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The compression creep test is analyzed with respect to the of the material for large deformations. The importance of the
friction at the loaded ends of the specimen. An analytical stress exponents of a single experiment for the identification of
and a finite-element solution performed for large deforma- the dominating creep mechanism is shown.
tions reveals that friction leads to a strain-independent
reduction of the creep rate which only depends on the stress 11. Evaluation of the Compression Creep Test
expbnent of the creep law and the geometry of the specimen.
The assumed material behavior is a time-dependent, iso-
choric, nonlinear viscosity. Compression creep tests on ( I ) Experimental Boundary Conditions
3-mol%-yttria-stabilized tetragonal zirconia polycrystals The fixture and the measuring system for a compression
(3Y-TZP) have been analyzed. The determination of a stress creep test inside a furnace are shown in Fig. 1. The loading ele-
exponent corresponding to the decreasing stress state in the ments between the attached rods of the measurement system-
specimen during large deformations results in a higher res- the two load pads-must be made of much higher creep resis-
olution of the stress-strain-rate relationship derived from a tant material than the specimen and, therefore, can be assumed
certain number of creep tests. For 3Y-TZP the compression to be rigid.
creep tests reveal a decreasing stress exponent with increas- The compressive stress is usually applied on the specimen
ing stress. using a dead load, hydraulic, or spring system. In most cases,
the experimental boundary condition is a constant load ( F =
I. Introduction constant), which is considered for the following calculation.
The measuring system provides a data set of displacements
2468
October 1993 Critical Evaluation of the Compression Creep Test 2469
The transition from the engineering values to the true values
which describe the material behavior can easily be performed
for the frictionless case, using the boundary coddition of a con-
stant volume during the deformation.
Based on V = constant and F = constant, which can be writ-
ten as A,h, = Ah and a,A, = a,A, the following equations for
the transition are obtained:
u, = (1 - &,)a, (7)
E, = -In (1 - E,) (8)
1
El = Ee- (9)
l - E,
volumetric rate of deformation to the hydrostatic stress.’, Only the creep rate for the constrained boundary condition decreases
the deviatoric p,m of the stress vector causes a deformation, fol- by a constant factor.
lowing the equation Using the explicit time-integration scheme ( 5 = 0.0) in Eq.
(16) and the creep law in Eq.(6) for both solutions, a compari-
son can be shown in the formulation of the true values for strain
Based on the creep law assumed for the uniaxial material rate and strain (Fig. 8). The logarithmic strain rate versus strain
behavior in Eq. (6), the nonlinear viscosity shows a constant slope in the creep curve for large deformations
caused by the stress reduction corresponding to the rising cross-
sectional area of the specimen during the def~rmation.~ Assum-
ing a constant cylindrical shape of the specimen-the friction-
is achieved for the corresponding material viscosity in the less case-and using Eqs. (6) to (8), the relation
finite-element calculation.
Considering the symmetries in the cylindrical specimen, we
regard the area for the calculation (Fig. 3) of this axisymmetric
problem to be one-fourth of the longitudinal cross section of is obtained for long times.
the specimen. The constant slope for large deformations in Fig. 8 therefore
To estimate the influence of the singularity at the edge of the provides the direct derivation of the “local” stress exponent of
loaded area on the deformation, we use finite-element meshes the creep law in the stationary creep regime. The corresponding
with different refinements. results for the total constraint case reveal a vertical shift, but no
(3) Results and Discussion changes in the slope of the curve. This allows the derivation of
a local stress exponent from a compression creep test with large
Calculations have been conducted using some typical values
deformation and a stationary creep regime even under the
for 3Y-TZP for the parameters K , , K,, and n of the creep law.
The results in the following diagrams are based on the assumption of significant friction at the loaded specimen ends.
parameters K , = 2.353 X lo-’, K , = 1.0 X and n = 2.2 The shift of the creep curve for the total constraint boundary
with an applied compressive stress of u, = 35 and a starting condition is a result of the inhomogeneous stress distribution
condition of E, = E, = 0.0 at I, = 1. The stress, strain rate, and and can be defined by a creep reduction factor
time parameters are treated as if dimensionless, assuming that K, = &tola, constraint
the original values are normalized by the value 1 with the
~friction1ess
dimensions MPa, s-I, and s, respectively.
