OXYGEN INDUCED DAMPING PEAKS IN COLD WORKED COPPER

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OXYGEN INDUCED DAMPING PEAKS IN COLD WORKED COPPER

Ch. Wolny, R. Wolny, H. Müllner

To cite this version:

Ch. Wolny, R. Wolny, H. Müllner. OXYGEN INDUCED DAMPING PEAKS IN COLD WORKED COPPER. Journal de Physique Colloques, 1985, 46 (C10), pp.C10-243-C10-246.

�10.1051/jphyscol:19851055�. �jpa-00225439�

OXYGEN INDUCED DAMPING PEAKS I N COLD WORKED COPPER

C h .

WOLNY, R . WOLNY

H . M ~ L L N E R '

+Institut fur ~estk8rperphysik der Universitdt Wien, Strudlhofgasse 4, A-1090 Wien, Austria

Abstract - The influence of an oxidizing annealing atmosphere on the internal friction in the Hz-range has been investigated in cold worked copper. In the temperature region of the Hasiguti peak P2 an oxygen induced damping peak is observed and discussed on the basis of dislocation damping due to mobile pinning points.

I - INTRODUCTION

During the last years the influence of annealing conditions on the damping behabiour of copper has been of increasing interest /1-4/. Smarizing the experimental results /5,9/ it must be stated that internal friction strongly depends on the annealing atmosphere. In particular previous experiments /6/ and recent in- vestigations / l o / clearly reveal the existence of oxygen induced relaxation effects due to dislocations interacting with the oxygen dissolved.

I1 - EXPERIMENTAL PROCEDURE

Rod shaped polycristalline samples (4omm lenght, lmm diameter) of copper (5N,Johnson Matthey) were used for the present investigation.

All s m les were annealed at 1073K for loh in vacuum (p less than 4. lo-' Fa air) in order to provide identical material conditions ( A ) . Different lots of samples were annealed subsequently in a slightly oxidizing atmosphere at the same temperature for 1h.Oxygen of 99,99%

purity was used. The pressure is listed in Tab.1. The oxygen content dissolved in the samples was roughly estimated using the relations reported in / 20/.

Table 1: Material specification - annealing condition

material annealing time pressure oxygen content

condition in hours in Pa in ppm

A 10 < ^{4.1oI$air 4}

B + 1 2.30 O2 40

C + 1 4. 10-202 7

Inter a1 friction was measured with an inverted torsion pendulum (2Hz, 5. lo-' strain /l/)after in situ tensile deformation at 80K. Linear

Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:19851055

C10-244

JOURNAL DE PHYSIQUE

h e a t i n g was u s e d a t a h e a t i n g r a t e o f O,SK/min. The f u n d a m e n t a l f r e - quency o f t h e pendulum c o u l d be d o u b l e d b y r a i s i n g t h e moment o f i n e r t i a . T h i s a l l o w s t h e d e t e r m i n a t i o n o f t h e a c t i v a t i o n e n e r g y f r o m t h e same s a m p l e .

I11 - EXPERIMENTAL RESULTS

The i n t e r n a l f r i c t i o n r e s u l t s a f t - 2% t e n s i l e d e f o r m a t i o n a t 80K ob- t a i n e d f r o m s a m p l e s o f m a t e r i a l A a\nd

a r e shown i n F i g . 1 . The c u r v e s 2 a n d 3 which w e r e o b t a i n e d f r o m t h e m a t e r i a l A r e f l e c t t h e c h a r a c - t e r i s t i c damping b e h a v i o u r o f c o l d worked s a m p l e s . The H a s i g u t i p e a k s P2 a n d P3 a p p e a r d u r i n g t h e f i r s t t e m p e r a t u r e r i s e i m m e d i a t e l y a f t e r deformation. S u b s e q u e n t a n n e a l i n g a t 450K f o r 2 0 m i n . c a u s e s PI t o a p p e a r . The damping c u r v e s o f m a t e r i a l C show d i f f e r e n t b e h a v i o u r . I t c a n b e o b s e r v e d t h a t o x y g e 3 p p r e t r e a t m e n t l e a d s t o a n a d d i t i o n a l

