HIGH TEMPERATURE INTERNAL FRICTION OF Ni-20 wt% Cr

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HIGH TEMPERATURE INTERNAL FRICTION OF Ni-20 wt% Cr

R. Schaller, Jérôme Ammann, F. Cosandey

To cite this version:

R. Schaller, Jérôme Ammann, F. Cosandey. HIGH TEMPERATURE INTERNAL FRIC- TION OF Ni-20 wt% Cr. Journal de Physique Colloques, 1987, 48 (C8), pp.C8-451-C8-456.

�10.1051/jphyscol:1987869�. �jpa-00227173�

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JOURNAL DE PHYSIQUE

Colloque C8, supplement au n012, Tome 48, dbcembre 1987

HIGH TEMPERATURE INTERNAL FRICTION OF Ni-20 wt% Ct

R. SCHALLER, J. J

.

^AMMANN^and F. COSANDEY'

Institut de Gdnie Atomique, Ecole Polytechnique FedBrale de Lausanne, cH-1015 Lausanne, Switzerland

he

State University of New Jersey, RUTGERS, Department of Mechanics and Materials Science, PO Box 909, Piscataway, NJ 08854, USA

Rdsumd

-

Le spectre de frottement intkrieur haute temperature des alliages Ni-Cr 20% est essentiellement caracteris6 par un pic de relaxation (A lOOC K, 1 Hz) superposk

A

une montee exponentielle du fond avec la temperature. Un phenomgne dthyst6;&se rkversible apparaPt sur le pic entre 1.es courbes obtenues

A

la mcntee et

A

la descente en temperature. Ce'te hystergse est b e a u c o ~ p plus forte pour les dchantillons contenant 180 ppm Ce. Dans ce cas, on observe de forts accroissements du frottement interieur iu-dessus de la temperature du pic, qui peuvent Btre corr8lds

A

une 2ugmentation de la ductilite

A

haute tempkrature des alliages Ni-Cr, sous l'effet d'adjonctions de Ce.

Abstract - The high temperature internal friction spectrum of Ni-20 wt% Cr alloys is mainly characterized by a relevetion peak (at 1000 K for 1 Hz) superimposed to a backg:round increasing expor~entfally with the temperature. A reversible hysteresis appears in the peak temperature range between the curves measured upon heating anC upon cooling. This hysteresis is much stronger in specimens containing 180 at ppm Ce. In this case, strong increases of the internal frictjon are observed at temperatures higher than the peak one. The high i~lternal.

friction value mezsured upon cooling can be correlated with an increase of the high teniperature ductility in Ni-Cr alloys, which is due to Ce additions.

INTRODJCTION

Ni-Cr alloys are refractory materials exhibiting good mechanical properties at high temperature. Though, a decrease of ductility is observed above 500 OC in polycristalline specimens (fig. I), which may be associated with an embrittlement mechanism at the grain boundaries.

More precisely, grain boundary sliding, which can be activated at high temperature, may lead to voids and cracks formation at second phase particles, grain boundary ledges and triple points..

There is now clear evidence indicating that the intergranular mode of fracture by cavitation is governed primarily by the presence of deleterious trace elements such as S [1,2]. On the other hand, in Ni- Cr, trace additions of Ce lead to the restauration of ductility at high temperature (fig. 1). For alloys without Ce, the high temperature ductility is low and the fracture mode is intergranular [3]. As the Ce content increases, the fracture path reverts from intergranular to transgranular.

In order to understand the role played by Ce on the mechanical properties of Ni-Cr alloys, internal friction measurements have been

Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1987869

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C8-452 JOURNAL

DE

PHYSIQUE

p e r f o r m e d on t w o t y p e s o f Ni-20 wt% Cr a l l o y s c o n t a i n i n g r e s p e c t i v e l y 0 a n d 180 a t . ppln Ce

.

