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DISLOCATION RELAXATION IN A RANDOM

ARRAY OF SOLUTES

I. Ritchie, A. Atrens, C. So, K. Sprungmann

To cite this version:

I. Ritchie, A. Atrens, C. So, K. Sprungmann.

DISLOCATION RELAXATION IN A

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JOURNAL DE PHYSIQUE

CoZZoque C5, supple'ment au nolO, Tome 42, octobre 1981 page C5-319

D I S L O C A T I O N R E L A X A T I O N I N A RANDOPZ ARRAY O F SOLUTES I.G. Ritchie, A. ~trens*, C.B. So and K.W. Sprungmann

MateriaZs Science Branch, Atomic Energy of Canada Limited, Whiteshe22 NucZear Research EstabZishment, Pinawa, Manitoba ROE 1L0, Canada

" B B C Brown, Boveri and Compar~y, Limited, CH-5405 Baden-DattwiZ, SuitzerZand

Abstract.- An amplitude-dependent internal friction peak occurs at 1 475 K in

well-annealed, pure a-Zr after slight deformation. Qualitatively, the results agree with a model for the motion of zig-zag dislocations in an array of ob- stacles. Comparison of theoretical and experimental results yields estimates of the effective activation enthalpy and activation volume of the process involved.

1. Introduction.- Recently, there have been advances in the understanding of high- temperature, solid-solution hardening (SSH) by dynamic simulation using computer

techniques. For example, Schwarz and L.abusch(') have employed such a technique to

c~lculate the SSH component of the flow stress (of), while Schwarz (2) has used the

same programs to calculate amplitude (€)-dependent internal friction (A). The results

reveal a simple quantitative correspondence between A ( € ) and of. These studies are

providing new insight into the nature of strain-aging effects and the athermal pla- teau in af vs. temperature (T) curves for solution-strengthened alloys.

In a-Zr, anomalous mechanical behaviour (particularly creep) and the athermal

plateau in the o VS. T curve is attributed to the strong interactions between dis-

locations and interstitial impurities (usually oxygen) ( 3 ) . In the same T range,

peaks of A vs. E with some of the characteristic properties of a thermally assisted

unpinning process have been It is shown in this paper that these

peaks can be generated in well-annealed specimens of comparatively high purity a-Zr after a very slight deformation at room temperature. Consequently, we can compare the results with calculations based on a very simple model proposed by Schlipf and

~chindlma~r(~-~), which is valid for the motion of zig-zag dislocations in a random

array of solute obstacles in the low concentration limit.

2. Material.- Measurements of A in flexure (frequency, f 4 Hz) were carried out on

specimens of a nominally 5N pure Zr. The interstitial impurity concentrations (vg/g)

of the as-received (cold-rolled strip) material were found to be H < 5, N = 6, and 0 in the range 17 to 23. Specimens were used which had been annealed in a vacuum

furnace at 1075 K (final grain size 0.7 mm) and then slightly deformed in bending

at room temperature. Even though precautions against the pick-up of 0 were taken,

after annealing and testing analysis revealed some pick-up of both 0 and H. The

final concentrations (pg/g) were H = 14

+

2 and 0 = 30. The equipment and measure- ( 9 )

ment techniques employed have been described in detail elsewhere

.

(3)

C5-320 JOURNAt DE PHYSIQUE

3. R e s u l t s . - T y p i c a l c u r v e s of A v s . T ( E c o n s t . ) and A v s . E (T c o n s t . ) a r e shown i n f i g u r e s 1 and 2 , r e s p e c t i v e l y . It must b e p o i n t e d o u t , however, t h a t i d e n t i c a l r e s u l t s were n o t o b t a i n e d on e v e r y specimen t e s t e d , presumably b e c a u s e t h e a t t e m p t e d " v e r y s l i g h t d e f o r m a t i o n " d i d n o t a l w a y s s u c c e e d . N e v e r t h e l e s s , once t h e y had been o b t a i n e d w i t h a g i v e n specimen, t h e r e s u l t s were s u r p r i s i n g l y s t a b l e and r e p r o d u c i b l e on h e a t i n g and c o o l i n g , p r o v i d e d t h a t t h e specimen was n o t h e a t e d above a b o u t 510 K. T h i s i s i n agreement w i t h t h e work of ~ t r e n s ' ~ ) who showed t h a t a s i m i l a r peak d i s -

a p p e a r e d a f t e r h e a t i n g f o r 20 m i n u t e s a t 500 K. 3.0 I I I 1 I l /'l. 480K

/

.' 2.0

-

-

'... .. -...

-

497 K 4 0 0 450 500 550 . .-Ll. 1. TEMPERA1URE.K O h 4 5 6 7

NOMINAL SURFACE STRAIN AMPLITUDE

F i g . 1 : I n t e r n a l f r i c t i o n a s a f u n c t i o n F i g . 2 : I n t e r n a l f r i c t i o n a s a f u n c t i o n of t e m p e r a t u r e a t v a r i o u s c o n s t a n t - s t r a i n o f nominal s t r a i n a m p l i t u d e a t v a r i o u s a m p l i t u d e s . The v a l u e s of E i n d i c a t e d c o n s t a n t t e m p e r a t u r e s . The s t r a i n ampli- a r e a p p r o x i m a t e l y 5 x

l o 7

t i m e s t h e s t r a i n t u d e i s 5 X 1 0 - ~ t i m e s t h e nominal s t r a i n a m p l i t u d e f o r R = 2/ ( 3 ~ ) . a m p l i t u d e f o r R = 2 / ( 3 n ) .

