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HAL Id: jpa-00223976

https://hal.archives-ouvertes.fr/jpa-00223976

Submitted on 1 Jan 1984

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.

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1 keV X-RAY ABSORPTION SPECTROSCOPY OF BULK MATERIALS BY ELECTRON YIELD

MEASUREMENT

J. Esteva, R. Karnatak

To cite this version:

J. Esteva, R. Karnatak. 1 keV X-RAY ABSORPTION SPECTROSCOPY OF BULK MATERIALS BY ELECTRON YIELD MEASUREMENT. Journal de Physique Colloques, 1984, 45 (C2), pp.C2- 279-C2-280. �10.1051/jphyscol:1984262�. �jpa-00223976�

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JOURNAL DE PHYSIQUE

Colloque C2, suppl6ment au n02, Tome 45, fkvrier 1984 page C2-279

1 kev X-RAY ABSORPTION SPECTROSCOPY OF BULK MATERIALS BY ELECTRON

Y I E L D MEASUREMENT

J.M. Esteva and R.C. Karnatak

L.U.R.E., B&. 209 C, 91405 Orsay Cedex, France

and E.R.A. 719, B&. 350, U n i v e r s i t S Paris-Sud, 91405 Orsay Cedex, France

Resume L On p r e s e n t e une c o m p a r a i s o n d e s s p e c t r e s o b t e n u s d a n s m i o n d e 1 keV p a r r e n d e m e n t p h o t o e l e c t r i q u e ( " y i e l d " ) e t

des s p e c t r e s d ' a b s o r p t i o n c o r r e s p o n d a n t s o b t e n u s p a r m e s u r e d e t r a n s m i s s i o n . On d i s c u t e l e s a v a n t a g e s d e l a m @ t h o d e d u " y i e l d "

e t l e s p o s s i b i l i t e s d ' a p p l i c a t i o n a u x e t u d e s de m a t e r i a u x . A b s t r a c t - A c o m p a r a t i v e s t u d y o f e l e c t r o n y i e l d a n d t h e c o r r e s - p o n d i n g a b s o r p t i o n s p e c t r a i n t h e 1 keV r e g i o n o b t a i n e d b y t r a n s m i s s i o n m e t h o d i s p r e s e n t e d . A d v a n t a g e s o f y i e l d s p e c t r a a r e d i s c u s s e d a n d t h e i r p o s s i b l e a p p l i c a t i o n t o m a t e r i a l r e - s e a r c h i s i n d i c a t e d .

The a p p l i c a t i o n o f X - r a y s p e c t r o s c o p i c m e t h o d s t o t h e s t u d y o f e l e c t r o - n i c p r o p e r t i e s o f m a t e r i a l s h a s s u b s t a n t i a l l y c o n t r i b u t e d t o e l u c i d a t e t h e i r e l e c t r o n i c s t r u c t u r e . The i n n e r s h e l l a b s o r p t i o n s p e c t r o s c o p y h a s p r o v e d t o b e an e f f i c i e n t p r o b e t o u n d e r s t a n d t h e e f f e c t o f l o c a l i s e d e l e c t r o n s , c r y s t a l f i e l d s , a n d h y b r i d i z a t i o n o n t h e g r o u n d s t a t e p r o - p e r t i e s o f c e r t a i n m a t e r i a l s . T h i s i s due t o t h e f a c t t h a t t h e f i n a l a c c e s s i b l e s t a t e s i n a b s o r p t i o n t r a n s i t i o n s a r e s e p a r a t e d b y s e v e r a l eV a n d t h e d i p o l e s e l e c t i o n r u l e s r e m a i n s t i l l v a l i d . I n t h e 1 keV r a n g e ( 8 0 0 - 2 0 0 0 e V ) ( 1 ) t h e p h o t o e l e c t r i c y i e l d m e a s u r e m e n t s w i t h h i g h r e s o - l u t i o n m o n o c h r o m a t o r a s s o c i a t e d w i t h s y n c h r o t r o n r a d i a t i o n h a s become a p o w e r f u l m e t h o d ( 2 ) t o o b t a i n a b s o r p t i o n s p e c t r a o f c e r t a i n m a t e r i a l s f o r t h e s t u d y o f a t o m i c s o l i d s t a t e e f f e c t s ( 3 - 4 ) .

I n u s u a l X - r a y a b s o r p t i o n e x p e r i m e n t s , t h e l i n e a r a b s o r p t i o n c o e f f i - c i e n t & i s o b t a i n e d b y m e a s u r i n g t h e i n c i d e n t ( 1 0 ) a n d t h e t r a n s m i t t e d ( I ) i n t e n s i t i e s t h r o u g h a s a m p l e o f t h i c k n e s s X b y t h e e x p r e s s i o n I = 10 e - p X . Among v a r i o u s t y p e s o f i n t e r a c t i o n s i n v o l v e d i n t h e a b - s o r p t i o n p r o c e s s , t h e i n n e r - s h e 1 l e x c i t a t i o n h a s a p r o m i n e n t c o n t r i b u - t i o n t o w a r d s t h e s e c o n d a r y e l e c t r o n e m i s s i o n . The g e n e r a l t h e o r y r e l a - t e d t o t h e m i g r a t i o n o f e l e c t r o n s t o t h e s u r f a c e i n s o l i d s i s c o m p l e x . I n a s i m p l i f i e d a p p r o a c h , f o r b u l k s a m p l e s , t h e t o t a l e l e c t r o n y i e l d i s d e f i n e d as t o ' b e p r o p o r t i o n n a l t o t h e f r a c t i o n o f t h e i n c i d e n t beam i n t e n s i t y I a b s o r b e d i n t h e s a m p l e . Thus i n y i e l d p r o c e s s , Y = I o - I