The finite-element solution for the fully constrained end which is the ratio of the creep rates for the total constraint and
faces shows, for the initial state at E, = 0 in Fig. 4, a severe the frictionless case in the initial state. As shown in Figs. 7 and
inhomogeneous distribution of the vertical stress (the stress 8, the K , factor is constant over the broad regime of time or
component parallel to the load axes) in the specimen. Based on strain considered in these investigations.
the result of the stress distribution for a significant deformation The K , factor depends on the stress exponent of the creep
E, = 15.6%, shown in Fig. 5, we can assume that the stress dis- law-the degree of nonlinearity of the material behavior. The
tribution remains approximately constant during the deforma- deviation of the creep rate due to the total constraint boundary
tion. The von Mises stress distribution at E, = 0 in Fig. 6 shows condition can be expressed as (1 - K , ) and is shown in Fig. 9 as
the inhomogeneous deviatoric flow of the material leading to a function of the stress exponent n.
the measurable deformation of the specimen. The shape of the specimen is another important parameter for
Figure 7 shows the direct comparison of the time-dependent the inhomogeneous stress distribution and the resulting creep-
engineering strain rates between the boundary conditions of rate deviation. For the different cylindrical specimens calcu-
frictionless and total constraint. The general time-dependent lated here in the initial state, an increase in the ratio of diameter
behavior for both boundary conditions is the same, but the to height leads to an increase in the creep-rate deviation (1 -
curve of the finite-element solution is shifted slightly along the K , ) shown in Fig. 10. Specimens with lower ratios of diameter
vertical axis toward smaller values. This leads to the result that to height become very sensitive to deviations from the ideal
shape, leading to structural instabilities and, therefore, unpre-
dictable results.
Fig. 4. Distribution of the vertical stress at Fig. 5. Distribution of the vertical stress at Fig. 6. von Mises stress distribution at E , =
E, = 0% for total constraint end faces (units in E, = 15.6% for total constraint end faces 0% for total constraint end faces (units in
MPa). Applied force is equal to an average (units in MPa). Applied force is equal to an MPa). Applied force is equal to an average
compressive stress of 35 MPa (corresponding average compressive stress of 30 MPa (cor- compressive stress of 35 MPa (corresponding
stress fringe labeled with A). responding stress fringe labeled with B). stress fringe labeled with A).
1
1 10 100 1000 10000 100000 = 0
T i m e Csl 1 1.5 2 2.5 3 3.5 4 4 5 5
Stress e x p o n e n t
Fig. 7. Engineering strain rate E, as a function of time for the friction-
less (analytical solution) and the total constraint case ((A) finite- Fig. 9. Creep-rate deviation (1 - K,)for the total constraint case as a
element solution). function of the stress exponent of the creep law.
50
n
u)
\ 40
7
u
a, 1 E-4
c
30
F
.-c
0 20
2 1 E-5
v)
a
10
3
I
t- ~ -
total constrain
--
1 E-6
0
0 .05 10 15 .20
0 .5 1.0 1.5 2.0 2.5
True strain
Diameter / Height
Fig. 8. True strain rate Et as a function of true strain E, for the friction-
less (analytical solution) and the total constraint case ((A) finite- Fig. 10. Creep-rate deviation (1 - K,)for the total constraint case as
element solution). a function of the specimen geometry-the diameter-to-height ratio.
2472 Journal of the American Ceramic Society-Debschiitz et al. Vol. 76,No. 10
Y
.-K
l.E-6
+
.-
C cn
l.E-6 a,
c
u) 3
L
a, +
?
+ 1 .E-7
1.E-7 ~
.05 .10 .15 .20
.05 .10 .15 .20 T r u e strain
True strain
Fig. 13. True strain rate versus true strain at 1200°C and 20, 3.5, SO
Fig. 12. True strain rate versus true strain at 1200°C and 3.5 MPa M i a under constant load. Stress exponents n are determined by the
under constant load and under constant stress. slopes of the strain rates between 0.02 and 0.17 strain.
October 1993 Critical Evaluation of the Compression Creep Test 2473
7
&I
€2
= exp[ --(-R $)j
Q l -
TI
n 12000 c. n=2.a
C. ~ 3 . 2
at a temperature of 1200°C for k 3%. The strain range for the C , n=2.9
determination of the stress exponent is at least 0.1 strain, so that
the error introduced by temperature is less than k0.3 for the
exponent.
The influence of the choice of the range for the least-squares
fit is k0.2. As an example, in Fig. 13, the determination of the
stress exponent in the range between 0.08 and 0.18 strain
instead of 0.02 and 0.18 reveals a stress exponent of 2.4 instead
of 2.2 for the test at 1200°C and 50 MPa and an exponent of 4.6 l.E-8 1 1
instead of 4.5 at 20 MPa. As shown in Fig. 8, the effect of the 10 20 50 100
unknown friction at the loaded ends is negligible. In addition,
the error by temperature variations and uncertainties by deter- Stress CMPal
mination of the beginning of the stationary region yields an Fig. 15. Comparison of stress exponents from (-) single creep tests
error in determination of the stress exponent in a constant load and ( - - - ) stress exponents of the whole stress range for different
test of 20.5. In these limits, observed stress exponents of 4.5 temperatures.
and 2.2 are significantly different.
