H i g h q u a l i t y , e l e c t r o n t r a n s p a r e n t specimens o f m e t a l / o x i d e cross s e c t i o n s a r e necessary t o p e r f o r m some of t h e more s o p h i s t i c a t e d s t u d i e s i n v o l v i n g TEM and STEM a p p l i c a t i o n s . d u r a b l e specimens i n a simple and c o n s i s t e n t f a s h i o n . T h i s communication d e s c r i b e s a t e c h n i q u e t h a t can be used t o p r e p a r e specimens o f m e t a l i o x i d e c r o s s s e c t i o n s i n a 3 mm diameter mount.The a l l o y of i n t e r e s t i s c u t i n t o b a r s a p p r o x i m a t e l y 1.5 mm by 0.75 mm by 10 mm. Only one of t h e l a r g e f a c e s need be prepared f o r o x i d a t i o n t r e a t m e n t s . The b a r s a r e o x i d i z e d under t h e a p p r o p r i a t e e x p e r i m e n t a l c o n d i t i o n s . Next, a t h i n c o a t of s i l v e r p a i n t i s a p p l i e d t o t h e d e s i r e d o x i d i z e d s u r f a c e o f each b a r ( F i g . 1 ) . The p a i n t e d surfaces a r e p l a c e d and h e l d t o g e t h e r u n t i l t h e p a i n t d r i e s . The r e s u l t i n g j o i n t has s u f f i c i e n t s t r e n g t h f o r s u i t a b l e h a n d l i n g o f t h e specimen b a r sandwich.
The sandwich i s then p l a c e d i n a s p e c i a l l y designed s t a i n l e s s s t e e l mold and c e n t e r e d w i t h set-screw p i n s ( F i g . 2 ) . The purpose o f t h e mold d e s i g n i s t o h o l d t h e sandwich i n p l a c e i n s i d e a 3 mm diameter bore i n t o which a m o l t e n a l l o y i s i n j e c t e d . F o l l o w i n g a l i g n i n g o f t h e sandwich i n t h e mold, a p i e c e ofa Zn-4 a t % A l -1 a t % Cu a l l o y i s p l a c e d i n t h e r i s e r p o r t i o n o f t h e mold. T h i s a l l o y was chosen because o f i t s low m e l t i n g temperature (415 " C ) , s u f f i c i e n t s t r e n g t h and h i g h thermal expansion c o e f f i c i e n t which r e s u l t s i n a compressive s t r e s s on t h e specimen sandwich h e l p i n g t o h o l d t h e two h a l v e s t o g e t h e r . The e n t i r e mold i s heated q u i c k l y w i t h an o x y -a c e t y l i n e t o r c h u n t i l t h e a l l o y i s m o l t e n . A g l a s s tube connected t o a r u b b e r b u l b i s p l a c e , 1983; Newcomb and Stobbs, 1985; S a w h i l l and Hobbs, 1984; Bennett, D e s p o r t and Labun, 1987). The use o f epoxy r e s i n s ( K i n g , Peterson and Reddy, 1984) i s e l i m i n a t e d so t h a t o r g a n i c s o l v e n t s can be used t o c l e a n t h e specimens. Two d i f f e r e n t e x p e r i m e n t a l c o n d i t i o n s can be i n c o r p o r a t e d i n t o one specimen.
d over t h e r i s e r and i n c o n t a c t w i t h t h e mold. A b l a s t o f a i r causes t h e m o l t e n a l l o y t o flow around and encapsulate t h e specimen b a r sandwich. The i n j e c t i o n process i s necessary t o c o u n t e r s u r f a c e t e n s i o n e f f e c t s o f t h e m o l t e n a l l o y d r o p l e t . 4 f t e r...