E X P E R I M E N T A L

The a l l o y s (Ni-20 w t % C r a n d Ni-20 w t % Cr-180 a t ppm C e ) w e r e p r e p a r e d by vacuum i n d u c t i o n m e l t i n g f o l l o w e d by c a s t i n g a n d h o t r o l l i n g . Ce was a d d e d t o t h e m e l t b y a d d i n g s m a l l amounts o f a Ni-15 w t % Ce a l l o y [ 4 ] . T h i n b a r s p e c i m e n s 1 1 0 x 2 . 5 x 0 . 5 mm3 w e r e m a c h i n e d f r o m c o l d r o l l e d a n d h e a t t r e a t e d b a r s . A f t e r m a c h i n i n g , t h e s a m p l e s w e r e vacuum a n n e a l e d a t 1100 OC i n o r d e r t o o b t a i n s i m i l a r g r a i n s i z e s ( - 80 pm) f o r b o t h a l l o y s . F i n a l l y , a n a g e i n g o f 24 h r s a t 8 0 0 O C u n d e r vacuum was r e a l i z e d , i n o r d e r t o s t a b i l i z e d t h e m i c r o s t r u c t u r e . I n t e r n a l f r i c t i o n m e a s u r e m e n t s h a v e b e e n p e r f o r m e d a t low f r e q u e n c y i n a c l a s s i c a l t o r s i o n pendclum f r o m room t e m p e r a t u r e u p t o 1000°C u n d e r vacuum ( - 10-5 t o r r )

.

S t r a i n a m p l i t u d e was 5 . 1 0 - 6 , a n d h e a t i n g o r c o o l i n g r a t e s 2 K/min. I n t e r n a l f r i c t i o n was d e d u c e d f r o m t h e wave f o r m a n a l y s i s o f t h e f r e e d e c a y s i g n a l [ 5 ]

.

R E S U L T S

D u r i n g t h e f i r s t h e a t i n g , t h e i n t e r n a l f r i c t i o n o f Ni-20 w t % C r i n c r e a s e s r a p i d l y w i t h t h e t e m p e r a t u r e a b o v e 850 K a n d r e a c h e s a r a t h e r h i g h l e v e l a t 1000 K ( - 3.10-2) ( f i g . 2 ) .

F i g . 1. U l t i m a t e e l o n g a t i o n o f F f g . 2 . I n t e r n a l f r i c t i o n a n d Ni-20 w t % C r a l l o y s , d i f f e r i n g v i b r a t i o n a l f r e q u e n c y o f N i - from o n e a n o t h e r by t h e Ce con- 20 w t % Cr

c e n t r a t i o n , a s a f u n c t i o n o f t e m - a ) F i r s t h e a t i n g a t 2 K/mn

p e r a t u r e . N o t e t h e d u c t i l i t y b ) S u b s e q u e n t c o o l i n g down a f t e r d e c r e a s e a b o v e 500 OC. o n e h o u r a n n e a l i n g a t 1300 K .

A f t e r o n e h o u r a n n e a l i n g a t 1300 K, t h e i n t e r n a l f r i c t i o n m e a s u r e d d u r i n g c o o l i n g i s l o w e r a n d t h e v i b r a t i o n a l f r e q u e n c y i s h i g h e r t h a n d u r i n g p r e c e d e n t h e a t i n g . T h i s g i v e s a n a c c o u n t f o r a h a r d e n i n g p r o c e s s d u e t o t h e a n n e a l i n g ; f o r i n s t a n c e , d i s l o c a t i o n p i n n i n g b y p o i n t d e f e c t s .

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After this first temperature run, the internal friction spectrum is rather stable. It is mainly composed of a relaxation peak located at

1 0 0 0

K (frequency -

¹

Hz) and superimposed to an exponential increase of the background with the temperature (fig. 3).

Fig 3.Internal friction

1.00

spectrum of Ni-20wt% Cr

a)

heating (2 K/mn) b) cooling (2 K/mn)

. 9 5

2 0 . 0 - ' x l 0=

-

F ( H z )

1 5 . 0 -

Fig. 4. Internal friction

1 0 . 0 -

spectrum of Ni-20wt%

Cr + 180

at. ppm Ce

' I

a) heating (2 K/mn)

5.0

b) cooling

( 2

K/mn)

0 . 0

In addition, an hysteresis appears between the curves measured during

the increases and decreases of temperature. The peak observed during

cooling is higher than during the previous heating. This hysteresis is

characteristic of a structural evolution between heating and cooling

cycles. It is important to note that this hysteresis is fully

reproducible upon repeated heating and cooling cycles, which indicates

that this evolution is stable and reversible.

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T h i s h y s t e r e s i s i s e v e n more p r o n o u n c e d f o r t h e a l l o y s w i t h

F ' H z ' 1 8 0 ppm Ce a s d e p i c t e d i n

1'""

F i g . 4 . Upon h e a t i n g , t h e i n -

t e r n a l f r i c t i o n s p e c t r u m i s

1 . 2 5

q u i t e s i m i l a r t o t h e o n e o b s e r v e d i n p u r e Ni-20 w t % C r .

