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INTERNAL FRICTION AND MAGNETIC AFTER
-EFFECTS IN Fe-V-N ALLOYS
J. Zgadzaj, J. Ilczuck, J. Morón
To cite this version:
JOURNAL DE P H Y S I Q U E
CoZZoque C 5 , supplhment au n020, Tome 42, octobre 1981 page C5-835
INTERNAL F R I C T I O N AND MAGNETIC AFTER
-
EFFECTS I N Fe-V-N ALLOYS J . Zgadzaj, J . I l c z u k and J . W . ~ o r o AI n s t i t u t e o f Physics and Chemistry o f Metals, Silesian University, 40-007
Katowice, 3ankowa 1 2 , Poland
A b s t r a c t . - I n t e r n a l f r i c t i o n and m a g n e t i c p c r m c a b i l i t y d i s a c c o - mmodation have been s t u d i e d f o r a dozen o r s o samples o f f o u r
d ~ e - ~ / 0 , 3 4 - 1 . 0 : $ / a l l o y s n i t r i d e d i n t h e ammonia atmosphere a t 673 K. The o b t a i n e d c u r v e s r e v e a l t h r e e d i s t i n c t bands o f mag- n e t i c a f t e r - e f f e c t /Ir,,U,C/ and a s m a l l peal< o f t h e Snoek r e l o - x a t i o n . Band A c o r r e s p o n d s t o t h e F a s t - E i e i J e r i n a r e l a x a t i o n and c o n s i s t s o f t h r e e e l e m e n t a r y p r o c e s s e s ~ i t h 6 ~ - % ~ - ~ * s . Band C i s i d e n t i c a l w i t h t h o r e l a x a t i o n d i s c o v e r e d i n 1973 by t h e K.H. J a c k g r o u p w h i l e band
B
h a s n o t been o b s e r v e d i n t h e l i t e r a t u r e t i l l now. 1. I n t r o d u c t i o n.-
M i g r a t i o n a l r e l a x a t i o n s i n F e - V alloys r e l a t e d t o t h e p r e s e n c e o f n i t r o g e n i n t h s s o l i d s o l u t i o n have many t i m e s been s t u d i e d s i n c e 1953[I]
by t h e i n t e r n a l f r i c t i o n / I F / method. The most i n t e r e s t i n g r e s u l t s have been r e f e r r e d i n [I-61.
I n samples n i t r i d c d a t 1223 K b e s i d e t h e Snoek r o l a x a t i o n a second h i g h p e a k has b e c n ob- s e r v e d / t h e i-1.i r e l a x a t i o n / 11-41.
N i t r i d i n g o f Fe-V samples a t 673t o 923 K l e a d s t o t h e appearance o f a t h i r d r e l a x a t i o n a l p r o c e s s a t y e t h i g h e r t e m p e r a t u r e s [ 5 , 6 ]
.
I n p a p e r [ 7 ] r e l a x a t i o n s i n n i t r i d e d Fe-V a l l o y s were i n v e i t i - s a t e d b y means o f m a o n e t i c p e r m e a b i l i t y d i s a c c o m m o d a t i o n /P;P3/ mea- s u r e m e n t s . I n t h e p r e s e n t p a p e r a r e compared r o s u l t s o b t a i n e d b y b o t h methcds-
I F and NPD.2. E x p e r i m e n t a l and i n v e s t i q a t c d samples.- I n t e r n a l f r i c t i o n has been measured b y means o f a n a c o u s t i c r c l a x o n c t e r [ 8 ]
.