damping p e a k d e n o t e d a s

i n c u r v e 2 . T h i s p e a k h a s n o t b e e n r e c o g - n i z e d b e f o r e a l t h o u g h i n d i c a t i o n s o f a weak s h o u l d e r a t t h e low tem- p e r a t u r e s i d e o f P2 c'an b e s e e n i n c u r v e s p u b l i s h e d by o t h e r s / 1 1 , 1 2 / . Curve 3 r e v e a l s t h a t P1 i s h i g h e r a n d f l a t t e r i n o x i d i z e d s a m p l e s compared w i t h t h a t obse+ved i n m a t e r i a l A. F u r t h e r m o r e c u r v e 1 i n d i - c a t e s l o w e r damping v a l u e s i n undeformed o x i d i z e d s a m p l e s . A s i t w a s shown p r e v i o u s l y / 1 / t h e s e damping v a l u e s show a m i n o r p r o n o u n c e d d e p e n d e n c e o n a m p l i t u d e .

F i g . 1

1"

Damping i n c o p p e r a f t e r 2% t e n s i l e

d e f o r m a t i o n a t 8 o K - I n f l u e n c e o f oxygen-

?

p r e a n n e a l i n g .

L e t t e r s d e n o t e m a t e r i a l c o n d i t i o n a c c o r d i n g t o Tab. 1.

I . . . p r e a n n e a l e d s t a t e 2 . . . a f t e r d e f o r m a t i o n

PO

&re-..

3 . . . a f t e r s u b s e q u e n t a n n e a l i n g

a t 450K f o r 20 'min.

100 150 300

7 t Y P E R A r U I E 01)

- ~ i ~ . 2 shows t h e damping c u r v e s i n t h e t e m p e r a . t u r e r e g i o n o f t h e H a s i g u t i p e a k s P1 a n d P 2 , m e a s u r e d o n s a m p l e s o f m a t e r i a l A,B and C i m m e d i a t e l y a f t e r 4 % t e n s i l e d e f o r m a t i o n a t 80K. I t i s c l e a r l y v i s i b l e t h a t a t h i g h e r o x y g e n c o n t e n t t h e s p l i t t i n g up o f t h e damping v a l u e s i n t o two p e a k s i s more p r o n o u n c e d . F i g . 3 shows t h i s e f f e c t f o r d i f f e r - e n t d e g r e e s o f d e f o r m a t i o n .

F i g . 2 :

T e m p e r a t u r e r e g i o n o f

a n d P2 a f t e r t e n s i l e d e f o r m a t i o n a t 80K.

- I n f l u e n c e o f oxygen c o n t e n t F i g . 3 :

T e m p e r a t u r e r e g i o n o f

a n d P2 a f t e r d i f f e r e n t amounts o f c o l d work a t 80K

1 ... ^{2 % , 2} ... ^{4 %}

F i g . 2 F i g . 3

d i f f e r e n t s a m p l e s e q u a l l y t r e a t e d . A c o m p a r i s o n o f t h e r e s u l t s o f t h e p r e s e n t i n v e s t i g a t i o n w i t h d a t a f r o m t h e l i t e r a t u r e /11 t o 1 9 / i s g i v e n i n F i g . 4 .

T a b l e 2 : A c t i v a t i o n e n e r g y o f damping p e a k s o b s e r v e d i n m a t e r i a l C Peak

1

P2 P3

a c t i v a t i o n

e n e r g y i n ( e V ) o , 3 2 ~ 0 , 0 1 0 , 2 6 + 0 , 0 2 0 , 3 6 + 0 , 0 2 0 , 4 3 + 0 , 0 7 -

, F i g . 4 : A r r h e n i u s - p l o t o f c o l d work p e a k s

The r e s u l t s o b t a i n e d f o r t h e P a n d P2 p e a k s i n t h e p r e s e n t i n v e s t i g a - t i o n a r e i n good a g r e e m e n t w i t 2 l i t e r a t u r e d a t a . F o r t h e

p e a k , how- e v e r , t h e d e t e r m i n e d v a l u e o f t h e a c t i v a t i o n e n e r g y i s s i g n i f i c a n t l y l o w e r t h a n t h o s e o f t h e H a s i g u t i p e a k s .