F i g u r e 1 c a n be d e s c r i b e d a s a f a m i l y of p e a k s of a l m o s t c o n s t a n t h e i g h t , w i t h a common high-T t a i l , and i n c r e a s i n g b r o a d e n i n g on t h e low-T s i d e , a s c i n c r e a s e s . The r e s u l t s i n f i g u r e 2 c a n be d e s c r i b e d by a A v s . E peak which p a s s e s t h r o u g h t h e "window" o f e x p e r i m e n t a l l y i n v e s t i g a t e d E , from h i g h E t o l o w , & , a s T i n c r e a s e s . The s h a p e s and b e h a v i o u r o f t h e p e a k s i n f i g u r e s 1 and 2 a r e s i m i l a r t o t h o s e p r e d i c t e d t h e o r e t i c a l l y f o r t h e r m a l l y a s s i s t e d u n p i n n i n g o f Because o f t h e p r e p a r a t i o n of t h e s p e c i m e n s , t h e f r e s h d i s l o c a t i o n s s h o u l d b e "zig-zagged1' t h r o u g h a random a r r a y o f i n t e r s t i t i a l s o l u t e s . 4. T h e o r e t i c a l ~ o d e l ( ~ - ~ ) . - I t i s assumed t h a t t h e f r e s h l y c r e a t e d network l e n g t h s c a n be t r e a t e d by t h e v i b r a t i n g - s t r i n g model b u t , b e c a u s e o f t h e i r i n t e r a c t i o n s w i t h t h e random a r r a y of o b s t a c l e s , e a c h n e t w o r k l e n g t h (L) w i l l t a k e on a z i g - z a g con- f i g u r a t i o n c h a r a c t e r i z e d by a n a m p l i t u d e (2) and a l e n g t h ( R ) a s shown i n f i g u r e 3. A t t r a c t i v e and r e p u l s i v e o b s t a c l e s a r e supposed t o b e p r e s e n t i n e q u a l numbers, and t h e " i d e a l i z e d " b a s i c s t e p i n t h e d i s l o c a t i o n m o t i o n i s t a k e n t o b e t h e jump from one z i g - z a g c o n f i g u r a t i o n , An Bn AnC1, i n t o a n e q u i v a l e n t o n e , An Cn An+l ( s e e f i g u r e 3 ) . I n t h e p r o c e s s , t h e d i s l o c a t i o n i s unpinned a t t h e a t t r a c t i v e o b s t a c l e B pushed

(4)

past the repulsive obstacle R and recaptured by the attractive obstacle C The

n' n'

corresponding potential energy diagram (figure

4)

has four minima that must be taken

into account. At the lowest E , the dislocations interact with the attractive ob-

stacles only. This gives rise to a Debye peak which is E-inde~endent'~). At higher

E , the dislocations are forced to interact with the repulsive obstacles also. Ac-

cording to Schlipf and ~chindlrnayr'~), the dislocation velocity

(9)

is given by

9

= Zw sinh (gb 3 ~ e f / c ~ T )

[l1

where w = jump frequency at a = 0, g 1 (geometrical factor), b = Burgers vector,

c = concentration of obstacles, k = Boltzmann's constant and aeff = effective stress.

If internal stresses are neglected, aeff is composed of the external stress (U) and

the back stress, ( ~ % / b ) d ~ ~ / d x ~ , due to the line tension (Ta). T is taken to be

II

0.5 ~b~ where G is the shear modulus. For E > c ~ T / R E ~ ~ , eqn. [l] defines an E-de- pendent dislocation mobility and a solution in closed-form is not possible. Assuming interstitial 0 obstacles, c 2 X 1 0 - ~ , and since Young's modulus (E) = 99 GPa, and

the average orientation factor R 1 2/(3n) (for a random assemblage of grain orienta-

tion~), the above inequality predicts €-dependence for E > 4 X l ~ at - 475 K. ~ This is in keeping with the results in figures 1 and 2, indicating that a solution of eqn. [l] is necessary.

POTENTIAL ENERGY E(sl

l

Fig. 3 : Upper diagram shows the basic Fig. 4 : The potential energy of the

jump of the dislocation from one attrac- zig-zag element is plotted as a function

tive obstacle B,, over a repulsive ob- of the reaction path parameter, S.

stacle R,, to an attractive obstacle C,. The lower diagram also defines zig-zag bow-out of a network length (L).