(C) Microstructural Analysis: The microstructure of
deformed specimens has been investigated by TEM (Fig. 14). stress exponent with increasing stress, observed in alumina”
The faceted grain shape is clearly visible. No differences in the and in zirconia,’’ cannot be explained in this way. Simple
microstructure between the deformed and original specimens superposition can lead only to an increase of the stress exponent
can be detected; i.e., no grain-shape or grain-diameter change is with increasing stress.
found. No cavitation can be observed. The deformation is not One possibility for explaining a decrease of the exponent
caused by grain elongation or grain growth, according to other with increasing stress is a mechanism with a threshold stress.’’
investigations reported elsewhere. l4 In the regime of the threshold, the creep law (Eq. (6)) is not
(0) Stress Exponent: As illustrated above, the stress valid, and the measured stress exponents are not characteristic
exponents have been determined by two methods. First, a com- for any mechanisms.
parison of the strain rates at significantly different stresses The activation energy and the stress exponents measured in
yields one value for the stress exponent for the whole stress the high-stress range show quite common v a l ~ e s . ’ ~In - ’ this
~
range tested. Second, evaluation of the decrease of the strain range, shape-conserving mechanisms, such as diffusion-accom-
rate corresponding to the decreasing stress in a single experi- modated grain-boundary sliding,” can be rate limiting. This
ment under constant load with large deformation yields a stress mechanism has a stress exponent of 2 if it is interface controlled
exponent corresponding to the testing stress level. Every test and reveals no changes in the microstructure consistent with
stress level yields a special stress exponent. our observations.
A comparison of these differently derived stress exponents is In the low-stress range, the measured stress exponents are
shown in Fig. 15. The stress exponents of a single experiment very high and cannot be correlated to a deformation mechanism
are shown in the diagram as short straight lines with the corres- directly. It can be concluded, then, that the measured values
ponding slopes. The other stress exponents are the slopes of the belong to a transition region, where the stress exponent has no
least-squares fitted straight lines through the strain rates at dif- physical meaning. The stress dependence of the stress expo-
ferent stresses, shown as dashed lines. nents evaluation from the single experiments indicates a thresh-
As an example, at 12OO0C, the stress exponent of the entire old stress of about 15 MPa. The mechanisms in the low-stress
stress range is 2.8, and the stress exponents of the single creep range will be discussed in detail elsewhere.Z2
tests are 4.5, 3.9, and 2.2 for 20, 35, and 50 MPa (see Fig. 13),
respectively.
An increase of the stress exponent with increasing stress, IV. Conclusions
which is observed in some ceramics,” can be explained by a (1) The effect of friction at the loaded ends of compression
superposition of two mechanisms. However, a decrease of the creep specimen decreases the strain rate by a time- and strain-
independent factor K , which is the ratio of the creep rates for the
total constraint and the frictionless case.
(2) The stress exponent of the creep law determines the
creep-rate deviation ( 1 - K,). For a typical diameter-to-height
( d / h ) value of 0.5, the creep-rate deviation ( 1 - K , ) ranges
from 8% to 14% for n = 1 to 5.
(3) Different specimen shapes influence the deviation (1 -
K , ) significantly. For d / h values from 0.5 to 2, the creep rate
deviates from 8% to 35% for n = I .
(4) Based on the calculated strain-independent strain-rate
reduction in the case of friction, the evaluation of a stress expo-
nent from the decreasing stress during the large deformation is
possible in a single experiment. This provides as high resolu-
tion of the stress-strain-rate relationship in a low-stress regime.
(5) Variations in this relationship are detectable with this
evaluation and reveal changes in the rate-controlling mecha-
nisms.
(6) 3-mol%-yttria-stabilized tetragonal zirconia polycrys-
tals (3Y-TZP) show a regime of a stationary compression creep
from 3% to more than 20%.
Fig. 14. TEM micrograuh of microstructure after 30% true strain. (7) The stress exponent decreases from 4.5 to 2.2 with an
Dgeection of the load F t s [ndicated by an arrow. increasing stress from 20 to 50 MPa.
~~~
Y
2474 Journal of the American Ceramic Society-Debschutz et al. Vol. 76, No. 10
(8) The changes of the stress exponent in the investigated 9J. H. Agyris and H.-P. Mlejnek, The Finite Elemenr Method (in Ger.). Vieweg
& Sohn, Braunschweig, Germany, 1987.
stress regime indicate a transition in the rate-controlling mecha- u.
‘OR. Diez, Hindenlang, and A. Kurz, “LARSTRAN-USeT’SManual,’’ LASSO
nism at very low stresses (-15 MPa). At higher stresses (-50 lngenieurgesellschaft, Stuttgart, Germany, 1991.
MPa), diffusion-accommodated grain-boundary sliding is iden- “K.-J. Bathe, Finite Element Procedures in Engineering Analysis. Prentice
tified as the dominant mechanism with a stress exponent of Hall, Englewood Cliffs, NJ, 1982.
”J. H. Argyris and J. St. Doltsinis, “A Primer on Superplasticity in Natural
n = 2. Formulation,” Comput. Methods Appl. Mech. Eng., 46,83-131 (1984).
”C.-M. J. Hwang and I-W. Chen, “Effect of a Liquid Phase on Superplasticity
of 2-molB-Y,O,-Stabilized Tetragonal Zirconia Polycrystals,” J. Am Ceram.
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