t r u c t u r e of t h e e l e c t r e t t y p e ( t h e r m o e l e c t r e t f o r amorphous p l a s t i c - p o l y v i n y l c h l o r i d e , and p h o t o e l e c t r e t f o r amorphous s e l e n i u m ) w i t h a n a s s o c i a t e d "memory e f f e c t " i s induced i n i n t e r f a c i a l l a y e r s . These groups"remember" t h e s t r u c t u r a l i n f o r m a t i o n of t h e s u b s t r a t e and t r a n s m i t i t t o t h e overgrowth. T h i s i m p l i e s t h a t c r y s t a l l i z a t i o n can be c o n s i d e r e d a s a m a t r i x r e p l i c a t i o n p r o c e s s , "programmed" by t h e e l e c t r i c a l s t r u c t u r e of t h e s u r f a c e of t h e c r y s t a l s u b s t r a t e s .
However, d e s p i t e D i s t l e r ' s numerous r e s u l t s of e p i t a x i a l growth through amorphous i n t e r l a y e r s , o t h e r r e s e a r c h groups 115-211 were u n s u c c e s s f u l i n t h e i r a t t e m p t s t o reproduce t h e s e f i n d i n g s . The main e x p l a n a t i o n g i v e n t o u n d e r s t a n d t h i s discrepancy p o i n t s towards a porous o r i s l a n d s t r u c t u r e of t h e amorphous i n t e r l a y e r s on Distler's s u b s t r a t e s s o t h a t e p i t a x y might have n u c l e a t e d on b a r e r e g i o n s and t h e n s p r e a d l a t e r a l l y o v e r t h e amorphous i n t e r l a y e r .
The purpose of t h i s s t u d y i s t o t a k e a new approach t o t h e same u n r e s o l v e d problem.
The method used t o s t u d y p o s s i b l e l o n g range e f f e c t s is a m o d i f i c a t i o n of t h e s p h e r e - p l a t e t e c h n i q u e , which a l l o w s t h e d e t e r m i n a t i o n of p r e f e r r e d o r i e n t a t i o n s , i n c l u d i n g e p i t a x i a l o r i e n t a t i o n s f o r a number of d i f f e r e n t systems. The b a s i c assumption i n t h i s t e c h n i q u e i s t h a t a l a r g e number of o r i g i n a l l y randomly o r i e n t e d s i n g l e c r y s t a l s (which i s t h e m a t e r i a l of t h e overgrowth) s i n t e r e d on a s i n g l e c r y s t a l s u b s t r a t e w i l l r o t a t e d u r i n g a n n e a l i n g i n t o o r i e n t a t i o n s c o r r e s p o n d i n g t o low i n t e r f a c i a l e n e r g i e s , t h e d r i v i n g f o r c e being t h e r e d u c t i o n i n t h e i n t e r f a c i a l energy 1221. I n t h e p a s t , t h i s t e c h n i q u e h a s been s u c c e s s f u l l y a p p l i e d t o t h e d e t e c t i o n of
Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1988514
C5-166 JOURNAL DE PHYSIQUE
e p i t a x i a l o r i e n t a t i o n s of m e t a l p a r t i c l e s i n d i r e c t c o n t a c t w i t h v a r i o u s s u b s t r a t e s 123-25/. I n t h e p r e s e n t s t u d y , t h e t e c h n i q u e i s a p p l i e d t o a s y s t e m c o n t a i n i n g a n amorphous i n t e r l a y e r between t h e s i n g l e c r y s t a l l i n e s u b s t r a t e and t h e m e t a l s p h e r e s . I1
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EXPERIMENTALFor t h e s e e x p e r i m e n t s , t h e s p h e r e - p l a t e t e c h n i q u e /25,26/ was m o d i f i e d i n t h e f o l l o w i n g way. The s p h e r e ( p a r t i c l e ) p r e p a r a t i o n was o b t a i n e d by e v a p o r a t i n g t h i n p o l y c r y s t a l l i n e s i l v e r f i l m s d i r e c t l y o n t o t h e s u b s t r a t e m a t e r i a l . These samples were t h e n a n n e a l e d t o form s i n g l e c r y s t a l l i n e s p h e r e s f o r s u b s e q u e n t s p h e r e r o t a t i o n e x p e r i m e n t s /25,26/. I n o r d e r t o s t u d y t h e s p h e r e r o t a t t o n , a u t o m a t i c p o l e f i g u r e r e c o r d i n g was performed by u s i n g t h e Schulz r e f l e c t i o n method and i n t e r f a c i n g t h e x-ray s c i n t i l l a t o r c o u n t e r w i t h a PDP-11 computer. P o l e f i g u r e measurements were t a k e n by changing t h e a n g l e s of r o t a t i o n and i n c l i n a t i o n c o n t i n u o u s l y f o r 6' s p i r a l scans. X-ray i n t e n s i t y s c a n s were a l s o p l o t t e d on a c h a r t r e c o r d e r f o r p a r t i c u l a r a r e a s of i n t e r e s t i n t h e p o l e f i g u r e i n o r d e r t o r e v e a l t h e f i n e s t r u c t u r e of t h e i n t e n s i t y d i s t r i b u t i o n .
