Refractories
9, 1994
RESEARCH
UDC 666.3/.7.017:620.172.251.2
H I G H - T E M P E R A T U R E C R E E P IN R E F R A C T O R Y C E R A M I C S .
DENSELY SINTERED MULTIPHASE MATERIALS
V. S. Bakunov 1
Translated from Ogneupory, No. 9, pp. 2 - 8, September, 1994.
Original article submitted June 7, 1994.
High-temperature creep in densely sintered multiphase ceramics is considered. The presence of other phases,
namely, crystalline and glassy, is shown to affect the behavior of specimens. Data on creep during phase
transitions in the materials are presented.
At high contents of impurities and controlled additions in
the initial materials the phase composition of a ceramics is
changed, which radically changes its behavior under a me-
chanical load; deformation of solid solutions is an intermedi-
ate case. We shall distinguish between crystalline and glassy
inclusions. The latter are commonly low-melting as com-
pared to the matrix. Creep is affected by the type and compo-
sition of the other phase and its distribution over the volume
of the material. Deformation due to phase transitions, i.e., so-
called plasticity of phase transitions, is a special case.
Loading causes volume deformation in every phase in ac-
cordance with its mechanical characteristics. The resultant ki-
netics of the process (just like the kinetics of complex chemi-
cal reactions [I, 2]) can be limited by the fastest stage if the
reactions are parallel or by the slowest stage if the reactions
occur sequentially. Creep is accompanied by self-consistent
deformation in microvolumes of the specimen in the sense
that no macroscopic violations of its continuity are observed.
The rate of the process v is determined as 1/v = ~ 1/pivi for
sequential stages and as v = ~ pivi for parallel stages, where
v i is the deformation rate of the given phase and Pi is its vo-
lume fraction.
In creep, the geometric distribution of the phases over the
volume of the material is of great practical importance, be-
cause creep resistance is mainly determined by the continu-
ous phase. Thus, formation o f glassy layers along crystal
boundaries leads to sharp growth of the creep flow rate even
when their content is insignificant. On the other hand, con-
Institute of High Temperatures, Russian Academy of Sciences, Moscow,
Russia.
277
Vol. 35, No.
tinuous strong skeleton is creep resistant at comparatively
large amounts of less strong inclusions.
In high-temperature creep a distinctive feature of the be-
havior of the materials is the absence of concentrated stresses
on the phase interfaces; these stresses relax.
Phase transitions. As shown in [2], changes in the phase
composition of the material during testing substantially affect
the cource of the creep process. At each moment of time the
deformation corresponds to a new phase composition and
structure of the specimen and testing conditions. As a rule,
when the composition rapidly changes (i.e., the phase equi-
librium is established in a short time), we can experimentally
determine only changes in the parameters of the dependence
= f ( T , ~, S), while for a slowly changing composition we
can also determine the creep curves.
The effect of continuous alteration of the phase composi-
tion and the structure of a ceramics in creep tests in a reduc-
ing gaseous medium in a testing furnace has been studied in
[3] for cerium dioxide, which is known [4] to lose oxygen un-
der these conditions. Even at insignificant reduction the mate-
rial exhibits a second phase that can be regarded as a solid
solution of Ce203 in CeO 2. It seems that all intermediate
structures in the range of compositions between Ce203 and
CeO 2 are formed by combinations of cerium ions of valences
3 and 4. We may assume that such structures are of fluorite
type with anion vacancies. A decrease in the oxygen content
in CeO 2 leads to the deformation of the crystal lattice and
weakening of the interionic bonds, which changes the struc-
ture-sensitive properties of the material.
Experimental investigations of creep in CeO 2 during re-
duction in a helium medium consisted in the following. A
CeO 2 specimen was placed in a furnace and kept there at a
0034-3102/94/3509-0277512.50 © 1995 PlenumPublishingCorporation
278
250
3 b
200 3
.I=15o
~1oo
50
0 ol
2.00 1.95 1.9o 2,00 1 . 9 5 1.90
X X
Fig. 1. Creepflowrate ~-in a ceriumdioxideceramics(CeOx)as a function
of its reductionx at (a) 1350~C,(b) 1400°C, (e) 1450°Cand (1) 0.6 MPa,
(2) 1.4 MPa,and (3) 2.5 MPa.
