JOURNAL, DE PHYSIQUE Colloque C 8 , supplement au n l l , Tome t5, novembre 1984 page C8-117

DIAMOND ANVIL CELL = SHOCK WAVE GUN ? M. Madon, J . Peyronneau and J . P . Institut Jussieu, de Physique 75230 Paris Poirier Pierre et Marie Curie, 4, Place

du Globe, University Cedex OS, France

Rsin - L ' o b s e r v a t i o n en microscopie l e c t r o n i q u e par transmission d ' o l i v i n e (Mg jFe^SiO,, dforme dans une c e l l u l e enclumes de diamant chauffe par laser montre que cet appareillage cre des c o n d i t i o n s de dformation semblables c e l l e s produites par des ondes de choc. Abstract Transmission electron microscope observations of olivine (MgjFe^SiO,, deformed i n a laser-heated diamond-anvil high pressure c e l l reveal that t h i s device creates deformation c o n d i t i o n s s i m i l a r to those produced by shock waves. The a ( o l i v i n e ) , ( ( " m o d i f i e d " s p i n e l ) and y ( s p i n e l ) polymorphs of a composi3 t i o n close to the magnesian end of (MgjFe^SiGV are e s s e n t i a l minerals of the E a r t h ' s upper mantle [ 1 , 2 ] , p e r o v s k i t e (Mg,Fe)Si0 3 and magnesiowustite (Mg,Fe)0 probably being major c o n s t i t u e n t s of the lower mantle [ 3 , 4 ] . The phase t r a n s i t i o n s between these minerals are the object o f sustained i n t e r e s t [ 5 , 6 ] and one of the most promising l i n e s o f i n v e s t i g a t i o n consists i n using transmission e l e c t r o n microscopy (TEM) and e l e c t r o n d i f f r a c t i o n analysis to examine high pressure phases synthesized i n the l a b o r a t o r y [ 7 , 8 ] or r e s u l t i n g from n a t u r a l processes [ 9 , 1 0 ] . In t h i s paper, we present the r e s u l t s of TEM observations of o l i v i n e brought to pressures between 50 and 70 GPa and temperatures between 1000 and 2000 C in a laser-heated diamond-anvil c e l l .
1 - SAMPLES

The s t a r t i n g m a t e r i a l was n a t u r a l San Carlos o l i v i n e (Mg 0 _ 8 8 , F e 0 _ 1 2 ) 2 s i 0 1 ( w i t h 0.5 % of f i n e l y powdered carbon to f a c i l i t a t e absorption of the laser beam. The powdered mixture was imbedded i n the hole (250 \m diameter) o f a s t a i n l e s s s t e e l gasket (200 \im t h i c k ) and the sample was brought to pressures between 50 and 70 GPa. Pressures were measured by the s t r a i n gauge technique described by Peyronneau 4 a l . i n t h i s j o u r n a l . The samples were then raised to temperatures between approximately 1000 C (estimated from the brightness of the sample) and 2000 C (estimated using the m e l t i n g point of o l i v i n e under pressure) by scanning across the sample a l a s e r beam focused on a 30 pm diameter s p o t . The quench products were glued on copper g r i d s and ion-beam t h i n n e d . The t h i n edges of the holes were then examined i n a P h i l i p s E 300 e l e c t r o n microscope at 100 Kev and i n a Jeol 2000 EX at 200 Kev. M
2 - TEM OBSERVATIONS

