Mechanical Stability of DLC Films on Metallic Substrates

8/13/2019 Mechanical Stability of DLC Films on Metallic Substrates

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D L C o a t j l l g s I i a v hee l l depo s i ted on to fou r m eta l l i c suh ,,~ tla tes , and : ll ., ,o o l lt t~ s i l i con , w i th the h i t e r l ~ t s b e j l lg prepared in ' , : , , ' thuswa ys. F i lm s wi th lq. ll l~e I~ll " h icknes.ses have be en pr ied( ICed and spec im el~. , , have bee n su bjec te d to c l '~anges i l~ lem pera ture. Fron~ akno w le dge O f the 0 'enid tLa l s t r ess leve ls in these I i ln ls ~ .ls a I t | l l c t jo l l o f t e n l l ~ e r a l u r e ( s e e P ~ . l r t I ) , the s t ra in e t le l~ ) re lea., ,e rate fo r i t+te i 't 'ac ia ldebon t l i t lg has bee l l n lo l l i t o red t l t l i ' j l l g depos i l io l~ i l l l d s t lbse t luen l l e n l p e l ~ . l t L l l ~ e l l I s . l I l ie s , "F i le value of the M t 'aJ I~ ene rgy re lease rate at upo in t whe n in te r t 'ac ia l d ebo nd in~ occu r red ha . ', been taken :~ ,s t t] e in t c r fuc ja l t o t ighnens ( l r a c l u r e e l l e l ~ y ) , I t is conc luded t~om lhQ,, ,eob .se i ' va t ions tha t lhe jn te r fac ia l I oughness is low fo r DLC f i ln ls depos i ted O n t o m e c h a r l i c a l l y - p o l i s h e d s u r f a c e s o f l i l a n i u r r u m i l d s t e e l o rs ta in less s tee l , hu t qu i te h igh on a tumin i tmL Pre -c tea ldng by bomb~l rdmen l w i th energe l ic a i ' gon ions ra ises the in le r l ' ac ia l I oug lmess fo rthe s tee ls ~ . |nd fo r ~du t l l in iunL bu t I lo t f o r t i taniut t l . " l ' i ]ese o b s e l V a t j o l i s h W v e b e e n I e t~ . |le d to the TR|ILII 'e o f t h e o x i d e I ]h l~s on thesest lhs l l 'a les . A th in sPulte l 'ed inter layer of a . h l l l l i n i l . l n l w ~ . | s l o u r i d I ~ r a ise the in te r l ' ac ia l I ou~h t lens s ig r f i l ' i ean l ly fo r t i le s tee ls ~ . t l l d I o rt i t an i t , n t . Howevc l - . expe r in lcn ln w i lh s i l i co n suhs t la te spec ime ns show ed th [ |t t he good in te r lac ia l a t lhes jon oh ta it lu ' d , , ,. il l) A I jn te r luyers issevere ly imp a i red by hea l iiL~ in v~ .zc tturn to IemPera tt z i' es o f th~ o rder o f 50 ( )GC. I I hus been e~ lab l ished tha t th in h l lpa i rm ent o f adhes io i~ is~.1 o l t se t lue l |ge ~1" ihe Ie lea . ,,e o f . ' r en t rapped in t i le A I d t l r i t t~ spu t te r depo s i l i~m, w h ic h I '~ rmuo le .~ he f tu 'mat ion o f b l i s te r s and de la ehn le t l lo f I h e f i l m . a~ 1 9 9 N E l s e v i e r S e k ; e S . A .K m ' u ' r . ' d . L Ad hc,',io n: ('au 'hon; I')]anu md ; ell'e:',,.',,

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v a r i o u s a l l t ' [ l c l i v e I '~ r or ~ er li es . M a n y o f t h e s e f e a t u r e s a r ed e p e n d e n l o i '~ t h e b o m b a r d n l e r ~ t b y i o n s a n d a t o m s w h i c hl a k e s p l a c e d u r i n g d e p o s i l i o n T h i s h on ' d' ~ u i' d rn e n t, h o w -e v e r , a l s o t e n d s t o g i v e r i s e to s i o t l i l ' i c a i l l l e v e l s o r r e s i d u : ds tr es s , w h i c h i s n o r m a l l y c o m p r e s s i v e i n t i le a p p r o x i m a t er a n g e o f - 0 , 5 - - 2 . 0 G P a ~ .s e e P a r t I ) . T h e s e h i g h .s ir en sl e v e l s h a v e s e V e l ~ . | l c o n s e q u e n c e s i l l t e r m s o 1' t i le p e r i l s ' -.)r n a n c e o f t h e C { ) l t l J l l g , l r o m i n e l l t a n i o n g t h e s e i s t i le I ] |L . 'It h a t , p a r t i e L i l : . l r l y w h e n i h e c o ~ . l t i r l g i s r e l a t i v e l y t i l i c k , t h e r ei s u s t ro n g d r i v i l l g f o r c e f o r i t t o b e c o ln C d e t a c h e t l , " i 'l f isd r i v i n g f o r c e i s b e s t e x p r e s s e t l a s t i l e s tr a i n e n e r g y r e l e a s en 'u t e f o r i n t e r l ' a i u l d e h o n t l i n ~ g . ( ; , , ~ , l l l d , / o r t i le as ,soot ;areals t r e s s i n t e n s i t y f ; .| c t o r, K , . W r ~ e rl t h e s e i ~ a r a m e t e r s r e a c h: q ] l m , ) p r i a t e e r i t i e u l v a l u e s , v , 'h ic l~ e h a r a c l e r i s e t h e I o t l , , h -h e s s o r t h e i n t e r f a c e , t h e n d e l ~ o n d i n g i s e x l ' ~ e e t e d t o O e k . ' L t r