1 . 2 0 Upon c o o l i n g .however, a v e r y

h i g h p e a k a p p e a r s a t a tem- p e r a t u r e a b o u t 1 0 0 K h i g h e r t h a n t h a t o f t h e p e a k m e a s u r e d u p o n h e a t i n g . B u t , i f t h e

1 . 1 8

1300 r e l a x a t i o n p e a k i s a l w a y s o b s e r v a b l e d u r i n g h e a t i n g , a p e a k d o e s n o t a l w a y s a p p e a r Fig. 5. Internal f r i c t i o n hysteresis upon c o o l i n g . S o m e t i m e s , o n e i n Ni-20 w t % Cr

+

180 a t . ppn Ce. o b s e r v e s o n l y a h i g h i n t e r n a l f r i c t i o n b a c k g r o u n d d u r i n g c o o l i n g ( f i g . 5 )

.

I n t h i s c a s e , t h e p e a k h a s c o m p l e t e l y v a n i s h e d o r i s b u r i e d w i t h i n t h e l a r g e b a c k g r o u n d . . As b e f o r e , t h e s p e c t r a o b s e r v e d d u r i n g h e a t i n g a n d c o o l i n g a r e f u l l y r e p r o d u c i b l e upon r e p e a t e d h e a t i n g and c o o l i n g c y c l e s i n d i , c a t i v e o f a n e q u i l i b r i u m s t r u c t u r a l c h a n g e s i m i l a r t o a p h a s e t r a n s f o r m a t i o n . The t r a n s i t i o n t e m p e r a t u r e b e t w e e n t h e t w o s t a t e s c o r r e s p o n d s t o t h e p o i n t a t w h i c h h y s t e r e s i s b e t w e e n h e a t i n g a n d c o o l i n g occur;.

DISCUSSION

The i n t e r n a l f r i c t i o n peak a p p e a r s i n t h e same t e m p e r a t u r e r a n g e where t h e d u c t i l i t y o f Ni-20 w t % C r d e c r e a s e s ( f i g . 1 a n d 3 ) . So, it i s p o s s i b l e t o assume t h a t t h e a n e l a s t i c r e l a x a t i o n which i s r e s p o n s i b l e f o r t h e p e a k , i s c e r t a i n l y a s s o c i a t e d w i t h t h e p l a s t i c p r o p e r t i e s e x h i b i t e d b y t h i s a l l o y i n t h i s t e m p e r a t u r e domain.

A s i m i l a r peak h a s been o b s e r v e d by G r i d n e v a n d co-workers [6] _{i n}N i - 3 . 2 , 11 a n d 1 9 . 5 w t % C r a l l o y s . These a u t h o r s i n t e r p r e t e d t h e peak a s due t o g r a i n b o u n d a r y r e l a x a t i o n , t h e d r a g g i n g f o r c e b e i n g due t o t h e p r e s e n c e o f C r atoms a t t h e g r a i n b o u n d a r i e s . A s t h e y d i d n o t measure t h e i n t e r n a l f r i c t i o n d u r i n g c o o l i n g , t h e y d i d n o t o b s e r v e a n h y s t e r e s i s a s s o c i a t e d w i t h t h e p e a k .

But, on t h e o t h e r hand, an h y s t e r e s i s phenomenon s i m i l a r t o t h e one p r e s e n t e d on f i g . 4 , was o b s e r v e d i n Fe-3% S i - 0 . 0 1 8 % Sb a l l o y s by I w a s a k i a n d F u j i m o t o [ 7 ] . But, p u r e Fe-3% S i a l l o y s do n o t e x h i b i t an h y s t e r e s i s . H y s t e r e s i s was t h e n a t t r i b u t e d t o t h e s e g r e g a t i o n of Sb a t g r a i n b o u n d a r i e s . T h i s s e g r e g a t i o n l e a d s t o t h e m a t e r i a l e m b r i t t l e m e n t c h a r a c t e r i z e d by i n t e r g r a n u l a r f r a c t u r e . I n t h i s c a s e , t h e i n t e r n a l f r i c t i o n peak i s s m a l l . On t h e c o n t r a r y , p u r e Fe-3% S i e x h i b i t a l a r g e peak and t h e f r a c t u r e i s t r a n s g r a n u l a r .

