Internal friction measurements in iron-nickel-carbon alloys
Citation for published version (APA):
Klostermann, J. A., Laan, van der, J. G., & Willemse, P. F. (1973). Internal friction measurements in
iron-nickel-carbon alloys. Scripta Metallurgica, 7(1), 81-88. https://doi.org/10.1016/0036-9748(73)90186-5
DOI:
10.1016/0036-9748(73)90186-5
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Published: 01/01/1973
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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 IN I R O N - N I C K E L - C A R B O N A L L O Y S J.G. v a n der L a a n , P.F. W i l l e m s e a n d J.A. K l o s t e r m a n n U n i v e r s i t y of T e c h n o l o g y T w e n t e , E n s c h e d e , the N e t h e r l a n d s ( R e c e i v e d N o v e m b e r 8, 1 9 7 2 ) I n t r o d u c t i o n In b . c . c . i r o n w i t h low c a r b o n c o n t e n t , a " S n o e k - p e a k " can be f o u n d by 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 as a r e s u l t of s t r e s s - i n d u c e d d i f f u s i o n of i n t e r s t i t i a l c a r b o n a t o m s in the o c t a h e d r a l s i t e s ( 1 ) . S c h e i l et a l . ( 2 ) a n d J a c k s o n et a l . ( 3 ) o b s e r v e d t h a t the a d d i t i o n of n i c k e l to the i r o n l o w e r s this p e a k ; and at a n i c k e l
c o n t e n t of ca. 15 w t . p c t the p e a k has d i s a p p e a r e d c o m p l e t e l y ( 3 ) .
At a t e m p e r a t u r e of ca. 2 0 0 ° C , h o w e v e r , a n o t h e r i n t e r n a l f r i c t i o n
p e a k has b e e n m e a s u r e d in this c a s e by S c h e i l ( 2 ) and F o r s t e r ( 4 ) .
S i m i l a r o b s e r v a t i o n s , i.e. the f a d i n g of the S n o e k - p e a k and
the o c c u r e n c e of a 2 0 0 ° C - p e a k , are d e s c r i b e d for m a r t e n s i t i c i r o n -
c a r b o n a l l o y s ( c a r b o n c o n t e n t 0 . 5 - 1 . 0 w t . p c t ) . A 2 0 0 ° C - p e a k has b e e n m e a s u r e d a l s o by K o s t e r et a l . ( 5 ) in l o w - c a r b o n s t e e l s a f t e r p l a s t i c d e f o r m a t i o n . It h a s b e e n s u g g e s t e d ( 2 , 3 ) t h a t the d e c r e a s e of the S n o e k - p e a k h e i g h t w i t h i n c r e a s i n g n i c k e l c o n t e n t m a y be due to: i. T h e i n t e r a c t i o n s of the c a r b o n a t o m s w i t h i m p e r f e c t i o n s in the m a r t e n s i t i c s t r u c t u r e or
2. the o r d e r i n g and s t a b i l i s a t i o n of the c a r b o n a t o m s r e s u l t i n g
in a t e t r a g o n a l d e f o r m a t i o n of the l a t t i c e d u r i n g the g a m m a -
a l p h a t r a n s f o r m a t i o n .
T h e 2 0 0 ° - p e a k is s u g g e s t e d to a r i s e f r o m the i n t e r a c t i o n
b e t w e e n the c a r b o n a t o m s and the d i s l o c a t i o n s w h i c h are p r e s e n t
in the m a r t e n s i t i c s t r u c t u r e ( 2 ) or are i n t r o d u c e d by p l a s t i c
d e f o r m a t i o n ( 5 ) .
82 I N T E R N A L F R I C T I O N IN F e - N i - C A L L O Y S Vol. 7, No. I The a b o v e m e n t i o n e d i n t e r a c t i o n b e t w e e n d i s l o c a t i o n s and c a r b o n atoms c o u l d be the r e s u l t of C o t t r e l l - a n d / o r S n o e k l o c k i n g p r o p o s e d by C o t t r e l l ( 6 ) and S c h o e c k and S e e g e r ( 7 ) r e s p e c t i v e l y . P l a s t i c d e f o r m a t i o n of F e N i C a l l o y s w o u l d c a u s e then an un- l o c k i n g of d i s l o c a t i o n s f r o m the C o t t r e l l c l o u d s i n c r e a s i n g the a m o u n t of free i n t e r s t i t i a l c a r b o n . This s h o u l d r e s u l t in a r e t u r n of the S n o e k - p e a k .
It is the o b j e c t of the p r e s e n t i n v e s t i g a t i o n to s t u d y this p h e n o m e n o n and the p o s s i b l e d e c r e a s e w i t h time of the S n o e k - p e a k due to d i f f u s i o n of the i n t e r s t i t i a l c a r b o n t o w a r d the d i s l o c a t i o n s . Also the l a t t e r e f f e c t c o u l d give some i n f o r m a t i o n on the d i s l o c a t i o n d e n s i t y of F e N i C m a r t e n s i t e ( 8 ) .