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[ I - 5 ] . F o r e x ~ . m l p l e , d e lw m d i lv - ,e I S e x p e c t e d I o o c c u r w h e n( ; I re a c he . ~ t h e e r i t i :. d i n t e r l ' a c i u l s t r a i n e n e t g y t l c a s r a t e ,o r i l 'l t e rf ~ l c ia . I f t a c t u r e e r l e r g y , G I , . h i p r a c t i c e , I h c t ' e m a y b e, ~ O l n e b a r r i e r I o im t i ~ . l t io r l o f t i l e i i l t e t - I ' a iu l t a ~ c k [ 6 - ~ ] , ,,,ot h a i a h i ~ h e r d r i ,, i n ~ , f o r c e I h a t l t h a t p t ' c d i d e d t n i .~ h l i n f a db e rl e c e s s a r v . H o \ ; ' e v e r , i n il J l ll J O n o f d e b o l ' , .l i r lg m a y o c c u rr e at li l~ , , r r o n l e d , , ', e s v . l l e r e t la v , ,n a r e i n e v i l a b l v p r e s e t l l ,I ~ a r l i e u l a l' l y f o r r e h l t i v e l y t h i n f i h l l s [ 8 ] . T h e r e a r e a l s o\ ' ~ L r i o t i s i s s u e s c o l l c e r l l j l l . ~ l l l e e x a c t n l e c h a n i s m s h y \ v h i c ht I l e I ' il m m a \ ' r ~ e c n m e d e t a c h e d , i n c l u d i n g t h e t' ra c tt z| 'ei )' te e h :, ln it .' s o f t i l e b u c k l i n g r , o c e s ., , [ 0 - 1 2 ] a l t d t i l e p o s s i t ' ,i l -J t y o f g u s a c c u m u l a t i o n a t I h e i n t e r l ~ c e i J r o m o t J n ~ t h ei n i t i a l d e b o n t l i n g [ I 1 . 1 3 - 1 6 ) . D I . C f i l m s h a v e a ls o b e eno ~ Js e rv e d [ t 7 ] to b u c k l e w h e n e x p o . s ed t o a i r f o r p r o l o n g e dp e r i o d ~ , T h e r e h a s a l s o b e e n i nte re .,, 1 1 1 ~ - 2 0 1 i l l t h e d e ~ c l -o l ' u n e n t o f t l u ' o u g h - t h i c k n e . s . ' , c t ' a c k n , , , , i t h i t l o a t h l ~ , s a s urCsL II I o1" r es id [ l~ , ll s I r en ,sen . Th e fo rn la l jo l l o f th ese m u3a l 'f e t h e o n s e t o f d e h o n d i n g .

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P ro v id e d th e g e n e ra t io n o f r e s id u a l , ; t r e s s c a n b e p re -d i c t e d w i t h c o n f i d e n c e ( i . e . , t h e d e p o s i t i o n s t r e s s a n dd e p o s i t i o n t e r n p e r a t u r e a r e k n o w n , a n d t h e s y s t e m r e n , a i n se l a s t i c d u r i n g c o o l i n g ) , i n f o r m a t i o n a b o u t t h e c r i t i c a l s t r a i ne n e rg y re l e a s e r a t e , G , ~. ( i n t e r fa c i a l f r a c tu re e n e r g y ) c a n b eo b t a i n e d b y o b s e r v i n g w h e t h e r a f i h n w i t h a p a r t i c u l a rt h i c k n e s s h a s d e b o n d e d b y t h e t i m e i t c o o l s t o r o o mte m p e ra t t , r e . It" t h e a s s u m p t io n i s i n a d e th a t G , ~ . i s g iv e n b yt h e w d u e o f G i w h e n d e b o n d i n g o c c u r s , t h e n a n o b s e r v a -t io n th a t a p a r t i c u la r , . ~ a t in g r e m a in s a t t a c h e d to th es u b s t r a t e p r o v i d e s a i o w e r b o u n d o n G i ~ ,, w h e r e a s i f d e -t a c h m e n t h a s o c c u r r e d , a n u p p e r b o u n d c a n b e d e d u c e d . As e r i e s o f e x p e r i m e n t s w a s , t h e r e f o r e , c a r ri e d o u t b y s i m p l yd e p o s i t i n g f i l m s o f v a r i o u s t h i c k n e s s a n d o b s e r v i n g w h e t h e ro r n o t t h e y had d e b o n d e d w h e n t h e c h a m b e r w a s o p e n e da f t e r d e p o s i t i o n a n d c o o l i n g .2.2.2. Viewing o'ing d~Tm sition