7-5-

w h e r e I i s t h e beam i n t e n s i t y a t a d e p t h L c o r r e s p o n d i n g t o t h e e f f e c - t i v e l i m i t f o r t h e e l e c t r o n s c a p a b l e o f m i g r a t i n g t o t h e s u r f a c a n d d e t e c t e d ; L i s c a l l e d t h e s a m p l i n g d e p t h . By p u t t i n g I = 10 e - ~ ' , i t

c a n e a s i l y be 3 h o w n l t h a t Y = ( 1 - e-NL). I n 1 keV r e g i o n , f o r m o s t ma- t e r i a l s , f i * l O cm- a n d L v 5 0 8 . T h i s i m p l i e s , u L e l . U n d e r t h i s c o n d i - t i o n Y

=rfiL

w h e r e i s a m u l t i p l i c a t i o n f a c t o r d e s c r i b i n g t h e number o f e l e c t r o n s o r i g i n a t i n g f r o m t h e a b s o r b e d p h o t o n . Thus y i e l d s p e c t r u m s h o u l d m i m i c t h e c o r r e s p o n d i n g a b s o r p t i o n s p e c t r u m o b t a i n e d b y t r a n s - m i s s i o n m e t h o d . I n t h e e x p e r i m e n t a l s e t u p , t h e s y n c h r o t r o n beam mono- c h r o m a t i z e d b y a d o u b l e c r y s t a l m o n o c h r o m a t o r i m p i g e s on t h e s a m p l e Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1984262

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C2-280 JOURNAL DE PHYSIQUE

p l a c e d a t an a n g l e of 25" and t h e e m e r g i n g e l e c t r o n s a r e d e t e c t e d a s a f u n c t i o n of i n c i d e n t e n e r g y . The d e t e c t o r i s a c h a n n e l t r o n p r o v i d e d w i t h two a c c e l e r a t i n g g r i d s . The d e t a i l s of t h i s e x p e r i m e n t a r e g i v e n e l s e w h e r e ( 2 ) .

C o n t r a r y t o u s u a l X-ray a b s o r p t i o n t e c h n i q u e which r e q u i r e s t h i n sam- p l e s , t h i s method o f f e r s wide p o s s i b i l i t i e s of d e a l i n g w i t h b u l k m a t e - r i a l s . S i n c e t h e s a m p l i n g d e p t h i n t h e y i e l d method i s s m a l l t h e s u r - f a c e d e p e n d a n t s t u d i e s of m a t e r i a l s r e q u i r e U H V t e c h n i q u e s . Samples c a n b e t r e a t e d m e c h a n i c a l l y o r t h e r m a l l y u n d e r U H V c o n d i t i o n s . As an exemple we show i n t h e f i g u r e 1 t h e h i g h r e s o l u t i o n ( b a n d b 0 , 3 eV) 2p y i e l d s p e c t r u m from a m e c h a n i c a l l y s c r a p e d c o p p e r p l a t e u n d e r U H V .

A n o t h e r i n t e r e s t i n g example i s t h e c a s e of t h e 3p e d g e s o f La. In f i - g u r e 2, we show t h e 3p3,2 d i s c o n t i n u i t y of m e t a l l i c La o b t a i n e d by s c r a p i n g i n s i t u i n U H V , With t r n s m i s s i o n m e t h o d , s u c h e d g e r e q u i r e s a f i l m t h i c k n e s s o f a b o u t 3 0 0 0

1

and l o n g e x p o s u r e ( 2 h o u r s ) . More- o v e r , t h e d e s i r e d q u a l i t y o f t h e s p e c t r a a s a f u n c t i o n of t h e f i l m t h i c k n e s s r e q u i r e s s e v e r a l e x p e r i m e n t s . The 3p3,? s p e c t r u m of La was o b t a i n e d w i t h 0 , 3 eV s t e p s and an accumulating-;;me o f 4 s e c .

The a b s o r p t i o n s p e c t r a from e l e m e n t s i n s i n g l e c r y s t a l s i s e a s i l y ob- t a i n e d by y i e l d m e t h o d , a f t e r c l e a v i m g i n U H V c o n d i t i o n s . Such e x p e - r i m e n t s on NaCl and SmS a r e i n p r o g r e s s . P r e l i m i n a r y e x p e r i m e n t s on t h e e f f e c t of beam p o l a r i s a t i o n on t h e a b s o r p t i o n s p e c t r a from s i n g l e c r y s t a l a r e e n c o u r a g i n g . They a r e e x p e c t e d t o g i v e u s e f u l i n f o r m a t i o n on t h e c r y s t a l f i e l d e f f e c t i n r a r e e a r t h and t r a n s i t i o n e l e m e n t s .

CU 2p TOTAL YIELD

. . .

La 3p TOTAL YIELD

F i g u r e 1 F i g u r e 2

REFERENCES

( 1 ) M . LEMONNIER e t a l .

Nucl. 1 n s t r u m . M e t h o d s 1 5 2 , 109 ( 1 9 7 8 ) ( 2 ) J.M. ESTEVA e t a l .

J . E l e c t r . S m Re1

.

Phenom. 31, 1 ( 1 9 8 3 ) ( 3 ) J.M. ESTEVA e t a l .

Phys. Rev. L e t t . 2 , 910 ( 1 9 8 3 ) ( 4 ) J . C . F U G G L E e t a l .

Phys. Rev. K T 4 6 3 7 ( 1 9 8 3 )

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