E x p e r i m e n t a l p r o c e d u r e
The c o m p o s i t i o n of the F e N i C a l l o y s u s e d in this i n v e s t i g a t i o n are g i v e n in t a b l e I.
T A B L E I
The c o m p o s i t i o n of the u s e d s a m p l e s .
prep. %Ni %C %Fe
I ]6.1 0.05 b a l a n c e 2 25.0 0.05 b a l a n c e 3 28.9 0.05 b a l a n c e 4 3].5 0.05 b a l a n c e in w t . p c t . The s p e c i m e n s w e r e p r o d u c e d by a r g o n arc m e l t i n g of h i g h p u r i t y i r o n ( 9 9 . 9 9 8 pct) and n l c k e l ( 9 9 . 9 9 9 pct) w i t h a d d i t i o n of e u t e c t o i d a l iron carbon. The as cast s a m p l e s w e r e h o m o g e n i s e d for 170 hr at ll50°C and s u b s e q u e n t l y d r a w n into w i r e of 0.61 m m d i a m e t e r and 165 m m l e n g t h .
The d a m p i n g m e a s u r e m e n t s w e r e p e r f o r m e d in a K ~ - t y p e ( 9 ) t o r s i o n p e n d u l u m d e s c r i b e d e l s w e r e ( 1 0 ) . The d a m p i n g was m e a s u r e d at a f r e q u e n c y
of ] Hz. The m a x i m u m e l a s t i c s t r a i n at the s u r f a c e of the s p e c i m e n
-6
was I0
R e s u l t s
The r e s u l t s of the d a m p i n g m e a s u r e m e n t s of the F e N i C - a l l o y s w i t h 16.1; 25; 28.9 and 31.5 w t . p c t Ni resp. a f t e r h e a t i n g at
900°C d u r i n g 5 min. in p u r i f i e d A r g o n a t m o s p h e r e and q u e n c h i n g in liquid N 2 are s h o w n in fig. 1 (mean time of the m e a s u r e m e n t s a f t e r q u e n c h i n g I hr). JD z 140~-
12o~
i
8o~ 6O 40 12°tl '
2O • F e 16,11~ Q 0 5 C v F e 2 ~ N , o o r o C o F e 2 9 N ~ X ~ S C • F e 3 1 . , 5 ~ Q 0 5 C I , I , t J I 30 40 50 60 TEMPERATURE.°C FIG. 1 I n t e r n a l f r i c t i o n v.s. t e m p e r a t u r e of v a r i o u s i r o n - n i c k e l c a r b o n a l l o y s l hr a f t e r q u e n c h i n g from the g a m m a p h a s e ( 9 0 0 ° C ) in l i q u i d N 2 ( - 1 9 6 ° C )This f i g u r e i n d i c a t e s that the a l l o y s w i t h ]6.1 and 25 w t . p c t Ni do not e x h i b i t a S n o e k - p e a k , w h i c h a g r e e s w i t h p r e v i o u s i n v e s t i g a t i o n s
(2,3). The a l l o y s w i t h 29 and 31.5 w t . p c t Ni, h o w e v e r , s h o w a small d a m p i n g p e a k at a b o u t 4 0 ° C
It is a l s o e v i d e n t f r o m f i g u T e ] that there is a large d i f f e r e n c e in i n t e r n a l f r i c t i o n level b e t w e e n the a l l o y s w i t h 16 and 25 w t . p c t Ni.
The S n o e k - p e a k o b s e r v e d in the 29 and 31.5 pct Ni a l l o y s d e c r e a s e s w i t h time as s h o w n in f i g u r e 2.
84 I N T E R N A L F R I C T I O N IN F e - N i - C A L L O Y S Vol. 7, No. i 7O Z .=. Z 4o 3C 2C 10 • Fe2gNiO.05C o FO31.SN ~0.O5C
2'0
5'o
TIME,MINUTES FIG. 2 The p a t h of the i n t e r n a l f r i c t i o n p e a k h e i g h t at 37°C m e a s u r e d v.s. time for F e 2 9 N i 0 , 0 5 C and F e 3 1 . 5 N i 0 , 0 5 C a f t e r q u e n c h i n g ( f i n i s h q u e n c h i n g is t = 0)A f t e r the d i s a p p e a r a n c e of the S n o e k - p e a k in t h e s e a l l o y s , the w i r e was l o a d e d "in s i t u " w i t h a t e n s i l e s t r e s s of 30 k g / m m 2,
r e s u l t i n g in a d e f o r m a t i o n of a b o u t 0 . 0 3 pct. Due to this d e f o r m a t i o n the S n o e k - p e a k r e a p p e a r e d in b o t h a l l o y s , b u t d i s a p p e a r e d a g a i n a f t e r some time, as i l l u s t r a t e d in f i g u r e 3 for the 29 w t . p c t Ni alloy.