F o r s o m e e x p e r i m e n t s , t h e s p u t t e r i n g t a r g e t f l a n g e ( s e eF i g . I i n P a r t I ) w a s r e p l a c e d b y a g l a s s v i e w i n g w i n d o w .T h i s a l l o w e d d i r e c t i n -s i t u o b s e r v a t i o n o f d e b o n d i n g d u r -i n g d e p o s i t i o n . W h e n d e b o n d i n g o c c u r r e d , d e p o s i t i o n w a ss t o p p e d a n d t h e f i l m t h i c k n e s s w a s m e a s u r e d a s o u t l in e d i nP a r t I . T h i s a l l o w e d t h e v a l u e o f G , t o b e d e t e r m i n e df r o m a k n o w l e d g e o f t h e d e p o s i t i o n s t r e s s ( s e e P a r t )u n d e r t h e c o n d i l i o n s c o n c e r n e d .2.2.3. Viewing during i~ost-deposititm cooling

F o r s p e c i m e n s w h i c h h a d n o t d e b o n d e d a f t e r d e p o s i t i o na n d c o o l i n g t o r o o m t e m p e r a t u r e , f u r t h e r i n f o r m a t i o n a b o u tt h e i n t e r f a c i a l t o u g h n e s s c a n b e o b t a i n e d b y o b s e r v i n g t h es p e c i m e n d u r i n g s u b s e q u e n t c o o l i n g b e l o w r o o m t e m p e r a -t a r e . S i n c e i n m o s t c a s e s t h e t h e r m a l e x p a n s i v i t y o f t h es u b s t r a t e i s g r e a t e r t h a n t h a t o f t h e D L C c o a t i n g , s u c hc o o l i n g w i l l g e n e r a t e c o m p r e s s i v e s t r e s s i n t h e D L C . e n -h a n c i n g t h e d e p o s i t i o n s t r e s s a n d r a i s i n g t h e v a l u e o t ' G, .C o o l i n g t h r o u g h 2 0 0 C w i l l , l o t a t y p i c a l e x p a n s i v i t yin i s ln a t c h o f 1 0 x 1 0 ~ ' K i , g e n e ra t e a f ilm s t r e s s (o n a ni n f in i te s u b st r a te ) o f a b o u t - 0 . 3 5 G P a ( = A a ~ T E 'D tx , ) ,T h i s i s s i g n i f i c a n t c o m p a r e d w i t h t y p i c a l s t r e s s l e v e l s a tr o o m t e m p e r a t u r e ( s e e P ar t ) . s o t h a t p r o n m t i o n o fd e b o n d i n g b y t h i s m e l h o d s h o u l d i n p r i n c i p l e b e p o s s i b l e .a t l e a s t l o r m o s t m e t a l l i c s u b s t r a t e s . T h e c o o l i n g o p e r a -t io n s w e re c a r r i e d o u t u s in g th e a p p a ra tu s , d ro w n in F ig . I .T y p i c a l l y . t h e s p e c i m e n c o o l e d f r o m r O O l ll t e m p e r a t u r ed o w n t o a b o u t - 1 9 3 C o v e r a p e r i o d o f a b o u t 3 0 r a in .T h i s i s c o n v e n i e n t f o r c o n t i n u o u s o b s e r w ~ t i on a n d f o ra c c u r a t e r e c o r d i n g o f t h e t e m p e r a t u r e a t w h i c h a n yd e b o n d i n g t n i g h l o c c u r .2.3. Amu,al ing e.vlwriments

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d u r i n g h e a t t r e a t m e n t . S p e c i m e n s w e r e h e a t e d u n d e r v a c -u u m ( 5 P a ) f r o m m o r n t e m p e r a t u r e t o 5 5 0 C . a t a c o n s t a n th e a t i n g r a t e o f a b o u t 2 0 C p e r r a i n . T h i s w a s c a r r i e d o u t i na c h a m b e r w i t h a v i e w i n g w i n d o w . T h e s e s p e c i m e n s w e r ei n s p e c t e d v i s u a l l y d u r i n g h e a t i n g a n d i n t h e o p t i c a l m i c r o -s c o p e / S E M a f t e r t h e y h a d c o o l e d t o r o o m t e m p e r a t u r e .D e d u c t i o n s w e r e m a d e a b o u t t h e c o n d i t i o n s u n d e r w h i c ha n y o b s e r v e d d e b o n d i n g h a d ~ x : c u r r e d .

