J.

MONTEMAYOR
et al. : High-Temperature Creep on KBr Single Crystals 67

phys. stat. sol. (a) 88, 67 (1976)

Subject classification: 10.2;22.5.2

Departamento de Estado SdEido, Institute de Piaim,

Universidad Nacionul Autonoma de Mexicol)

High-Temperature Creep on KBr Single Crystals

BY
J. MONTEMAYOR, and E. CARRILLO
R. G~MEZ-RAM~REZ,

Constant stress creep tests are performed on KBr single crystals in the range 0.65 to
0.94Tm and 80 to 140 p/mm2. The activation energy for creep is determined as a function
of temperature by incremental temperature tests and is found to be independent of stress.

*
At high temperatures (0.74to 0.94Tm)the activation energy is found to be Qc = (1.43
0.13)eV while a t intermediate temperatures (0.65 to 0.74Tm)&, = (0.885 0.08) eV.
The first value is very close to the self-diffusion activation energy of the Br ion. It is sug-
gested that the lower value corresponds to the activation energy for pipe diffusion along
dislocation cores. The stress exponent n in the expression for the steady state strain r a k
is measured and found to be (5.3 0.3).These results indicate that the creep behavior of
KBr single crystals and that of pure metals are similar, and that the rate-controlling mecha-
nism is probably related to dislocation climb.
Des essais de fluage ont Btb effectuBs Bur des monocristaux de KBr dam l’intervalle de
650 i 940 K et de 80 & 140 p/mm2. L’bnergie d‘activation de fluage a 6th determinke en
une fonction de la tempbratwe, en essais avec accroissements de temperature et on a trouvb
qu’elle est independante de la contrainte. Pour hautes tempbratures (740 940 K) l’bnergie
d’activation a 6th Q, = (1,43& 0,13)eV, tandis que pour bempbratures intermediaires
(650it 740 K)&, = (0,88 f 0,08)eV. La premiere valeur est trks prochaine & celle de l’bner-
gie d’activation pour l’autodiffusion des ions Br. On sugbre que la plus petite valeur cor-
respond B l’bnergie d’activation pour la diffusion le long de dislocations. On a mesure
I’exposant rn de la contrainte dans l’expression de la vitesse de deformation en regime per-
*
manent, la valeur trouvQ a Btb de (5,3 0,3).Ces rBsultats laissent & penser que les com-
portements, dans le oas de fluage des monocristaux de KBr et des metaux purs sont semblab-
les et que le mkchanisme qui contrdle le processus est relie probablement au monG des
dislocations.

1. Introduction
It is well known that the high-temperature creep behavior of metals may
be understood in terms of diffusion-controlled processes [I, 21. The creep be-
havior of ionic materials has not been studied as extensively as that of metals;
however the data available [3 to 131 allow us to believe that creep is also control-
led by diffusive processes in ionic crystals.
Mukherjee et al. [2] have shown that the most appropriate expression for
the steady state strain rate is given by

where G is the shear modulus, b is the Burgers vector, k is the Boltzmann

constant, T the absolute temperature, cs the applied stress, A and n are constants,
I) Apdo. Postal 20-364,Mexico 20, D.F.
5’
68 J. MONTEMAYOR,R. G~MEZ-RAM~REZ,
and E. CARRILU)

and D is the diffusion coefficient,

D=D,exp
and Q is the activation energy.
( --
$1 ,

Sherby et al. [ l ] have shown that there is an excellent agreement in metals

as well as in ionic materials between the true activation energy for creep and
the activation energy for self-diffusion of the slowest-moving species. The true
activation energy is only obtained when the temperature dependence of the
shear modulus is taken into account. The value of the stress exponent n is
usually taken as a criterion to favor a given mechanism as the rate controlling
process in steady state.
The purpose of this paper is to report the steady state creep behavior of KBr
single crystals under compressive stresses along the [loo] axis, and its depend-
ence upon temperature and stress.