- 5 .

-

> ⁰

0 z YI 3 1

A, A . . . p r e s e n t i n v e s t i g a t i o n

. . . l i t e r a t u r e d a t a

0 Y

a Y

I t i s w o r t h t o m e n t i o n t h a t t h e d a t a r e p o r t e d i n / 1 7 / f o r t h e P1 peak l i e e x a c t l y on t h e A r r h e n i u s g r a p h f o r

However i t was m e n t i o n e d i n / 1 7 / t h a t P1 was much h i g h e r i n s a m p l e s w i t h h i g h e r oxygen c o n t e n t . I V - DISCUSSION

Y N d i f f e r e n t s t a i n a m p l i t u d e y :

I M O J T (K-'1 0

. . . E = 3 .lo-', . ^.

^.f = 6 . l o

11-

The f a c t t h a t o x i d i z i n g a n n e a l i n g a t m o s p h e r e a f f e c t s i n t e r n a l f r i c t i o n b e h a v i o u r i n c o p p e r i s c o n f i r m e d by r e s u l t s o f o t h e r a u t h o r s , t o o / 7 ,

8 , 9 , 1 7 / . The r e l a x a t i o n e f f e c t o b s e r v e d i n t h e p r e s e n t i n v e s t i g a t i o n was n o t r e c o g n i z e d b e f o r e . The c o r r e s p o n d i n g p e a k d e n o t e d a s Po c a n n o t b e a t t r i b u t e d t o o n e o f t h e H a s i g u t i p e a k s b e c a u s e o f i t s s i g n i f i c a n t s m a l l e r a c f i v a t i o n e n e r g y . A s t h i s peak i s o n l y o b s e r v a b l e i n o x i d i z e d s a m p l e s i t c a n n o t b e c a u s e d by d e f o r m a t i o n i n d u c e d i n t r i n s i c d e f e c t s . Due t o i t s d e p e n d e n c e on oxygen c o n t e n t and on t h e amount o f d e f o r - m a t i o n d i s l o c a t i o n s i n t e r a c t i n g w i t h t h e oxygen d i s s o l v e d a r e t h o u g h t t o b e r e s p o n s i b l e f o r t h i s e f f e c t . I t i s d i f f i c u l t t o o b t a i n i n f o r m a - t i o n on t h e . s p e c i a 1 f e a t u r e s o f

a p p e a r i n g a f t e r c o l d work a n d o n t h e p r o c e s s e s i n v o l v e d b e c a u s e

i s a l w a y s accompanied w i t h P 2 . I t i s i n t e r e s t i n g t o compare t h e p r e s e n t r e s u l t s f r o m Hz-measurements w i t h k H z - d a t a / 6 , 1 0 / m e a s u r e d on e q u a l l y h e a t t r e a t e d C u - f o i l s . The l a t t e r r e v e a l t h e p r e s e n c e o f a n oxygen i n d u c e d peak ( F i g . 5 ) i n f u l l y a n - n e a l e d s a m p l e s . The f r e q u e n c y - t e m p e r a t u r e p l o t o f t h i s peak a g r e e s w i t h t h e e x t r a p o l a t i o n o f t h e A r r h e n i u s l i n e o f F i g . 4 . Thus t h e a c t i - v a t i o n e n e r g i e s a r e e q u a l a n d o n e c a n c o n c l u d e t h a t b o t h p e a k s a r e due t o t h e same p r o c e s s . Among t h e d i f f e r e n t models d e a l i n g w i t h d i s l o c a - t i o n s i n t e r a c t i n g w i t h p o i n t d e f e c t s t h e t h e o r e c t i c a l c o n s i d e r a t i o n s