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Re+ , i t t u a l +q f 'e ,e , l ex e l s ( . ' ln d h e r l ee s t r a i n e t lt :r g .' + r eJe i l ~ , e I '; .l ld h ) Wef t, ' ca l c l t l ; l l e d u s i n g d e p o x i l i o l l x t r ' e , ,s v a l u e s ( s ee P ar t 1 } ] t i l l1 t i l e f o l h w eJ l | g t h e r l l l a le \ p u n , , i x i l y d i l t a [ 3 7 1 : + ~ 1 ~ t . < . = 2 . 3 . '< 1( 1 n K ~ . c t l , = R . 5 111 " K r . + + , q ~ = 1 2 . 2 x I t ) n K I , ~ % s = 1 6 I11 " K I , < + x 1 = 2 4 1 0 l l h u' , t rh , q l a t u " p r i t~ r t o d e l ~ o , , i t h , , l L , I I ) I . ( " o n l h c i l l l c r l a ~ . ' i i l l I t~ l . l g h l le s s . f o rd i f h . ' rL 'n l " , t t 't ,' .+ l a l e s .

bomb ardn len l p rocess . T i le same is ro le Ib r a lumin ium , hu lthe high value o1" G,~ observed in the absence o f pre-elean-ing was increased s igni f icandy by argon bombardment toover 350 , I m : , T l l is is pres lmlahly associated wi thren lova l o f g e r t e r a l c o n t a n l i n a t i o n S ll C Jl its h y t h ' a t e d layers(Itl the surface o f the i t lunl i l l ; l . For t i le s teels , t i le s t l r | ' ~ t c et )x ide I ' i l lns were presumably removed by the bornbard-m e r i t p r u c e s s .In v iew of the excel lent adhesion exhib i ted on a lu-m in ium, an A I i n te r layer o f fe rs p romise as a method o fimproving, the bonding. I t was indeed fotm d t l)a t a l l l it (80r im ) l a y e r o f A I d e p o s i t e d o n t h e s u b s t r a te p r i o r t o D L Cdeposi t ion ra ised the in ter fac ia l toughness substant ia l ly fort i tan ium and for both s teels . The impor tance of sur faceox ide in con tac t w i th the DLC was h igh l i gh ted fo r th i sc a s e a i m b y i n t r o d u c i n g a s t a g e i n w h i c h t il e a l u i l l in i u n li n t e r l a y e r w a s e x p o s e d t o a i r. a l l o w i n g f o r m a t i o n o f a t h ins u r f a c e o x i d e . ( I l l f a c t , t h e r e w o u l d b e ; ll l e a s t +.1 m o n o l a y e ro f o x i d e p r e s e n t i n a n y e v e n t , b t ~ t t h i s w o u l d t e n d t ot h i c k e n a p p r e c i a b l y a n d a l s o t o f o r m w e a k h y d r a t e d l a y e r so n e x p o s u r e t o air). I n t r o d u c t i o n o f the o x i d : i t i o n s t a g er e s u l t e d i n t h e m e a s u r e d i n t e r f a c i a l I < m g l m e s s f a l li n g t ov ; d u e s c l o s e I t) t h o s e i n ti le a b s e n c e o f t i le i n t e r l a y e r o rpre-c leaning step.

hi | ' i tcl , there is evidence that oxidation of the AIin ter layer c l langud the hu. 'a t ion e l the debtm ding event ,F i g . 3 s h o w s E D X s p e c t r a t a k e n I ' r o n l f r e e S t i l ' f a c e s b e f o r ed e p o s i t i o n o f ti le D L C f il rr t a n d a f t e r i t h a d d e b o n d e d , f o rs p e c i m e n s w i t h a n d w i t h o u t t h e i n t e r l a y e r o x i d a t i e n s t a g e ,i t c a n b e s e e n t l ) a t a n AI peak ab.~ent af ter d e h t m d i n g w i t ht i l e t m o x i d i s e d A I i n t e r l a y e r h a s a l ' q ' ~ e a r e d i n t h e s p e c i m e ne x p o s e d t o t h e p r i e r o x i d a t i o n o f t h e in t e r l a y e r , h f o l l o w s