The i n t e r f a c i a l s y s t e m chosen f o r t h e work is t h e Ag/SiO / S i system. S i l i c o n p o s s e s s e s a n a t i v e amorphous o x i d e cap (SiOx) of a p p r o x i m a t e f y 20-30
8
/ 2 7 / , which can be removed w i t h e t c h a n t s o r b u i l t - u p by a n n e a l i n g t o e x p l o r e o r i e n t a t i o n r e l a t i o n s h i p s a c r o s s a n i n t e r f a c i a l l a y e r of v a r y i n g t h i c k n e s s . For t h i s work we used s i l i c o n s u b s t r a t e s a s r e c e i v e d ( n a t i v e o x i d e l a y e r 20-30 8 ) and w a f e r s which were pre-annealed a t 850°C i n a i r f o r 45 min. t o build-up a t h i c k o x i d e l a y e r . S i l v e r f i l m s were d e p o s i t e d o n t o b o t h t y p e s of s u b s t r a t e s by vapour d e p o s i t i n g h i g h p u r i t y s i l v e r (99.999%) from a t u n g s t e n b a s k e t , 5 cm from t h e s o u r c e , o n t o m i c r o p o l i s h e d (10-12 m i l s . ) s i l i c o n s u b s t r a t e s (n-type, -5 ohm-cm, o r i e n t e d i n t h e (100) d i r e c t i o n ) i n a vacuum of t h e o r d e r of 1.3 x 1 Pa. The s u b s t r a t e s were r o t a t e d t h r o u g h o u t t h e e v a p o r a t i o n p r o c e s s t o e n s u r e t h e growth of u n i f o r m c o n t i n u o u s t h i n f i l m s . Films r a n g i n g from 0.1 t o 0.15 pm i n t h i c k n e s s werel grown a t room t e m p e r a t u r e (25OC). The r a t e of e v a p o r a t i o n of s i l v e r was 5-108
s-,
and t h e f i l m t h i c k n e s s was measured g r a v i m e t r i c a l l y .The s u b s t r a t e s were c l e a n e d p r i o r t o vapour d e p o s i t i o n and o x i d a t i o n f o l l o w i n g a m o d i f i e d c l e a n i n g p r o c e d u r e (number 7059) of Corning G l a s s Co., Corning, N.Y. The c l e a n i n g p r o c e d u r e c o n s i s t e d of b o i l i n g t h e s u b s t r a t e s i n d i s t i l l e d w a t e r w i t h and w i t h o u t d e t e r g e n t i n a n u l t r a s o n i c b a t h , f o l l o w e d by d e g r e a s i n g i n b o i l i n g a c e t o n e and i t s vapour, t h e n methanol and propanol.
The samples were t h e n a n n e a l e d a t t e m p e r a t u r e s up t o 700°C and up t o 75 min. i n a q u a r t z g l a s s t u b e f u r n a c e u s i n g a n i n e r t d r y N -H atmosphere ( 1 5 v o l . % H ) a t am-
b i e n t p r e s s u r e . 2 2 2
I n a s e p a r a t e s e t of e x p e r i m e n t s which a r e p u b l i s h e d e l s e w h e r e / 2 6 / , e v a p o r a t e d s i l v e r f i l m s were a n n e a l e d on s i l i c a (amorphous S i 0 2 ) s u b s t r a t e s a s a r e f e r e n c e system f o r comparison w i t h t h e s i l i c o n ( c r y s t a l l i n e ) s u b s t r a t e s .