15 '."TI5

\ 1 6 0 1 8 0 2 0 0

013 \

\

P, PO PI

TEMPERATURE K

F i g . S

Oxygen i n d u c e d peak i n a n n e a l e d

C u - f o i l s m e a s u r e d a t 450 Hz w i t h

C10-246 JOURNAL DE PHYSIQUE

r e p o r t e d by Liicke / 2 / a n d W i n k l e r / 3 , 4 / seem t o b e s u i t a b l e f o r f u r t h e r d i s c u s s i o n on t h e Po p e a k . E s p e c i a l l y t h e l a t t e r d e a l s w i t h t h e com- b i n e d m o t i o n o f p i n n i n g p o i n t s p a r a l l e l ( l o n g i t u d i n a l ) a n d p e r p e n d i c u - l a r ( t r a n s v e r s a l ) t o t h e d i s l o c a t i o n l i n e . A n a l y t i c a l e x p r e s s i o n s w e r e d e r i v e d c o n c e r n i n g t h e c o r r e s p o n d i n g r e l a x a t i o n t i m e s T T a n d r L . Both t i m e s a r e d e p e n d e n t on t e m p e r a t u r e , d e f e c t m o b i l i t y and mean f r e e l o o p l e n g h t . ~ e s i d e s r ~ i s m a i n l y d e t e r m i n e d by t h e s t r a i n , rT by t h e p o s i t i o n o f t h e d e f e c t , r e s p e c t i v e l y . A c c o r d i n g t o t h i s model w i t h i n c r e a s i n g t e m p e r a t u r e o n e would e x p e c t one o r two damping p e a k s

(w'I;~ = 1 and@% = 1) d e p e n d i n g on t h e r e l a t i v e m a g n i t u d e o f t h e two r e l a x a t i o n t i m e s Z L / Z T 1 1 and z L / Z T 4 l 7 r e s p e c t i v e l y . S h a p e , t e m p e r a - t u r e and h e i g h t o f t h e s e p r e d i c t e d p e a k s depend i n a complex manner on s t r a i n . Based o n t h i s model a d e t a i l e d a n a l y s i s o f t h e r e s u l t s c o n c e r n i n g Po i s g i v e n i n / l o / from which one c a n c o n c l u d e t h a t b o t h , l o n g i t u d i n a l a n d t r a n s v e r s a l m o t i o n c o n t r i b u t e t o

I t w a s e s t a b l i s h e d t h a t i n t e r n a l f r i c t i o n i s s t r o n g l y i n f l u e n c e d by t h e a n n e a l i n g atmos h e r e . I n s l i g h t l y o x i d i z e d s a m p l e s a n oxygen i n d u c e d damping p e a k Pp was o b s e r v e d . The p r e s e n c e o f PO s h o u l d b = t a k e n i n t o a c c o u n t i n e v a l u a t i n g r e s u l t s f r o m i n v e s t i g a t i o n s d e a l i n g w i t h t h e U a s i g u t i p e a k s P i and P2. Based on t h e model o f d i s l o c a t i o n damping due t o m o b i l e d e f e c t s a t t h e d i s l o c a t i o n l i n e it w a s c o n - c l u d e d t h a t t r a n s v e r s a l as w e l l a s l o n g i t u d i n a l m o t i o n o f oxygen w i l l c o n t r i b u t e t o P O .

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and UltrasonicAttenuatim in

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/7/

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/ 1 4 / J . C . ~ ; R e v . S c i S c i ~ . V o l . 3 2 , P t r . 3 , 1%1,335 /15/R.R .Hasiguti; Journal.Zess .Can.Metals, 28,1972,249 /Ib/S.Okuda.R.R.Hasiguti;Acta Mt.Vo1.11,1%3,257 /17/M.Koi~a,R.R.ksiguti;Acta Elet.Vo1.11,1%3,1215

/18/F.P.k,G.Sokol& ,K.IiXh; J d de Pnysique C5,1981,241 /19/W.J.Baxter,J.lrtilks;Acta kt.Vo1.10,1%2,175

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