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X . L . t e n g , 7+,W. Cl ym , / 77+i. S o l i d I , il m s 3 1 2 1 I tJ g , O 2 I ~ - 2 2 7

T a b l e 2D e p o s i t i o n c o n d i t i o n s a n d d e b o n d i n g b e h a v i o u r o f S i s u b s t r a t e s p e c i m e n s s u b j e c t e d t o h e a t I : , ~ ,~tments

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S p e c i m e n d e t a il s D e t m n d i n gS u ~ t ra t e ( m s ) P r e - c l e a n in g c o n d i t it m s D L C p r e l a y e r ( p . m ) A I ( / J. n O O x i d i s e D L C ( p r o ) T e m p . ( ' ~ C ) G , . ( J m - : ) A p p e a r a n c eSt . 0 .38 - ( I O - 0 . 8 4 1) 1 7 ,8 D L C / S i d e b o n dSt , 0 .38 Ar , I Pa 0 i ) - 5 .7 41 ) 127 Fruc tu red wi th in S iS t . 0 . 3 8 A r . I P a 0 1) - 4 , 5 5 41 ) 9 7 D L C / S i d e l 'a m dSt , 0 .38 Ar- II )C], CH ~, 1 l " ~ 0 ,02 0 - t ,0 50+,) 19 .2 I so l a t ed b l i s t e rs tF ig , 6a tSt , 0 .38 Ar-1 ()9~ CH.~, 2 Pa 0 .05 0 - 1 ,0 451) 19 .5 L ink ed b l is t er , '+ (F ig . 6b )St , 0 .38 Ar , I P i , 0 0 .08 0 .1 450 2 .0 W rink le s (F ig . 7 )S t , 0 , 3 8 A r . t P+'l 0 0.(18 - 4(XI ~ Isola ted bl is te rs (Fi g. 8)R e s i d u a l s t r e s s l e v e l s ( a n d h e n c e s t r a i n e n e r g y r e l e a s e r a t e s ) w e r e c a l c u l a t e d u s i , g d e p o s i t i o n s t r e s s v a l u e s ( s e e P a r t ) a n d t h e f o l l o w i n g v a l u e s [ 3 71 f u r t h ethernm l exp ans iv i ty o f D LC and s i l i co . :


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224 A ' .L , IYng , I~W ( ' l yr ic / l hi n Srdid ~ i /ms 312 1~9,~'~ 219 227

duc t() a red tnc t ion in the e ffec t ive in tc r l i tc ia l toLnghness .T h e re fo re . w h i l , - v a lu e s f o r G , , . c a n b e e s t im a te d l r o m a no b s e r v e d t e n | p c r a t tl r e o f d e b o n d i n g , u s i n g t h e s a m e p r o c e -d t l r e s a s i n S e c t io n 3 . I . i t s h o u ld b e n o te d th a t t h e s e v a lu e sm a y b e o v e re s t im a te s a :; a c o n s e q u e n c e o f t h e f i= l l i n f ilms t i f fn e s s a n d h e n c e in f i l n i s t res s .

R e s u l t s o f t h e l l e a t in g e x p e r im e n t s a re s t~ m m a r i s e d inT a b le 2 a n d F ig . 4 . T h e f i r s t p o in t t o n o te i s t h a t t h ei n t e r f ac i a l t o u g h n e s s o f ~ ' s t a n d a r d ' ( p r o - c l e a n e d ) S i - D L Ci n t e r f a c e i s r e l a t i v e l y h i g h . I n e x p e r i m e n t s o f t h e t y p ed e s c r ib e d in S e c t io n 3 . 1 , i t w a s fo u n d th a t w h e n l a rg ed r iv in g fo rc e s lo r d e b o n d in g w e re g e n e ra t e d , t h e y a C t t l , ' f l l ycau sed fr , '~c tu re wif l l in the S i subs tra te , ra th e r Ihar a t thei n t e r f a c e . S u c h o b s e r v a t i o n s a l l o w e d a l o w e r b o u n d t o b ce s t a b l i s h e d o n G , , o f abo ut 130 J n l -~. He a t ing o f s p e c i -n l e n s w h i c h w e r e i n t a c t ; n r o o m t e m p e r a t u r e p r o d u c e dd e b o n d i n g a t a b o u t 5 4 0 C . c o r r e s p o n d i n g t o a G , , v a l u e o fa b o u t 1 0 0 J m - '. S u c h h e a t in g e v id e n t ly h a s o n ly a m i n o r

e f fe c t o n t h e in t e r fa c i a l t o u g h n e s s . H o w e v e r , t h i s s i t u a t io nc h a n g e s w h e n i I1 p r e - c l e a n i n g i s c a r r i e d o u t w i t h m e t h a n ep re s e n t i n th e b o r ;~ b a rd in g g a s . Wh e n th i s i s d o n e , s o m eD L C i s d e p o s i t e d d u r in g th e c l e a n in g p ro c e s s a n d th i s i ss o m e t im e s th o u g h t t o in lp ro v e th e in t e r t i | c in l s t r e n g th . Infac t , i t i s c lea r i ll ',~t th is p roc ess leads to a ,ve ak , : r in te r faceo n s u b s e q u e n t h e a t in g . B l i s t e r s t e n d to fo rm , fo l lo w e d b ye x t e n s i v e d e t a c h m e n t , a n d t h e a p p a r e n t i n l e r f a c i a l t o u g h -hess fa l ls t o b e l o w 2 0 J n l "~.