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I t i s p o s s i b l e t o a n a l y z e t h e Ni-Cr r e s u l t s i n a s i m i l a r way. F i r s t , a s f o r t h e m e c h a n i c a l p r o p e r t i e s ( d u c t i l i t y ) , t h e 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 s d i f f e r e n t i n a l l o y s w i t h a n d w i t h o u t Ce ( f i g . 3 a n d 4 ) . The mechanisms, w h i c h a r e r e s p o n s i b l e f o r t h e h i g h t e m p e r a t u r e i n t e r n a l f r i c t i o n , a r e t h e n c e r t a i n l y a s s o c i a t e d w i t h t h e m e c h a n i s m s w h i c h a r e r e s p o n s i b l e f o r t h e m e c h a n i c a l p r o p e r t i e s . P h e n o m e n o l o g i c a l l y , it i s p o s s i b l e t o n o t e t h a t t h e r a t h e r low l e v e l o f t h e i n t e r n a l f r i c t i o n p e a k i i ~ p u r e N i - C r i s c o r r e l a t e d w i t h t h e d e c r e a s e o f d u c t i l i t y a b o v e 5 0 0 ^{O S} ( f i g . 1 ) . On t h e o t h e r hand, t h e h i g h p e a k o r h i g h l e v e l o f t h e b a c k c z o u n d , c r e a t e d upon h e a t i n g a n d o b s e r v e d upon c o o l i n g i n t h e Ce c o n t a i n i n g a l l o y s , a r e a s s o c i a t e d w i t h t h e d u c t i l i t y r e c o v e r y . From a r u p t u r e v i e w p o i n t , a low l e v e l o f i n t e r n a l f r i c t i o n g i v e s a n a c c o u n t f o r I n t e r q r a n u l a r f r a c t u r e , a n d a h i g h l e v e l f o r t r a n s g r a n u l a r f r a c t u r e . I t i s t h e n p o s s i b l e t o c o r r e l a t e t h e a n e l a s t i c b e h a v i o u r o f N i - C r a l l o y s w i t h t h e s e modes o f f r a c t u r e .

The r h e o l o g i c a l d e s c r i p t i o n o f a n i n t e r n a l f r i c t i o n p e a k r e q u i r e s a n a p p l i e d s t r e s s , l e a d i n g t o t h e m o t i o n o f t h e s t r u c t u r a l d e f e c t , p l u s a d r a g g i n g a n d a r e s t o r i n g f o r c e o p p o s e d t o t h e i n i t i a l a p p l i e d s t r e s s . The p r e s e n c e o f a r e s t o r i n g f o r c e i s e s s e n t i a l t o t h e r e c o v e r a b l e n a t u r e o f t h e r e l a x a t i o n . I n t h e a b s e n c e o f a r e s t o r i n g f o r c e , a p u r e v i s c o u s b e h a v i o u r i s o b s e r v e d l e a d i n g t o a n e x p o n e n t i a l i n c r e a s e o f t h e i n t e r n a l f r i c t i o n w i t h t e m p e r a t u r e . A d m i t t i n g t h a t t h e h i g h t e m p e r a t u r e i n t e r n a l f r i c t i o n o f Ni-Cr i s d u e t o g r a i n b o u n d a r y r e l a x a t i o n , it i s p o s s i b l e t o a t t r i b u t e t h e o r i g i n o f t h e r e s t o r i n g f o r c e e i t h e r t o t h e o t h e r g r a i n s o r t o p r e c i p i t a t e s o r v o i d s , w h i c h h a v e grown o n t h e g r a i n b o u n d a r i e s . I n t h e l a t t e r c a s e , t h e r e s t o r i n g f o r c e w i l l i n c r e a s e i f t h e number a n d / o r t h e s i z e o f t h e p i n n i n g p o i n t s ( p r e c i p i t a t e s o r v o i d s ) i n c r e a s e s . C o n s e q u e n t l y , t h e r e l a x a t i o n p e a k w i l l d e c r e a s e . On t h e o t h e r h a n d , t h e d i s a p p e a r a n c e o f some p i n n i n g p o i n t s w i l l l e a d t o a n i n c r e a s e a n d a s h i f t t o w a r d s h i g h e r t e m p e r a t u r e o f t h e i n t e r n a l f r i c t i o n p e a k (see f i g . 4 )

.