2. Experimental Procedure
2.1 Samples
KBr single crystals were grown by the Czochralski method from Merck
chemical reagent. Spectrographic analysis showed the presence of small amounts
of impurities (Fe: 5 p p m and Ca: 10ppm). The crystal were heat-treated a t
600 "C for 48 h in a nitrogen atmosphere and cooled to 100 "C a t a rate of
14 K/h. The samples were obtained by cleaving the single crystals in air. When-
ever a cleavage step or a corner defect was visually detected, the sample was
rejected. The samples had a rectangular cross section and a height to width
ratio between 1.6 and 2.7. A typical size was 5 x 5 x 9 mm3.
2.2 CTeep tests
The samples were deformed under compression in a modified [ l a ] Sherby type
[ 151 creep testing machine. They were placed between two polished alumina
discs after covering their upper and lower surface with a thin layer of colloidal
graphite t o reduce friction.
The stress was kept constant by means of a hydraulic system consisting of
an adjustable valve and a graduated cylinder lying over the loading disc. The
system allows one to add weight continuously and uniformly. The net load
was checked each 2 min and corrected if necessary. In a typical test the greatest
deviations from the nominal stress (after the first minutes) are of the order of
0.2% and last 2 to 4min. The friction forces between the mobile parts of the
testing system were measured and continuously compensated.
The temperature was kept constant within &l "C. The tests were performed
i n air.
3. Results
In Pig. 1 a few typical creep curves obtained a t three different temperatures
and a t a fixed constant stress are shown.
3.1 Reproducibility of the steady-state strain rate
Several tests were run under the same conditions of stress and temperature
t o test the reproducibility of the strain rate a t steady state among different
samples. It was found that the dispersion of EB was 8%. The actual values of is
 three different temperatures, 0 = 120 p/mma

LJK
High-Temperature Creep on KBr Single Crystals

Fig. 1. Typical constant stress creep curves for

0.2
01

0 7 2 3
_--

4 5
69

6
th-

were found from the slope of the least squares straight line adjusted to the
experimental points of the secondary creep stage. Deviations of up to 0.5%
in the slope were found by adjusting straight lines to different segments of the
experimental curve in steady state. No correlation was found between Es and
the height-to-width ratio of the samples.

3.2 Appearance of the samples after deformation

During the tests the area of the sample in contact with the alumina discs
increased. Barreling was negligible up to a strain of 40%. However, when the
samples were not covered by colloidal graphite the contact area did not increase
and barreling was considerable. A similar behavior was observed when the
samples were not placed between alumina discs due to corrosion. Tests where
one or both of these problems were present, were discarded. I n samples with
a rectangular cross section, barreling was observed only on the face with the
smallest area (11 out of 14 cases). The barreled faces showed numerous slip
lines corresponding to traces of (110) slip planes, while the other faces usually
showed a remarkably uniform thickness, except for a pair of bright outstanding
thick diagonals. These diagonals showed a maxirrium projection out of the rest
of the surface of about 5 to 10pm. The effect of barreling was not compensated
a t all.
3.3 Activation energy
The activation energy for creep was obtained from the change in strain rate
after a n abrupt change in temperature in constant stress tests. The apparent
activation energy was calculated from
3 In EB A In En
Qapp =- a( -- _ A(l/kT) .
The changes in temperature varied from 10 to 20 "C . The new temperature
was stabilized in about 6min. The apparent activation energy was found to
be stress-independent in the range from 80 to 140 p/mm2. However, a temper-
ature dependence was observed: two different values were found in two different
temperature ranges,
T
QnPp= (1.01 0.07) eV , 0.65 5 - I0.74 ;
Tm -
T
Qapp = (1.68 0.13) eV , 0.745 & 5 0.94.
70 J. MONTEMAYOR,
R. G~MEZ-RAM~REZ,
and E. CARRILM

3.4 True activation enmgy

The shear modulus of KBr is strongly dependent on temperature [16].
Therefore the apparent activation energy must be corrected to obtain the true
activation energy. Prom equation (1)

Q z -
a In (EsTGn-l) z - A[ln EsTGn-ll
a(l / k T ) 4llkT) -
Here the Voigt average G, of the shear modulus was used:

G, =
cll - Cl, + 3c44
5

The true activation energy was found to be

T
Q = (0.88 0.08) eV , 0.65 5- 50.74,
Tm -
T
Q = (1.43 f 0.13) eV , 0.74 5 - 5 0.94
Trn -
as shown in Fig. 2.

3.5 Stress dependence of the steady state strain rate

To determine the values of the stress exponent n in ( l ) stress
, change tests
a t constant temperature were performed. The value of n was calculated follow-
ing two different methods:
a) A plot of In (EI/E2) versus In (al/az)waa obtained for all the stress changes
(Fig. 3). In this form the temperature dependence is eliminated and a compar-
ison of the behavior at different temperatures can be made. The exponent n
was found from the slope of a straight line obtained by the least squares method.
The value found in this way is
n = 5.3 & 0.3.
The same result was found from the slope of the least squares straight line
obtained for the points of Fig. 4 where a dimensionless strain rate function
i, kT/DG,b is plotted versus a normalized stress ala,.
b) In the second method, the stress exponent n, for each stress change was
calculated

Q4433.B

T2TI
- loo

050
066!0.08

iU0 600 TIK)-900

Fig. 2. Temperature dependence of the activation
energy for creep. At high temperatures Q = self-
diffusion activation energy of Br ions. At lower
temperatures Q N activation energy for self-diffusion
of Br ions along dislocation cores
 High-Temperature Creep on KBr Single Crystals 71

Fig. 3. Relative strain rate change versus Fig. 4. Dimensionless strain rate versus
relative stress changes at several tempera- dimensionless stress (read G, instead of GLu)
tures, n = 5.3 & 0.3

and an average over all tests was taken to obtain a value for n
n = 5.2 _+ 0.5.
We conclude that although both values are very close, the first method is
preferred because it yields a smaller dispersion.