8O = 7 0 ~ 6o 50 4 0 I = I , I , I , I 20 30 40 50 60 TEMPERATURE , °C FIG. 3 I n t e r n a l f r i c t i o n v.s. t e m p e r a t u r e for F e 2 9 N i 0 , 0 5 C a f t e r a t e n s i l e s t r e s s of 30 kg/ 2 m m at d i f f e r e n t times a f t e r s t r a i n i n g .
The d e c r e a s e of the p e a k h e i g h t w i t h time a f t e r s t r a i n i n g at 37°C is s h o w n in fig. 4.
Jo z 70 60 .=F.
==
~- 4C Z 3C 2C 1C • Fe 29Ni 0.05C o Fe 31.5N= 0.0,~C0
2'o 3'o ,'0
50 I 60 J 70 TIMEMINUTES FIG. 4 I n t e r n a l f r i c t i o n v.s. time at 37°C ( m a x i m u m p e a k h e i g h t ) a f t e r a t e n s i l e s t r e s s of 30 k g / m m 2 at t = 0The e f f e c t of t e m p e r i n g is s h o w n in fig. 5 for the 25 w t . p c t Ni alloy. In this alloy, w h i c h does not s h o w a S n o e k - p e a k a f t e r a n n e a l i n g and q u e n c h i n g , a d a m p i n g p e a k is p r o d u c e d by t e m p e r i n g for ~hr at 4 0 0 ° C and q u e n c h i n g in l i q u i d N 2. S i m i l a r to the p e a k s p r o d u c e d by d e f o r m a t i o n , also this p e a k d i s a p p e a r s a f t e r s o m e time.
~ 8 0 Fe25 N, 0.05C • H R o 2 HRS )afte quencr~ng 70~-
50"
°i
__ 60
I ~ o o o - _ _ o 4 o i ° 20 30 40 50 6 0 TEMPE RATURE, ° C FIG. 5 I n t e r n a l f r i c t i o n v.s. t e m p e - r a t u r e a f t e r a n n e a l i n g d u r i n g ~hr at 4 0 0 ° C and q u e n c h i n g in l i q u i d N 2 for d i f f e r e n t a g i n g t i m e s ( a g i n g d u r i n g S n o e k - p e a k m e a s u r e m e n t s . )86 I N T E R N A L F R I C T I O N IN F e - N i - C A L L O Y S Vol. 7, No. I
D i s c u s s i o n
The p e a k s o b s e r v e d at ca. 40°C a f t e r q u e n c h i n g a n d / o r d e f o r m a t i o n in 29 and 31.5 w t . p c t Ni a l l o y s (figs. l and 3) and in 25 w t . p c t Ni a f t e r t e m p e r i n g at 4 0 0 ° C (in fig. 5) s t r o n g l y s u g g e s t S n o e k - r e l a x a t i o n due to free i n t e r s t i t i a l c a r b o n . The a b s e n c e of such a p e a k in 16 and 25 w t . p c t Ni a l l o y s a f t e r q u e n c h i n g , c o u l d be the r e s u l t of:
I. A h i g h d i s l o c a t i o n d e n s i t y in the m a s s i v e m a r t e n s i t e phase, l o c k i n g p r a c t i c a l l y all i n t e r s t i t i a l s by C o t t r e l l - a n d / o r S n o e k - l o c k i n g . If this s u p p o s i t i o n is true then the 29 and 3|.5 w t . p c t Ni a 1 1 o y s s h o u l d p o s s e s s a lower d i s l o c a t i o n d e n s i t y . This seems not u n l i k e l y b e c a u s e at 28-30 w t . p c t Ni a t r a n s i t i o n o c c u r s f r o m m a s s i v e to a c i c u l a r m a r t e n s i t e . This t r a n s i t i o n is a c c o m p a n i e d by a c h a n g e in the m o d e of the s e c o n d s h e a r f r o m slip to t w i n n i n g ( l l ) .
2. The o t h e r p o s s i b l e e x p l a n a t i o n g i v e n by J a c k s o n et al(3) that the r a p i d l y f o r m e d m a s s i v e m a r t e n s i t e is t e t r a g o n a l due to t r a n s f o r m a - tion o r d e r i n g of c a r b o n a t o m s , is less l i k e l y , b e c a u s e a c c o r d i n g to Z e n e r ( 1 2 ) the c a r b o n will be r a n d o m l y d i s t r i b u t e d at this low c a r b o n c o n t e n t and the o b s e r v e d M s - t e m p e r a t u r e s .