I t s e e m s l i k e l y t h a t d e b o n d i n g c a n b e p r o m o t e d b y t h en u c le a t io n a n d g ro w th o r a g a s b u b b le a t Ih e in t e r fa c e . T h ee f fe t o f t h i s i s Io r e d u c e s h e a p p a re n t i n t e r fa c i a l t o u g h -n e s s . T h e i n i t i a t i o n a n d s u b s e q u e n t a r r e s t o f t h e g r o w t h o fb l i s t e r s i s d e p ic t c d s c h e m a t i c a l ly in F ig . 5 . A p o te n t i a l lyi m p o r t a n t f a c t o r i s t h e d e c r e a s e i n c r a c k o p e n i n g ( m o d e i )s t r e s s i n t e n s i ty l~l tor a t the c rack t ip a s the b l is te r a re ;~c x p a n d s [ I I ]. O n a l m e a l i n g , h y d r o g e n ( u n b o n d e d a n db o n d e d ) , a n d p o s s i b l y h y d r o c a r b o n g a s a n d a r g o n i n t r o -

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( c ) B l i s te r g r o w s u n t il a r r e s t e d b yr e d u c e d g a s p r e s s u r e a n d / o r l o w e rc r a c k - o p e n i n g s t r e ss i n t e n s i t y a t e d g e s

( dp A l t e r n a t i v e l y , f i l m b e n d i n g l e a d st o n e t t e n s i o n a n d b r i t t l e f r a c t u r e

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F [ : : . 5 . S c h u n l ; l l i c d e p i c t i o n o 1 il L tL ' rf a t, i, d t l u l u m i r m t i t m , . , , i f i l n l L l n dt .' l C O l n p r c ~ s i v c ' , U ,. , .' ,. l ' h c H l J l i ; . L l i . t l n , ? ~ L ' 1 1 1 ( ; a ) , Il l; , I. ~ l T , i ) r t m l o l u d 1 ')5 n u d c a l i o n o f a ~ a ., ,b t f l ~h i c , I ] uc k l J r i g ~ t 1 i 1 I dm . ( hk i '. , l ~ .i ', ,q ' p tl t' Cd q ~ i . t t | , - , i t I 'L ' , , L I IL ~ J t l d c c r c u , , - . e d jtlIpi;~ ,ll~. ,dl'',,.,',,L -,.T h e t ' f l i ' , l , , .' r I l lLW ,, ,gld' f i l i. ' ,c. I t ) . i ' , , . ', . 'ausc ~1 I ' , L I L I L ' . ~ d t ' . i . i L ' k~ . t p C l l i l l ~ ~ t r c . ~ s J n l L ' l l ~ J t y ; . t I1 L L i 1 ~ i L ~ , p l ' e , ~ . , , t l r c J ~ , i l ~ , i ~ n i l ' ] k ' i l i i l d l ' i ~ [ r l ~ I ] H ' ~ ' L ' . ~. L~ , ; .t C O I l b ~ ' { . i t i L ' l l~ . ' C t ) t r e d u c e d r ~ r , . . '. ' , .' , t |r . A l l : . I I I ~ . ' r I t i | t j v L ' ~ . ' l | d p o i i | L , ( d ) , o c c t z r ~ , i t ' t i l ef i l m u n d c r ~ . , s l h r o u u h - t l i ic k r z , , x I r : i c t u r c . r e l u x i n ~ m - p i a n o , ,t l. ~ ,, ,c ,, i n th e v i c i n i l ~ ; ro d r c lc ; ~ , ,i n g a n y g a x presxurc in i h c u t ~ x c n c e o f g ~ t~ e v o l u t i o r t , t h e, ,c q U e lZ C C s h o ~ v n i n ( i ) - ( i i i ) r a i L ' , o C c L ; r . ~ i l t z t h e C o l n p r e , , s i v e , , i r e ,, ', l e a d i n g t ~ ~ , hu a~ cruck in~. ~ t ' t h e f i ll n , f o l l o ~ e d h y d e h ~ u z d i n g .