Whatever the pressure applied on the samples, only two types of textures are observed according to the temperature o f the experiment: i ) The f i r s t type of texture i s obtained at "low" temperature (T1000 C) and c o n s i s t s i n amorphous zones w i t h i n c r y s t a l l i n e regions o f f i n e l y sheared o l i v i n e ( F i g . 1 ) . The d i f f r a c t i o n p a t t e r n corresponding to c r y s t a l l i n e regions i s the same a l l over the sample and shows the o l i v i n e p a t t e r n w i t h a second p a t t e r n superimposed on i t t h a t was indexed according to the s p i n e l s t r u c t u r e ( F i g . 1 - a ) . The o r i e n t a t i o n r e l a t i o n s h i p Jjetween the two patterns - ( 1 0 0 ) o l p a r a l l e l to (111)sp and 00l]ol p a r a l l e l t o [ l 1 0 ] s p ( F i g . 1 - b ) - i s compatible w i t h a model r e c e n t l y proposed [10,11 ] of an o l i v i n e - s p i n e l shear t r a n s i t i o n e f f e c t e d by the motion o f p a r t i a l d i s l o c a t i o n s

Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1984823

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F i g . 1.-a) D i f f r a c t i o n p a t t e r n o f c r y s t a l l i n e r e g i o n s showing t h e p r e s e n c e o f t w o s t r u c t u r e s : o l i v i n e and s p i n e l . -b) O r i e n t a t i o n r e l a t i o n s h i p between t h e two s t r u c t u r e s . - c ) and -d) TEM images showing g l a s s y z o n e s ( g ) between c r y s t a l l i n e r e g i o n s . on t h e c l o s e packed p l a n e s o f two s t r u c t u r e s . The o r i e n t a t i o n r e l a t i o n s h i p between E t h e two p h a s e s is n o t v i s i b l e on T M images ( F i g . 1 - c and d ) but we c a n s u p p o s e t h a t t h e two p h a s e s a r e v e r y f i n e l y i n t e r c a l a t e d and produce t h i s s h e a r e d s t r u c t u r e . The amorphous z o n e s a r e s e e n between c r y s t a l l i n e r e g i o n s a s p a t c h e s w i t h b l u r r e d o r f i n e l a n e l l a e along c r y s t a l l o g r a p h i c planes o f t h e host o u t l i n e s (Fig.1-c) c r y s t a l (Fig.1-d) . T h e s a n e t e x t u r e of amorphous z o n e s w i t h i n c r y s t a l l i n e r e g i o n s o f f i n e l y s h e a r e d o l i v i n e ( F i g . 1 - c ) h a s been o b s e r v e d i n o l i v i n e deformed by s h o c k waves a t 56 GPa [12]. I f we u s e t h e c a l c u l a t i o n o f shock t e m p e r a t u r e s measured i n s h o c k e d s i n g l e - c r y s t a l Mg2Si04 [ 1 3 ] , we o b t a i n a t e m p e r a t u r e o f 1000 O C a t 56 GPa, a s i n o u r experiments. i i ) The second t y p e o f t e x t u r e is o b t a i n e d a t h i g h t e m p e r a t u r e (T=2000 OC) a f t e r o l i v i n e b r e a k s down t o an a s s e m b l a g e o f ( 4 , F e ) O p l u s (Mg,Fe)5i03 g l a s s ( F i g . 2 ) . The e l e c t r o n d i f f r a c t i o n p a t t e r n s a l l o w t h e i d e n t i f i c a t i o n o f c r y s t a l l i n e p h a s e r n a g n e s i o w i j s t i t e (Mg,Fe)O and show t h e p r e s e n c e o f a n o r p h o u s z o n e s ( h a l o i n d i f f r a c t i o n p a t t e r n s ) e x p e c t e d t o be (Wj,Fe)SiO, g l a s s ( F i g . 2 - a ) . T M images show E t h e h e t e r o g e n e o u s t e x t u r e of c r y s t a l s and g l a s s : t h e (Mg,Fe)O c r y s t a l s a r e e l o n g a t e d (Fig.2-b) o r more o r less m i c r o c r y s t a l l i n e (Fig.2-c and d) w h e r e a s g l a s s y z o n e s In s i t u X-ray appear a s snooth a r e a s (Fig.2-b) o r polygonal "grains1' (Fig.2-d). m i c r o a n a l y s i s c o n f i r m s t h a t g l a s s h a s t h e c a n p o s i t i o n (Mg;Fe)Si03 and t h a t i r o n d i s p r o p o r t i o n a t e s between (Ng ,Fe)O and (Mg , F e ) S i Q 3 , g o i n g p r e f e r e n t i a l l y t o magnesiowiistite:

T h i s s t r o n g Fe-% a r t i t i o n i n g between t h e two p h a s e s h a s a l r e a d y been o b s e r v e d by X-ray d i f f r a c t i o n { 1 4 ] .