I n t h e c a s e o f Ni-20 w t % C r , a r e s t o r i n g f o r c e c a n b e c r e a t e d b y C r p r e c i p i t a t i o n o r v o i d f o r m a t i o n 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 u n a n d a n n e a l i n g a t 1300 K ( f i g . 2 ) . When t h e r e l a x a t i o n p e a k i s s t a b i l i z e d ( f i g . 3), t h e p i n n i n g p o i n t s on t h e g r a i n b o u n d a r i e s c a n l e a d t o v o i d a n d c r a c k f o r m a t i o n d u r i n c p l a s t i c d e f o r m a t i o n . C o n s e q u e n t l y , i n t e r g r a n u l a r f r a c t u r e o c c u r s l s a d i n g t o a d e c r e a s e o f d u c t i l i t y .

On t h e o t h e r hand, a l l o y s c o n t a i n i n g Ce a d d i t i o n s e x h i b i t a r e l a x a t i o n p e a k w h i c h i s n o t s t a b l e w i t h r e s p e c t t o h e a t i n g a n d c o o l i n g c y c l e s . A n n e a l i n g a t t e m p e r a t u r e s h i g h e r t h a n t h e p e a k t e m p e r a t u r e , l e a d t o a s t r o n g i n t e r n a l f r i c t i o n i n c r e a s e . T h i s g i v e s a n a c c o u n t f o r a d e c r e a s e o f t h e r e s t o r i n g f o r c e , f o r e x a m p l e by p i n n i n g p o i n t s d i s s o l u t i o n . The d i s a p p e a r a n c e o f p i n n i n g p o i n t s r e d u c e s t h e n u c l e a t i o n o f c a v i t i e s a t t h e g r a i n b o u n d a r i e s . C o n s e q u e n t l y , t h e f r a c t u r e p a t h r e v e r t s f r o m i n t e r g r a n u l a r t o t r a n s g r a n u l a r .

The r e s t a u r a t i o n o f d u c t i l i t y i s t h e n c a u s e d by t h e p r e s e n c e o f C e w h i c h s e e m s t o d e s t a b i l i z e , a t h i g h t e m p e r a t u r e t h e p i n n i n g p o i n t s l o c a t e d a t g r a i n b o u n d a r i e s . The n a t u r e o f t h e s e p i n n i n g p o i n t s must b e s t i l l d e t e r m i n e d . The f i n a l r o l e o f Ce i s t o r e d u c e c a v i t a t i o n i n N i - C r . A s i m i l a r r o l e i s p l a y e d by Y i n t h e s u p e r p l a s t i c b e h a v i o u r o f A1203

[ a ] .

CONCLUSIONS

The h i g h t e m p e r a t u r e i n t e r n a l f r i c t i o n o f Ni-20 w t % C r a l l o y s e x h i b i t s a r e l a x a t i o n p e a k l o c a t e d i n a t e m p e r a t u r e r a n g e w h e r e a d e c r e a s e o f

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d u c t i l i t y i s observed. A d d i t i o n s o f C e ( 1 8 0 a t . p p m ) , w h i c h l e a d t o d u c t i l i t y r e c o v e r y , g i v e r i s e t o a s t r o n g h y s t e r e s i s i n t h e h i g h t e m p e r a t u r e i n t e r n a l f r i c t i o n . I f t h e p e a k i s a t t r i b u t e d t o g r a i n boundary s l i d i n g , t h e e f f e c t of C e m a y be t h e d e s t a b i l i z a t i o n o f t h e g r a i n b o u n d a r y p i n n i n g p o i n t s a t h i g h t e m p e r a t u r e . A s a c o n s e q u e n c e , i n t e r n a l f r i c t i o n i n c r e a s e s . T h e d u c t i l i t y increases t o o , because t h e p i n n i n g p o i n t s a r e no m o r e a c t i v e i n c a v i t y n u c l e a t i o n d u r i n g p l a s t i c d e f o r m a t i o n .

ACKNOWLEDGEMENTS

We t h a n k G . E . M a u r e r of S p e c i a l M e t a l C o r p o r a t i o n f o r c o n t r i b u t i o n of t h e a l l o y s . T h i s research i s s u p p o r t e d i n p a r t b y t h e N a t i o n a l Science F o u n d a t i o n u n d e r G r a n t s N S F - D M R - 8 4 - 0 6 6 0 5 a n d N S F - I N T - 8 5 - 1 5 3 2 1 .

REFERENCES

L O Z I N S K Y , M . G . , VOLKOGAN, G . M . , PORTSOVSKY, N . Z . , R u s s . M e t . 5 ( 1 9 6 7 ) 6 5 .

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