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b e p r o m o t e d b y h e a t i n g a s y s t e m c o n t a i n i n g an A I in t e r -l a y e r . T h e r e s u l t o f h e a t i n g a s p e c i m e n w i t h a I 0 0 n mD L C l a y e r an d a n 8 0 n m A I i n t e r l a y e r ( o x i d i s e d ) i s sh o w nin F ig . 7 . I t i s c l e a r t h a t e x te n s iv e w r in k l in g o f t h e f i lm h a so c c u r r e d . T h i s i s a p p a r e n t l y a c o n s e q u e n c e o f t h e b u i l d - u po f A r r e l e a s e d f r o m t h e A I i n t e r l a y e r , r e d u c i n g t h e a p p a r -e n t i n t e r ra c i a l t o u g h n e s s to a v e ry lo w v a lu e ~ o f a b o u t 2 Jm - ~ . T h a t t h i s d e b o n d i n g i s a ss o c i a t e d w i t h p r o b l e m s:a r i s in g in th e A I l a y e r i s a p p a re n t f ro m th e o b s e rv a t io n th a tb l i s t e r i n g o c c u r r e d o n h e a t i n g w h e n o n l y t h e A I l a y e r w a sp re s e n t . T h i s c a n b e s e e n in F ig . 8 . T h i s i s a n im p o r t a n to b s e r v a t i o n , s i n c e i t m e a n s t h a t c o n d i t i o n s d u r i n g t h ep r o d u c t i o n o f s u c h a n i n t e r l a y e r m a y b e c r i t i c a l l y i m p o r -t a n t i f t h e d a n g e r o f d e b o n d i n g o n h e a t i n g i s t o b e a v o i d e d .F o r e x a m p l e , e n t r a p m e n t o f A r d u r i n g s p u t t e r d e p o s i t i o n o ft h e i n t e r l a y e r c o u l d i n p r i n c i p le b e r e d u c e d b y u s i n g al o w e r A r p r e s s u r e a n d / o r a h i g h e r s u b s t r a t e t e m p e r a t u r e( a l l o w i n g t h e a n y e n t r a p p e d A t ' t o d i f f u s e o u t o f t h e l a y e r ) .In p r a c t i c e , s u c h e n t r a p m e n t m a y b e d i M c u l t t o a v n i d .T h i s i s a n a r e a r e q u i r i n g f u r t h e r w o r k .

4 C o n c l u s i o n sThe f o l l o w i n g c o n c l u s i o n s c a n b e d r a w n f r o m t h i s

w o r k .( 1 ) W h e n D L C c o a t i n g s a r e d e p o s i t e d u n d e r s t a n d a r d

c o n d i t i o n s o n t o m e c h a n i c a l l y p o l i s h e d s u b s t r a t e s o f t i t a -n iu m , m i ld s t e e l o r s t a in l e s s s t e e l , d e b o n d in g t e n d s to t a k ep la c e r e a d i ly . T h e in t e r fa c i a l t o u g h n e s s lb r a l l o f t h e s ec a s e s h a s b e e n e s t i m a t e d a t a b o u t 7 J m - - ~ . T h i s l o w v a l u ei s a t t r i b u te d to th e p re s e n c e o f t h i c k , f r i a b le o x id e l a y e r s .F o r a l u m i n i u m , o n t h e o t h e r h a n d , t h e t o u g h n e s s w a s q u i t eh i g h , a t o v e r 0 0 J m - ' . I n t h i s c a s e , t h e o x i d e l a y e r w a sp r e s u m a b l y r e l a t i v e l y t h i n a n d c o h e r e n t , s o t h a t i t d i d n o tr e a d i l y p r o m o t e d e b o n d i n g . T h e D L C a p p a r e n t l y a d h e r e sw e l l t o s u c h a n a l u m i n a l a y e r .

(2 ) F o r th e tw o s t e e l s , a n in s i t u p re -c l e a n in g p ro c e s sa p p l i e d to th e s u b s t r a t e , i n v o lv i , ~ g b o m b a rd rn e n l b y a rg o nio n s , r a i s e d th e in t e r fa c i a l ~ 'o u gh n e, ,, s c o n s id e r a b ly , t o v a l -u e s in e x c e s s o f 2 0 0 J m - ' ~ . T h i s i s p r e s u m e d t o b ea s s o c i a t e d w i t h t h e e f f e c t i v e r e m o v a l o f t h e o x i d e l a y e r s .i n th e c a s e o f a l u m i n i u m , t h e t o u g h n e s s w a s r a i s e d t o av e r y h i g h v a l u e o f o v e r 3 5 0 J m ~ -~ . T h i s m a y h a v e b e e nc a u s e d b y a s m a l l r e d u c t i o n i n o x i d e l a y e r t h i c k n e s s a n dg e n e r a l r e m o v a l o f s u r f a ce c o n t a m i n a t i o n s u c h a s h y d r a t e dla y e r s . F o r th e t i t a n iu m s u b s t r a t e , o n th e o th e r h a n d , t h e