4. Discussion
Usually it is assumed that the stress exponent allows one t o identify the
rate-controlling mechanism in creep. However, often that is not the case,

*
because several theories [ 17, 181 based on different dislocation mechanisms
predict values of n close to 5. Here a value of n = 5.3 0.3 was found so that
we may say only that dislocations are involved. Other experiments are required
before a more precise statement on the controlling mechanism can be made.
On the other hand, the true activation energy for creep in KBr single crystals:
Q = (1.43 f 0.13) eV found in the temperature range from 487 to 667 "C,
agrees very well with the self-diffusion activation energy of the Br ion in KBr
[19]: (1.43 f 0.10) eV (490 & T & 727 "C), as expected. Therefore we conclude
that in KBr and within the temperature and stress ranges considered, the
strain rate is controlled by diffusion of the slowest moving ion in agreement
with previous results in different ionic materials.
At lower temperatures (377 t o 487 "C) the true activation energy for creep
found, was (0.88 f 0.08) eV. We believe that this value corresponds to the
self-diffusion activation energy of Br ion along dislocations. Burke and Sherby
[I,61 suggested a similar behavior in the creep of NaCl polycrystals. According
e0 their results, the change in Q occurs around TIT, = 0.74 and the ratio of
the low temperature to the high temperature activation energy is 0.60. Our
results show that in KBr the transition occurs a t about TIT, = 0.74 while
the ratio of the two activation energies is 0.62. The similarity shown suggests
that other alkali halides should behave similarly.

Acknowledgement
This work was partially supported by the Instituto Nacional de Energia
Nuclear.
72 J. MONTEMAYOR
et al. : High-Temperature Creep on KBr Single Crystals

References
[l] 0. D. SHERBY and P. M. BURKE,Progr. Meter. Sci. 13,325 (1967).
[2] A. K. MUKHERJEE, J. E. BIRD,and 5. E. DORN,Tram. ASM 62, 155 (1969).
[3] R. W. CHRISTY, Acta metall. 2,284 (1964); 4,441 (1956).
[4] YA. E. GEGUZIN,V. L. RABETS, and A. A. CHERNYSHOV,Soviet Phys. - Solid State 6,
1387 (1964).
[5] W. BLUMand B. ILSCHNER, phys. stat. sol. 20, 629 (1967).
[6] P. E. BURKE,Ph. D. Thesis, Stanford University, 1968.
[7] J. P. POIRIER,Phil Mag. 26, 701 ; 713 (1972).
[8] S. L. ROBINSON, P. M. BURKE,and 0. D. SHERBY, Phil. Mag. 29, 423 (1974).
[9] C. V. S. H. NARAYAN RAOand A. L. RUOFF,5. appl. Phys. 43,1437 (1972).
[lo] W. E. SNOWDEN and 5. A. PASK,Phil. Mag. 29, 441 (1956).
[ l l ] B. REPPICHand G. STREB,phys. stat. sol. (a) 16, 77 (1973).
[12] D. R. CROPPER and J. A. PASK, Phil. Mag. 27, 1105 (1973).
[13] W. R. CANNONand 0. D. SHERBY, 5. Amer. Ceram. SOC.66, 157 (1973).
[14] R. G~MEZ-RAK~REZ and J. A. MONTEMAYOR, Rev. Mex. Fis. (Supl. Fis. Apl.) 25, 84
(1975).
[15] 0. D. SHERBY,Trans. AIME 212, 708 (1958).
[16] 0. D. SLAGLE and H. A. MCKINSTRY, J. appl. Phys. 38, 437 (1967).
[17] J. WEERTMAN, J. appl. Phys. 28, 1185 (1957); 28,362 (1957); 26, 1213 (1955).
1181 C. R. BARRETT and W. D. NIX,Acta metall. 13,1247 (1965).
[19] 5. F. LAURENT and J. B-ENARD, J. Phys. Chem. Solids 3, 7 (1957).

(Received Apvil 20, 1976)