k l a g n e t i c p o r m e a b i - l i t y d i s a c c ~ m n o d a t i o n has been measured o n a M a x w e l l - i i i e n a c b r i d g e .4
I s o c h r o n a l MPO c u r v e s d ( d ) - -
-
have been d e t e r m i n e d . I n t h e n u m e r i -x
-x(t,) X t t , ) c a l a n a l y s i s o f a l l t h e o b t a i n e d c u r v o s t h e l i n e a r s p e c t r u m o f r e l a - x a t i o n t i m e s as w e l l a s t h e :'iert-t:arx l a w have b e c n a p p l i e d . I n t h e case o f s e v e r a l r e l a x a t i o n s t h e EIPD c u r v e i s d e s c r i b e d b v t h e f o r n u - l a : (1) t h e i - t h r o l a - x a t i o n ; t h e l a t t e r v a l u e i s p r o p o r t i o n a l t o t h e c o n c e n t r a t i o n /ci/ o f t h e i - t h r e l a x a t o r , Because t h e h e i s h t o f e a c h r e l a x a t i o n peak / A ~ / i s p r o p o r t i o n a l t o 4 / y i,
t h e f o l l o w i n g f o r m u l a i s v a l i d :JOURNAL DE PHYSIQUE
Some 4 ~ e - v a l l o y s c o n t a i n i n g 0.34 t o 1
'%
vanadium have been s t u d i e d . A f t e r s t r e s s - r e l i e f a n n e a l i n g j 1 2 2 3 K f o r 1 0 h and 1073K
f o r 1.5 h/ on i s o c h r o n a l MPD and I F c u r v e s no r e l a x a t i o n a l p e e k s ha- ve a p p e a r e d / c u r v e a i n f i g . 2 / . Samples have b e e n n i t r i d e d a t 673 K i n t h e ammonia atmosphere and t h e n aged for 3 0 m i n a t h i g h e r and h i g - h e r t e m p e r a t u r e s . By means o f e l e c t r o n m i c r o s c o p y i t has b e e n shown
measurements have g i v e n one b r o a d peak /fig.2/. I n t h e r e g i o n o f B+C bands o n I F c u r v e s a w i d o peak h a s b e e n o b s e r v e d , v i s i b l y b r o a - dened form t h e B s i d e w h i l e MPD has a l w a y s s p l i t i t i n t o two s e p a r a - t e r e l a x a t i o n a l p r o c a s s e s .
Fia.3 .The dependence o f Q - ~ o n t e m p e r a t u r e f o r t h e Fe-V/0.34
%/
sample a f t o r n i t r i d i n g a t 673K
f o r 30 min; f r e q u e n c y f=
8 7 cps. I n f i g . 4 a r e shown a s an i n s t a n c e t h e r e s u l t s o f a n a l y s i s o f i s o c h r o n a l MPD c u r v e s o b t a i n e d f o r t h e Fe-V/0.34:;/
sample.b ~ (
%104x
120
-
Fiq.4. The r e s u l t o f ana-l y s i s o f t h e i s o c h r o n a l MPD c u r v e o b t a i n e d f o r t h e Fe-V/0.34
;;/
sample a f t e r n i t r i d i n g f o r 3 0 min. 240 280 320 360 LOO I n t h eF-M
r e g i o n t h r e e e l e m e n t a r y p r o c e s s e s /I,II,IIIhave bean / o b t a i n e d w i t h a c t i v a t i o n e n e r g i e sQI
=
0.87 ev,eII
= 0.94 eV,Q I I
I
-
0.99 eV, f o r00
t h e v a l u e 4 . 5 - 1 0 - l 5 s 191 h a s been assumed. F o r e x p e r i m e n t a l p e a k s B and C two e l e m e n t a r y p r o c e s s e s have been o b t a i n e d f o r e a c h o f t h e n . However, i t s h o u l d be n o t i c e d t h a ti n
t h e case o f t h e s e p e a k s a c o n t i n u o u s s p e c t r u m s h o u l d r a t h e r be a p p l i e d i i t r e s u l t s f r o m p r o p o s e d i n t h e l i t e r a t u r e mechanisms g i v i n g r i s e t o t h e s e r e l a x a t i o n s / s e c t i o n 4/. I s o c h r o n a l a g e i n g o f n i t r i d e d Fe-V samples i n t h e r a n g e 673-
1173 K r e s u l t e d i n t h e d e c a y o f t h e Snoek r e l a x a t i o n / p r o c e s sO/
JOURNAL DE PHYSIQUE
a n d poaks A/AI
+
AII + AI/,II B/AIV + AV/ and C/AVI+
/AIVI t o t h e t o t a l KPD c u r v e i n dependence o n t h e a g e i n g t e m p e r a t u r e . Because t h e peak h e i g h t s Ai a r e p r o p o r t i o n a l t o t h e c o n c o n t r a t i o n ci o f t h e i - t h r e l a x a t o r / f o r m u l a(
2 )/
i t c a n be assumed t h a t Ai/zAi s t a t e f o r t h e a t o m i c f r a c t i o n s o f n i t r o g e n t a k i n g p a r t i n e a c h r e l a x a t i o n .Fig.5. The dependence: c u r v e a
-
o f A i 4-
AU' + A , 5-
Act
A 2-
A;;A
r'k
Z A; d-
+
v e r s u s a g e i n g tem- a f t e r n i t r i d i n g f o r 30 m i n . 4. D i s c u s s i o n . - I n f i g s . 1 and 3 on t h e t o m p e r a t u r e a x i s a r e marked peak t e m p e r a t u r e s c a l c u l a t e d f o r t h e Snoek r e l a x a t i o n , p r o c e s s e sI,
XI,
111 and f o r bands B and C on t h e b a s i s o f n u m e r i c a l l y o b t a i n e d d a t a f o r PIP0 c u r v e s . I t can be s c c z t ' . a t I F and MPD measurements g i v e t h e same r e s u l t s .Bmd-').