J The conc ep t o f a scr i ' *r ig ~ ,n t 'fec l iVe in le r fac ia l tqmghness on theh a ., ,i ,, ~1 ' t h e re s id u a l s t res . , , e~ p re~en t wh en d eb tm d in ~. ~ ccu rs c l ea r lybe t 'omes ve ry dcmh t fu l w hen the dcb~md ing i s la rL~c ly due i~ [zas evo lu -t ion and b t in le r Io rnmt i~ ,n . w i lh the res idua l s tr enses p~s s ih ly p la y ing m~r~l at a l l . F,v c n i n t h i s s i l u u li ~ n , h ~ w e v c r , t h e p r o c e d u r e i s s t il l a Ol tVell J en wa y ~i h ig h l ig h lh ~g Ih e I ' ac l Ih a l ~as ev ~) lu t io n i s d ram at ica l lyr ; fi~ in~ Ih e l ik e l ih u ~ d ~1' d eh em d in ~.

p re -c l e a n ih fg p ro c e s s d id n o t s ig n i l i c :m t ly a f fe c t t h e in t e r fa -c i a l t o u g h n e s s . A p p a re n t ly a r e l a t iv e ly th i c k a n d f i ' i a b l eo x i d e f i l m p e r s i s t s i n t h i s s y s t e m , i n h i b i t i n g g o o d b o n d i n g .

(3 ) F o r th e t i t a n iu m a n d tn ~ tw o s t e e l s , t h e in t ro d u c t io no f a n a l u m i n i u m i n t e r l a y e r b y s p u t te r d e p o s i t i o n h a s b e e nf i~ u n d to e l ' f e e t a s ig n i f i c a n t i n c re a s e in th e in t e r fa c i a lt o u g h n e s s , t o a r o u n d 4 0 - 5 0 J m - ~ . T h i s i s c o n s i s t e n t w i t ht h e g o o d b o n d i n g o b :, ~ er v ed b e t w e e n D L C a n d A I s u b -s t r a t e s a n d w i th a s p u t t e re d A I l a y e r a d h e r in g w e l l t o ac l e a n e d m e t a l l i c s u b s t r a t e . H o w e v e r , w h e n t h e s p u t t e r e dA I l a y e r w a s e ~ p o s e d t o a i r b e f o r e t h e D L C w a s d e p o s i t e d ,th e n th e in l e r f i l c i a l t o u g h n e s s w a s r e d u c e d to v a lu e s f a i r lyc lo s e In th o s e in th e a b s e n c e o f a n y p re -c l e a n in g o ri n t e r l a y e r d e p o s i t i o n .

( 4 ) E x p e r i m e n t s h a v e b e e n c a r r i e d o u t i n w h i c h D L Cc o a t i n g s o n s i l i c o n s u b s t r a t e s h a v e b e e n h e a t e d i n v a c u u mt o a b o u t 5 5 0 C . D L C a d h e r e s w e l l t o S i , p r o v i d e d ap re -c l e a n in g p ro c e s s i s c a r r i e d o u t . I t w a s fo u n d th a t , w h i l eg o o d a d h e s io n ( -, -, 1 0 0 J t n ~ 2 ) w a s r e t a in e d o n h e a t in g fo rt h e s t a n d a r d i n t e r f a c e , i t b e c a m e s e v e r e l y i m p a i r e d i nc e r t a in o th e r c a s e s a s a c o n s e q u e n c e o l ' t h e r e l e a s e o fa r g o n e n t r a p p e d w i t h i n t h e s t r u c t u r e , a n d t h e p r o m o t i o n o fd e b o n d i n g b y b l i s t e r l b r m a t i o n . I n p a r t i c u l a r , w h e n p r e -c l e a n i n g i s c a r r ie d o u t w i t h m e t h a n e i n t he a t m o s p h e r e , s otha t a th in p re -l t,~yer HI" DL C is fo rm ed , th is p r e - l ay erc o n t a i n s e n t r a p p e d A r w h i c h i s r e l e a s e d o n h e a t i n g . F u r -t h e r m o r e , i t a p p e a r s t h a i A r b e c o m e s e n t r a p p e d i n t h e Ai n t e r l a y e r w h e n t h i s i s f o r m e d b y s p u t t e r d e p o s i ti o n . T h u s ,D L C c o a t i n g s w i t h A I i n t e r l a y e r s a l s o d e b o n d e d r e a d i l y onh e a t in g .

A c k n o w l e d g e m e n t sFinancia l s uppor t has be en prov ided for one o l t i le

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