R u t h e r f o r d b a c k s c a t t e r i n g s p e c t r o s c o p y (RBS) of t h e amorphous o x i d e on s i l i c o n was c a r r i e d o u t t o d e t e r m i n e t h e o x i d e l a y e r t h i c k n e s s . T h i s was done u s i n g a 4 MeV Van de G a f f a c c e l e r a t o r p e r a t i n g a t 2 MeV, w i t h helium i o n s a s a s o u r c e , a t a
%a$
p r e s s u r e of 1.3 x 10 Pa i n t h e RBS chamber. The e n e r g y of t h e b a c k s c a t t e r e d i o n s was measured by a s o l i d s t a t e d e t e c t o r f i x e d a t a s c a t t e r i n g a n g l e of 115O a n d a t a d i s t a n c e of 5 cm from t h e sample.
111
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RESULTS AND DISCUSSIONFig. 1 i s t h e A g ( l l 1 ) p o l e f i g u r e of t h e a s e v a p o r a t e d s i l v e r f i l m on s i l i c a t a k e n from a p r e v i o u s s t u d y of t h e A g / s i l i c a i n t e r f a c e /26/. The p o l e f i g u r e e x h i b i t s a n almost random i n t e n s i t y d i s t r i b u t i o n w i t h a s l i g h t i n t e n s i t y i n c r e a s e between 50° and 60°. T h i s i n d i c a t e s a weak p r e f e r r e d o r i e n t a t i o n of s i l v e r g r a i n s w i t h t h e (100) p l a n e s a l i g n e d a l m o s t p a r a l l e l t o t h e s u b s t r a t e ( t h e a n g l e between (100) and (111) i s 54.7O).
The (1119 p o l e f i g u r e of s i l v e r on s i l i c a ( t h e r e f e r e n c e s y s t e m ) a n n e a l e d a t 700°C f o r 75 min. ( t h a t is a f t e r s p h e r e r o t a t i o n i n t o low energy p o s i t i o n s ) c o n s i s t s of t h r e e s t r o n g i n t e n s i t y maxima, a t 0 ° , 54.7O and 70.5O (Fig. 2). These i n t e n s i t y maxima c o r r e s p o n d t o s p h e r e s w i t h (111) p l a n e s p a r a l l e l t o t h e s u b s t r a t e s u r f a c e
54.7', r e f e r r e d t o i n Fig. 2 a s o r i e n t a t i o n B). The c o n s t a n t i n t e n s i t y d i s t r i b u t i o n a l o n g c i r c l e s of c o n s t a n t i n c l i n a t i o n a t 54.7' and 70.5' shows t h a t t h e r e i s no p r e f e r r e d r o t a t i o n a l o r i e n t a t i o n normal t o t h e s u b s t r a t e s u r f a c e . T h e r e f o r e , most of t h e s p h e r e s have r o t a t e d i n t o one of t h e f o l l o w i n g two o r i e n t a t i o n s :
A. A g ( l l 1 )
/ /
s i l i c a s u b s t r a t e B. Ag(100)/ /
s i l i c a s u b s t r a t eFig. 3 shows t h e A g ( l l 1 ) p o l e f i g u r e of t h e a s e v a p o r a t e d s i l v e r f i l m on s i l i c o n which h a s a n a t i v e o x i d e l a y e r . The same weak p r e f e r r e d (100) o r i e n t a t i o n a s o b s e r v e d on s i l i c a i s e v i d e n t .
Annealing t h i s sample a t 650°C f o r 5 min. g i v e s r i s e t o r e c r y s t a l l i z a t i o n of t h e s i l v e r f i l m and break-up of t h e f i l m i n t o p a r t i c l e s . The c o r r e s p o n d i n g p o l e f i g u r e (Fig. 4 ) r e v e a l s t h e same two o r i e n t a t i o n s A and B found i n t h e s i l i c a r e f e r e n c e s y s t e m (Fig. 2 ) a n n e a l e d a t 700°C f o r 75 min.