3. F i n a l l y the d i f f e r e n t r a d i i of the iron and n i c k e l atoms c o u l d c a u s e d i f f e r e n c e s in the sizes of the o c t a h e d r a l sites; c o n s e q u e n t l y r e s u l t i n g in a s t a b i l i s a t i o n of the i n t e r s t i t i a l atoms, w h i c h also c o n t r i b u t e s to the o b s e r v e d d e c r e a s e of the p e a k w i t h i n c r e a s i n g n i c k e l c o n t e n t .
In our o p i n i o n the first e x p l a n a t i o n for lack of f u r t h e r e v i d e n c e s seems to be the m o s t likely.
The d e c r e a s e in p e a k h e i g h t w i t h time could then be c a u s e d by d i f f u s i o n of c a r b o n atoms t o w a r d s d i s l o c a t i o n s . T h i s d e c r e a s e o p e n s the p o s s i b i l i t y to e s t i m a t e the d i s l o c a t i o n d e n s i t y a c c o r d i n g to the t h e o r y of H a r p e r ( 8 ) . H a r p e r s h o w e d that d u r i n g s t r a i n a g i n g of b . c . c . iron a m i g r a t i o n of c a r b o n a t o m s to d i s l o c a t i o n s may be d e t e c t e d by d a m p i n g m e a s u r e m e n t s . The d e c r e a s e of the p e a k is g i v e n by:
t
= exp. { - 2 L ( ~ H ) I/3/
(ADt/kT) 2/3}w h e r e Qo and Qt are the v a l u e s of the m a x i m u m of the i n t e r n a l
f r i c t i o n p e a k s m i n u s the b a c k g r o u n d at the b e g i n n i n g of a g i n g and
a f t e r an a g i n g t i m e t r e s p e c t i v e l y , L is the u n k n o w n d i s l o c a t i o n d e n s i t y , A is the p a r a m e t e r in the r e l a t i o n : U = A f ( r , ~ ) w h i c h d e s c r i b e s the i n t e r a c t i o n e n e r g y b e t w e e n a d i s l o c a t i o n and an i n t e r s t i t i a l a t o m as a f u n c t i o n of the p o s i t i o n of the a t o m , D is the d i f f u s i o n c o e f f i c i e n t at the a b s o l u t e t e m p e r a t u r e T, K the B o l t z m a n n ' s c o n s t a n t . U s i n g this e q u a t i o n a n d the a b o v e m e n t i o n e d v a l u e s (8) we h a v e c a l c u l a t e d f r o m the c u r v e s in fig. 4 a d i s l o c a t i o n d e n s i t y of a b o u t Ii II -2
7. ~0 and 4 . 1 0 l i n e s cm for the 29 a n d 3 1 . 5 pct Ni a l l o y s
r e s p e c t i v e l y . T h i s v a l u e is s o m e w h a t h i g h e r t h a n f o u n d in e l e c t r o n t r a n s m i s s i o n o b s e r v a t i o n s ( 1 3 , | 4 ) . It is h o w e v e r k n o w n t h a t the d i s l o c a t i o n d e n s i t y d e t e r m i n e d by t h i n f i l m e l e c t r o n m i c r o s c o p y ~s l o w e r t h a n t h o s e m e a s u r e d by o t h e r m e t h o d s ( | 5 , 1 6 ) . A f u r t h e r i n v e s t i g a t i o n of this p r o b l e m is b e i n g c a r r i e d out. The r e s u l t s w i l l be p u b l i s h e d in due c o u r s e . C o n c l u s i o n s In m a r t e n s i t e F e - N i - C a l l o y s w i t h 0 . 0 5 w t . p c t C and 25; 29 and 31.5 w t . p c t Ni a S n o e k - p e a k has b e e n f o u n d . T h e p e a k d i s a p p e a r s w i t h t i m e b u t can be m e a s u r e d a g a i n a f t e r t e m p e r i n g (25 w t . p c t ) or d e f o r m a t i o n (29; 3 1 . 5 w t . p c t ) .
T h e d i s a p p e a r a n c e c o u l d be due to the d i f f u s i o n of the i n t e r s t i t i a l
C a t o m s t o w a r d d i s l o c a t i o n s by w h i c h t h e y are l o c k e d . T h e d e c r e a s e of the p e a k h e i g h t w i t h t i m e m i g h t p r o v i d e a m e a n s to e s t i m a t e the d i s l o c a t i o n d e n s i t y . A c k n o w l e d g e m e n t T h e a u t h o r s w o u l d l i k e to t h a n k P r o f . d r . i r . C . A . V e r b r a a k for c r i t i c i z i n g the m a n u s c r i p t a n d h e l p f u l d i s e u s s i o n s a n d M r . A . M . N i j s s e n for e x p e r i m e n t a l a s s i s t a n c e .
88 I N T E R N A L F R I C T I O N IN F e - N i - C A L L O Y S Vol. 7, No. i
R E F E R E N C E S .
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