If it is assumed that the average bow-out of the network length (under stress) is given by a cosine function (an excellent approximation when non-linear effects are

negligible(7)), an approximate solution can be obtained for a linearized cyclic

stress, which in turn leads to a closed-form expression for A. The equations given

by Schlipf and Schindlmayr(8) are incorrect. We have repeated the calculations and find

A = (2/n) ( A L ~ ) ( E / G ~ ~ ) [2 in{ (p2+l)'/p}

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C5-322 JOURNAL DE PHYSIQUE

X

where Li2 = -o/ [(ln(l-E))/S]dg (the dilogarithm function), w = 2nf, a = oob3/ckT (uo is the stress amplitude), p = (n/2)/aowr, T = ~ ~ c k ~ / n ~ = ~ w'exp(-U w ~ ~ ~ b ~ ,

eff'

kT) where w' is an attack frequency and Ueff is the effective activation enthalpy,

and B = (p2!l)'/pr. The equations for q1 and q2 are

41 = [(P2+1)'-1~/[(p2+1)'+ll~; 9 2 = S 131 with

s

= [p/{ (p2+1)'-1}l. [(p2cosh2(~B/2w)+l)'-p cosh(n~/2w)].

A plot of AN (normalized A) vs. wr for various values of a. is shown in figure 5.

This family of curves can be described as a peak of almost constant height, which

broadens on the high wr (low T) side as a (or E) increases, while the low UT (high

T) asymptote is unchanged. These curves are qualitatively very similar to the ex- perimental results shown in figure 1.

Fig. 5 : Normalized internal friction as a function of wr for various

values of ao.

To make a more detailed comparison between theory and experiment, we have cal- culated A vs. T (E const.) and AN vs. E (T const.) curves for the same ranges of E

N

and T explored experimentally. These calculations have been carried out using

eqn. [ 2 ] adapted to the strain distribution in our flexure specimens(9). The para-

meters used in the calculations were: w' = 1 X 1012 S-l, Ueff = 1 eV (simply esti- mated from the peak position), w = 8n, ~b~ = 7.47 eV, c = 2 x 1 0 and L ~ ~ = 1000 b. The activation volume (V) of the process (b times the diamond area swept-out by the

dislocation, figure 3) is 2bZQ, or more simply, V = b3/c = 5000 b3. The calculated

results corresponding to figures 1 and 2 are given in figures 6 and

7,

respectively.

In figure 7, the arrows indicate the approximate range of E explored experimentally

in figure 2. Comparison of the experimental and theoretical curves shows that quali- tatively the agreement is very good.

5. Discussion.- The magnitudes of Ueff = 1 eV and V = 5000 b3 are consistent with

(6)

. X..,

g

0.2- a

z 0.1 -

,

' G ' :

i

!

6 7 8

Fig. 6 : Normalized internal

friction as a function of tem- perature calculated for the various indicated strain ampli- tudes.

Fig. 7 : Normalized internal

friction as a function of strain amplitude calculated for the various temperatures indicated. Arrows indicate the experimental strain amplitude range.

STRAIN AWUTUDE x 106

SSH in a-~r'l~). Fernandez and ~ovolo(~) have attributed an E-dependent A peak at

about 475 K in large-grained Zr to the interactions between oxygen and extended

dislocations. However, their results obtained at 50 kHz yield a much broader peak

(extending to 800 K on the high-T side) than the results in figure 1. Comparison of

their results with theoretical predictions for the unpinning of extended disloca- tions(13) yields a reasonable value for the binding energy of 1.3 eV, but an unrea-

sonably large dislocation loop length (= 5 X 104 b). In the model presented here,

Ueff is not simply related to the binding energy (see figure 4) but is not incon-

sistent with the high values reported for the binding energy (3y5'14). It should be

noted that the parameters used in the calculations for figures 6 and 7 are not the

only set which give qualitative agreement between theory and experiment. Neverthe- less, the very good agreement obtained using plausible parameters is very promising. It suggests that a quantitative comparison between theory and experiment can be attempted using single crystals (i.e. with R known), if an independent determination

of the network length, L, can be obtained and the concentration of interstitials is

known. REFERENCES

1. R.B. Schwarz and R. Labusch, 3 . Appl. Phys. s(10) (1978) 5174. 2. R.B. Schwarz, Proc. ICSMA 5, Aachen (1979)

2

953.

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CS-324 JOURNAL DE PHYSIQUE

A. Atrens, Scripta Metall.

8

(1974) 401.

L. Fernandez and F. Povolo, J. Nucl. Mater.

66

(1977) 79. R. Schindlmayr and J. Schlipf, Phil. Mag.

3

(1975) 13.

J. Schlipf and R. Schindlmayr, Phil. Mag.

3

(1975) 25.

J. Schlipf and R. Schindlmayr, Proc. ICIFUAS 5, Aachen 1973, Springer-Verlag,

Berlin (1975)

2

439.

K.W. Sprungmann and I.G. Ritchie, AECL-6438, 1980.

L.J. Teutonico, A.V. Granato and K. Liicke, J. Appl. Phys. x(1) (1964) 220. D.G. Blair, T.S. Hutchison and D.H. Rogers, Can. J. Phys.

2

(1971) 633.

P. Lukac, J. Scient. Ind. Res.

2

(1973) 569.

D.G. Blair, T.S. Hutchison and D.H. Rogers, Can. J. Phys.

48

(1970) 2955.

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