A f t e r a n n e a l i n g t h e same sample a t 700°C f o r 75 min., t h e t y p i c a l s p h e r e - p l a t e sample i s o b t a i n e d a s shown i n Fig. 5 w i t h s p h e r e s of a b o u t 0.1 t o 1.0 pm i n diameter. The A g ( l l 1 ) p o l e f i g u r e now c o n t a i n s t h e two t e x t u r e components A and B a s w e l l a s a t h i r d new p r e f e r r e d o r i e n t a t i o n C which i s e p i t a x i a l .
E p i t a x y a p p e a r s on t h e A g ( l l 1 ) p o l e f i g u r e (upper h a l f Fig. 6 a ) a s d i s t i n c t i n t e n s i t y maxima r o t a t e d 90' from each o t h e r a l o n g a c i r c l e a t 54.7' from t h e c e n t r e . For r e f e r e n c e p u r p o s e s t h e S i ( l l 1 ) p o l e s a r e shown i n t h e lower h a l f of Fig. 6b.
S i l i c o n s u b s t r a t e s t h a t were pre-annealed a t 850°C i n a i r f o r 45 min. p o s s e s s a b u i l t - u p amorphous o x i d e l a y e r on t h e s u r f a c e . The b a c k s c a t t e r e d y i e l d v e r s u s energy p r o f i l e f o r t h e samples w i t h n a t i v e o x i d e on t h e s u r f a c e and f o r t h e pre-annealed s i l i c o n a r e g i v e n i n Fig. 7. Oxygen and c a r b o n peaks a r e p r e s e n t on t h e s u r f a c e of t h e s i l i c o n . The oxygen y i e l d f o r t h e pre-annealed samples c o r r e s p o n d t o a n o x i d e l a y e r t h i c k n e s s of s 1 8 0
2.
Carbon i s presumably due t o some l o c a l i z e d p i c k - u p from t h e RBS beam l i n e .The A g ( l l 1 ) p o l e f i g u r e of t h e p r e - t r e a t e d s i l i o n s u b s e q u e n t l y a n n e a l e d a t 700°C f o r 75 min. shows t h e same t h r e e i n t e n s i t y maxima which were observed f o r t h e sample c o n t a i n i n g o n l y t h e n a t i v e o x i d e l a y e r , i.e. i n t e n s i t y maxima c o r r e s p o n d i n g t o c l o s e d and second c l o s e d packed p l a n e s p a r a l l e l t o t h e s u r f a c e , and t h e e p i t a x y o r i e n t a t i o n . I n o r d e r t o c l e a r l y show t h e main d i f f e r e n c e i n t h e p o l e f i g u r e s f o r samples c o n t a i n i n g only n a t i v e o x i d e l a y e r s and t h o s e w i t h a b u i l t - u p o x i d e l a y e r , x-ray i n t e n s i t y l i n e s c a n s a r e compared i n Fig. 8. For t h i s purpose, t h e sample i n c l i n a t i o n i n t h e t e x t u r e goniometer was k e p t c o n s t a n t a t 54.7' and t h e d i f f r a c t e d x-ray i n t e n s i t y was r e c o r d e d f o r one f u l l sample r o t a t i o n . Thus t h e f o u r peaks i n t h e l i n e s c a n c o r r e s p o n d t o t h e f o u r p o l e s r e p r e s e n t i n g t h e e p i t a x i a l o r i e n t a t i o n C i n t h e complete p o l e f i g u r e . T h i s comparison shows c l e a r l y t h a t t h e e p i t a x i a l o r i e n t a t i o n C o c c u r s even f o r t h e sample w i t h t h e t h i c k o x i d e l a y e r . The reduced i n t e n s i t y f o r t h e o x i d i z e d sample i s e v i d e n c e t h a t fewer s p h e r e s have r o t a t e d i n t o o r i e n t a t i o n C ( e p i t a x y ) , i n d i c a t i n g t h a t t h e catchment a r e a ( i . e . t h e w i d t h of t h e e n e r g y c u s p ) f o r t h i s o r i e n t a t i o n becomes narrower f o r t h i c k e r o x i d e l a y e r s .