T h r e e e l e m e n t a r y p r o c e s s e s i n band A, w i t h p r e - e x p o n e n t i a l f a c t o r ss,
havea l s o
b e e n o b t a i n e d b y : ? e l c h a n d C a r p e n t e rl a ] .
They c o n s i d e r t h a t i n t h e case o f t h i s r e l a x a t i o n n i t r o g e n atoms o r d e r d i r e c t i o n a l l y i n t h e v i c i n i t y o f a n i m m o b i l e V-N p e i r c a l l e d by them t h e VN d e f e c t . T h i s d e f e c t c o n s i s t s o fa
s u b s t i t u t i o n a l Vatom i n t h e l a t t i c e p o i n t . a n d o f a n i m m o b i l o N atom o c c u p y i n g a t e t r a h e d r a l s i t e s i t u a t e d as n e a r a s p o s s i b l e t o t h e vanadium atom.
Fi9.6 p r e s e n t s t h o dependence o f h e i g h t s o f i n d i v i d u a l elemen- t a r y p r o c e s s e s , f o r m i n g peak A, on t h e s q u a r e h e i g h t o f t h e Snoek peak ( A O 2 ) . I t c a n be seen t h a t t l r o r e i s a l i n e a r c o r r e l a t i o n b e t - ween A=, A,II IIAI and w h i l e t h e r e i s no s u c h dependence f o r Ai
=
f/Ao/ / i = 1,2,3/.n a l t o t h e c o n c e n t r a t i o n o f VN d e f e c t s a s w e l l as t o t h e c o n c e n t r a - t i o n o f N atoms, g i v i n g r i s e t o t h e Snoek r e l a x a t i o n , t h e n t h e f o l - l o w i n g r e l a t i o n s h o u l d be v a l i d :
F i .6. The dependence o f h e i g h t s o f e l e m e n t a r y p r o c e s s e s
&,
I11 o n t h e s q u a r e h o i ~ h t o f r h o Bnoeb peal;; t h e sam- p l e Fe-V/0.34%/.
The r e s u l t o f t h i s a r g u m e n t a t i o n seems t o be c o n f i r m e d b y t h e expe- r i m e n t a l r e s u l t s p r e s e n t e d i n f i g . 6 .
t3~fi3-C~
E x p e r i m e n t a l peak C i s r e l a t e d t o t h e d i r e c t i o n a l o r d e r i n g o fN
atoms i n t h e v i c i n i t y o f V-N p l a t e s s i t u a t e d i n{ l o o ]
p l a n e s o f t h e m a t r i x [5,6].