Fig. 2.-a) Electron d i f f r a c t i o n p a t t e r n o f magnesiowustite.-b), - c ) and -d) images showing d i f f e r e n t t e x t u r e s o f c r y s t a l s (Mq ,Fe)O a d g l a s s (Mg , F e ) S i 0 3 .

TEM

The t e x t u r e c o n s i s t i n g of ( b , F e ) O c r y s t a l s and ( b , F e ) S i 0 3 g l a s s h a s a l s o b e e n o b s e r v e d i n o l i v i n e deformed by shock waves between 78 and 92 GPa [ 1 5 ] . For t h e s e p r e s s u r e s , t h e c a l c u l a t i o n [ 1 3 ] g i v e s a t e m p e r a t u r e between 1800 a d 2200 O C compatible with our experimental conditions.
3

DISCUSSION

The e x p e r i m e n t a l o b s e r v a t i o n s r a i s e s e v e r a l problems t h a t we w i l l now d i s c u s s . i ) I n "low" t e m p e r a t u r e e x p e r i m e n t s between 50 and 70 GPa, i . e . i n t h e e s t a b i l i t y f i e l d o f p e r o v s k i t e and r n a g n e s i o w i i s t i t e , w o b s e r v e t h e l e s s s t a b l e y - s p i n e l . Now, o l i v i n e can t r a n s f o r m t o y - s p i n e l by a s h e a r o f t h e oxygen s u b l a t t i c e and a s h u f f l i n g o f t h e c a t i o n s [ l l ] , a mechanism t h a t d o e s n o t demand h i g h t e m p e r a t u r e s and can b e h e l p e d by s h e a r s t r e s s e s ; t h e t r a n s f o r m a t i o n o f y - s p i n e l t o p e r o v s k i t e and m a g n e s i o w i i s t i t e , on t h e o t h e r hand, p r e s u n a b l y i n v o l v e s d i f f u s i o n , h e n c e c a n o t t a k e p l a c e i f t h e t e m p e r a t u r e is n o t h i g h enough. A t h i g h p r e s s u r e s and low t e m p e r a t u r e s , o l i v i n e might t h e r e f o r e t r a n s f o r m i n t o y - s p i n e l , a more s t a b l e , a l t h o u g h n o t t h e most s t a b l e p h a s e , b e c a u s e t h e e n e r g y b a r r i e r is much lower t h a n f o r t r a n s f o r m i n g t o p e r o v s k i t e and m a g n e s i o w u s t i t e . I n o u r e x p e r i m e n t s , as well a s i n shock waves e x p e r i m e n t s [ 1 2 ] , g l a s s was l o c a l l y o b s e r v e d . T h e r e is a p o s s i b i l i t y t h a t h i g h l y deformed o l i v l n e m i g h t l o c a l l y t r a n s f o r m t o g l a s s , p e r h a p s b e c a u s e a v e r y h i g h d i s l o c a t i o n d e n s i t y makes t h e t r a n s f o r m a t i o n t o g l a s s k i n e t i c a l l y e a s i e r t h m t h e transformation to spinel. i i ) I n "high" t e m p e r a t u r e e x p e r i m e n t s , i r o n - r i c h m a g n e s i o w u s t i t e is found a s e x p e c t e d but t h e (Mg,Fe)Si03 p h a s e is a g l a s s i n s t e a d o f t h e e x p e c t e d c r y s t a l s w i t h p e r o v s k i t e s t r u c t u r e . The swe o c c u r r e n c e h a s been o b s e r v e d i n s w p l e s r e c o v e r e d from shock wave e x p e r i m e n t s [ 1 5 ] b u t a l s o i n s t a t i c e x p e r i m e n t s on CaSi03 [ 1 6 , 1 7 ] where a p e r o v s k i t e - s t r u c t u r e p h a s e h a s been i d e n t i f i e d i n - s i t u a t h i g h p r e s s u r e , a l t h o u g h t h e r e c o v e r e d s a m p l e s were g l a s s y , presumably d u e t o a r e t r o g r e s s i v e