Summarizing o u r r e s u l t s , i t c a n be s t a t e d t h a t f o r t h e i n t e r f a c i a l s y s t e m Ag/SiOx/Si t h e r e e x i s t s t h r e e cusps i n t h e i n t e r f a c i a l energy v e r s u s m i s o r i e n t a t i o n curve. Two of t h e s e a r e i d e n t i c a l t o t h e cusps found f o r t h e Ag/bulk s i l i c a ( S i 0 2 ) s y s t e m 1261.
The t h i r d o r i e n t a t i o n r e l a t i o n s h i p i s t h e Ag/Si e p i t a x y o r i e n t a t i o n which i s p r e s e n t even when a n o x i d e l a y e r of a b o u t 180
a
i n t h i c k n e s s s e p a r a t e s t h e two phases. The a b s e n c e of t h e e p i t a x y o r i e n t a t i o n a f t e r f i l m d e p o s i t i o n and s h o r t a n n e a l i n g t i m e s i n d i c a t e s t h a t t h i s o r i e n t a t i o n i s not due t o d i r e c t Ag/Si c o n t a c t which c o u l d have p o s s i b l y o c c u r r e d i f h o l e s had been p r e s e n t i n t h e o x i d e l a y e r s . Also, t h e examination of o x i d i z e d w a f e r s by means of SEM ( b a c k s c a t t e r e d imaging) d i d n o t show any e v i d e n c e of p o r o s i t y i n t h e o x i d e l a y e r . Thus, we a r e l e d t o conclude t h a t o u r r e s u l t s f u r t h e r s u p p o r t t h e p r e v i o u s f i n d i n g s where e p i t a x i a l o r i e n t a t i o n s e x i s t e d even through amorphous i n t e r l a y e r s . Although i t is s t i l l n o t c l e a r what t h e mechanism f o r infot'mation t r a n s f e r i s , i t a p p e a r s t h a t l o n g r a n g e o r d e r i n g e f f e c t s i n t h i s system e x i s t o v e r d i s t a n c e s of a t l e a s t 1802.
Work i s now i n p r o g r e s s t o measure s p h e r e r o t a t i o n on even t h i c k e r o x i d e i n t e r l a y e r s .C5-168 JOURNAL
DE
PHYSIQUEACKNOWLEDGEMENTS
The f i n a n c i a l s u p p o r t of t h e N a t u r a l S c i e n c e s and E n g i n e e r i n g Research C o u n c i l of Canada and t h e Advisory R e s e a r c h Committee of Queen's U n i v e r s i t y a r e g r e a t f u l l y acknowledged. One of t h e a u t h o r s (J.S.) is t h e r e c i p i e n t of a n O n t a r i o Graduate S c h o l a r s h i p . We would l i k e t o t h a n k J.L. Whitton f o r v a l u a b l e d i s c u s s i o n of t h e RBS r e s u l t s .
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Fig. 1: A g ( l l 1 ) p o l e f i g u r e of t h e a s F i g . 2 : A g ( l l 1 ) p o l e f i g u r e of t h e p a r t i c l e s e v a p o r a t e d overgrowth on s i l i c a . on s i l i c a a n n e a l e d a t 7 0 0 ' ~ f o r 75
min
.
evaporated overgrowth on a n s i l i c o n annealed a t f o r
s i l i c o n . min
.
Fig. 5: Scanning e l e c t r o n micrograph Fig. 6: ~ ~ ( 1 1 1 ) p o l e f i g u r e o f o t h e p a r t i c l e s of s i l v e r p a r t i c l e s on a a f t e r a n n e a l i n g a t 750 C f o r 75 min.
s i l i c o n s u b s t r a t e . ( a ) , and (111) p o l e f i g u r e of t h e s i l i c o n s u b s t r a t e (b)
.
b) 180 A oxide
I
Ia) native oxide
Rotation Angle
>
-
.-
<aEnergy
a) native oxide
Fig. 7 : Backscattered y i e l d v s . energy Fig. 8: A g ( l l 1 ) x - r a y o h t e n s i t y v s . r o t a t i o n f o r t h e n a t i v e o x i d e ( a ) , and a n g l e a t 54.7 i n c l i n a t i o n f o r par- b u i l t - u p o x i d e (b) on s i l i c o n . t i c l e s on t h e n a t i v e o x i d e ( a ) and
t h e b u i l t - u p oxide (b).