A c c o r d i n g t o O.H.3eck[ l o ]
edges o f t h e s e p l a t e s a r e o f i n t e r s t i t i a l t y p e d i s l o c a t i o n l o o p s n a t u r e s o i n t h e i r e n v i -ronment a p a r t o f f r e e N atoms c o l l e c t s . The b i n d i n g e n e r g y o f N atom i n t h e s t r a i n f i e l d o f t h e p l a t e q u a s i - d i s l o c a t i o n s i n c r e a s e s i t s a c t i v a t i o n e n e r g y o f m i g r a t i o n i n consequence o f what t h o peak r e l a t e d t o t h e d i r e c t i o n a l o r d e r i n g i s s i t u a t e d c o n s i d e r a b l y h i g h e r t h a n t h e t e m p e r a t u r e s o f t h e Snoek and t h e F-M peaks,
Band
_---
B . N i t r i d i n g o f Fe-V s a m p l e s i n c o n d i t i o n s g i v e n above l e a d s a l s o t o t h e appearence o f s t r u c t u r a l e l e m e n t s i n t e r m e d i a t e between VN d e f e c t s and c o h e r e n t w i t h t h e m a t r i x V-N p l a t e s . The m e n t i o n e d p l a t e s t r u c t u r a l e l e m e n t s , c o n t a i n i n g Fe, V, N atoms, a r e sometimes c a l l e d G-P zones o f a new t y p e /Fe-V-N zones/ [5,6].
The a u t h o r s o f [6j have m e n t i o n e d i n d e e d a b o u t a d d i t i o n a l i n t e r - n a l f r i c t i o n r e l a t e d t o e l e m e n t s o f s u c h a t y p e , however, t h i s I F h a s n o t been o b s e r v e d i n t h e f o r m o f a s e p a r a t e peak. A f t e r - e f f e c t bands B and C have a l r e a d y b e e n c u l l e d [11] t h e p l a t e o r 3-3 r e l a - x a t i o n s .
C5-840 JOURNAL DE PHYSIQUE
G-P zones o f a new t y p e and c o h e r e n t V-N p l a t e s . The i s o c h r o n a l a g e i n g i n t h e t e m p e r a t u r e r a n g e 673
-
1173 K causes m i g r a t i o n and c l u s t e r i n g o f N atoms and VN d e f e c t s and f o r m a t i o n o f a d d i t i o n a l G-P zones o f a new t y p e . I n consequence o f t h i s t h e i n t e n s i t i e s o f t h e Snoek and t h e F-M r e l a x a t i o n s d e c r e a s e and t h e c o n t r i b u t i o n o f peak B i n c r e a s e s /fig.S/. As a r e s u l t o f r e p l a c e m e n t o f Fe atoms i n zones b y V atoms and o f o r d e r i n g o f t h e s t o i c h i o m e t r i c c o m p o s i t i o n o f p r e - p r e c i p i t a t e s new V-N p l a t e s a p p e a r w h i c h w i t h i n c r e a s i n g a g e i n g t e m p e r a t u r e e n l a r g e t h e i r d i m e n s i o n and a t 1073 K t r a n s f o r m i n t o p r e c i p i t a t e s o f i n c o h e r e n t VN n i t r i d e . A t t h i s t e m p e r a t u r e t h e tweed p a t t e r n v a n i s h e s a s w e l l a s t h e m i g r a t i o n a l r e l a x a t i o n s . 5. R e f e r e n c e s .l.J.D.Fast, J . L . M e i j e r i n g , P h i l i p s Res .Rep.
8
,
1 /1953/2. A.J.Perry, M.Malone, M.H. Boon, J. A p p l . Phys. 37, 4705/1966/ 3. A.J.Perry, M.H.Boon, 3. M a t e r S c i .
2
,
873 /1969/4. W.H. Welch, S.H.Carpenter, A c t a M e t a l l .
21
,
1169 /1973/ 5. M.Pope, P.Grieveson, K.H.Jack, Scand. J.Met.2,
29 /1973/ 6. M.Pope, D.M. 3ones, K.H. Jack, P r o c e e d i n g s o f ICIFUACS-5,Aachen 1973, S p r i n g e r V e r l a g , B e r l i n 1975, p. 266
7. J. Zgadzaj, J.W. Moron, M. G i g l a , P r o c e e d i n p s o f t h o I11 P o l i s h C o n f e r e n c e on A n e l a s t i c R e l a x a t i o n and M a g n e t i c A f t e r - E f f e c t s i n S o l i d s RENIOM
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80, eds. 3.W. Moroh and J. I l c z u k , S i l e s i a n U n i v e r s i t y , K a t o w i c e 1981, i n p r e s s / i n P o l i s h / . 8. 6. J a n k o w s k i , J. I l c t u k , J.W. Moroh, a s r e f .[
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10. D.H. Jack, A c t a