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t r a n s f o r m a t i o n d u r i n g the r e l e a s e o f pressure. W have n o t been able so f a r t o e a s c e r t a i n whether t h e (Mg ,Fe)SiOg phase i n our experiments i s c r y s t a l l i n e under h i g h pressure, nor i s i t obviously p o s s i b l e t o know whether i t i s the case f o r recovered shock sanples. Two hypothesis may t h e r e f o r e be considered (both f o r t h e dianond a n v i l and the shock wave experiments): -a) The o l i v i n e i s f i r s t taken t o h i g h pressures, w e l l i n t o the s t a b i l i t y f i e l d o f perovs k i t e , b e f o r e being heated. There i s t h e r e f o r e 1bbq1a considerable anount o f energy s t o r e d i n the h,so. system, o f t h e order o f l o 5 J / mole (Fig.3). T.~SOO'< When t h e l a s e r bean h i t s the sample ( o r &en t h e temperature wave heats i t i n shock experiment) ,the temperature makes the t r a n s f o r m a t i o n . p o s s i b l e and the energy i s suddenly released, much i n the way chemical energy i s released by t h e explosion o f a s t i c k o f dynanite.The c r y s t a l l i n e l a t t i c e c o u l d be so much disorganized .t h a t a d i a p l e c t i c g l a s s could be formed. This scenario may perhaps be envisaged .i n cases where the systen i s brought very f a r from the Clapeyron a t low temperature. I t may, however, be simpler t o consider Fig.3.Free energy d r i v i n g t h e -b) t h a t the h i g h pressure phase was c r y s t a l l i n e , transformation o f olivine into i t s h i g h pressures phases versus as i t has been shorn t o be t h e case i n a few instances[14,16]. The pressure release usualpressure ( a f t e r data o f [18,191) l y t a k i n g place a t low temperatures, t h e h i g h pressure phase can be conserved and the d r i v i n g force f o r t r a n s f o r m a t i o n t o the low pressure phase b u i l d s up and e v e n t u a l l y reaches such a h i g h value t h a t the t r a n s f o r m a t i o n takes p l a c e i n a v i o l e n t manner; i f the t r a n s f o r m a t i o n i n v o l v e s d i f f u s i o n , i t i s conceivable t h a t t h e system f i n d s i t easier t o d i s o r g a n i z e completely i n t o a g l a s s a t temperatures too low t o a l l o w the o r d e r l y t r a n s f o r m a t i o n t o the low pressure c r y s t a l l i n e phase. Whatever the a c t u a l mechanism f o r the formation o f glass, t h e r e i s a s t r i k i n g s i m i l a r i t y between the TEM m i c r o s t r u c t u r e s o f s w p l e s o f o l i v i n e recovered frun h i g h pressure runs i n dianond a n v i l c e l l s and from shock experiments [12,15]. This suggests t h a t t h e d i a n o d a n v i l c e l l provides experimental c o n d i t i o n s t h a t , d e s p i t e appearances, are much c l o s e r t o the c o n d i t i o n s obtained i n shock experiments and i n shocked m e t e o r i t e s [ l o ] than t o s t a t i c c o n d i t i o n s . I.P.G. c o n t r i b u t i o n N '774

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