-1
~ 875
.w
2.000
-4 I I .........
5.8 6.0 6.2
Fig. 2. Temperature dependence o f creep for different values of x in
(shown at the straight lines).
high temperature (exceeding the temperature of the previous
tests) for the reduction to occur. The holding time up to the
requisite degree of reduction at the given temperature was de-
termined from the reduction curves [5]. Since the temperature
reached the requisite level rapidly, we did not take into ac-
count changes in the phase composition of the specimen dur-
ing this time. Then we established the specified temperature
of testing, loaded the specimen, and determined the deforma-
tion over time. Strictly speaking, the reduction of CeO 2 con-
tinued during the determination of the creep flow rate, but we
did not take this fact into account because at lower tempera-
tures the experiment lasted a short time.
The resultant creep curves [2] were used to plot the de-
pendence atthe rate of the process on the degree of reduction
at constant temperatures and loads (Fig. 1). During reduction
the deformation rate in CeO 2 first increases sharply and then
increases more slowly. By interpolating the plotted depen-
dences we determined the rates of the process for composi-
tions varying from CeOi.975 to CeOi.87~.
The dependences between creep and temperature for dif-
ferent levels of the material's reduction are presented is
Fig. 2. Results for unreduced CeO 2 were obtained in testing
in air. It can be seen from Fig. 2 that during reduction the de-
formation rate increses sharply and the activation energy of
V.S. Bakunov
~
I0 2.00
400 1.975
7.5
2001
5
,,,,,,,,,,,-" 1.925
]o0l ...,...--" ~ 1.90
~~,*'='~ 1.875
2.5
2,00 1.90
0..5 1.0 1.5 2.0
log 6
Fig. 3. Variation o f log Z as a function o f log tr in reduction o f C¢O:v
the process falls. At low reduction levels the change in the
activation energy is not large, which corresponds to the be-
havior of materials with low contents of admixtures. At the
next stage the activation energy decreases sharply when the
phase composition changes substantially; this is accompanied
by strong deformation of the lattice due to the presence of a
large number of excess vacancies. Subsequently, the vacan-
cies become so numerous that increase in the deviation of the
composition from the stochiometric one ceases to affect the
creep in the ceramics. R seems that here lies the region of ho-
mogeneity of the intermediate phase (or the formation of a
6.4 eutectic mixture in the CeO2 - Ce203 system, to be discussed
Io4/r,g-~ below).
C o Ox Depending on the stress, all the specimens studied exhi-
bited almost ductile behavior (see Fig. 3) and the index n was
close to I. Only cerium dioxide tested in air had a somewhat
greater n (n = 2).
Another case is considered in [6]. For a synthetic mullite
ceramic the temperature dependence of creep has inflections
in the temperature range 1600 - 1650°C; before and after this
interval the dependence log ~ - lIT is linear (Fig. 4a). When
the specimens were tested starting from a temperature above
the region of anomalous behavior (i.e., 1600 - 1650°C) the
curve of log ~ versus 1/T was a continuation o f the low-tem-
perature (1500-1600°C) part and had no inflections
(Fig. 4b). This change in the temperature dependence of the
deformation rate in the indicated region is explained by the
transformation 3A1203 • 2SIO2 ---) 2A1203 - SiO 2 transition in
the mullite composition.
In firing (with a maximum temperature o f 1710°C) even
the 3A1203 • 2SiO 2 specimens mostly form mullite 2A1203 •
SiO 2 (a solid solution of aluminum oxide in mullite) and si-
lica (see also [7]). During heating and prolonged holding at
1600°C under a load mullite with a 2 : 1 composition trans-
forms into 3 : 2 mullite; this is accompanied by bonding of
silica, a decrease in the glassy phase content, and growth of
the apparent plasticity. No reverse transformation of 3 : 2
mullite to 2 : 1 mullite is observed when the test temperature
is increased further, which may be explained by the fact that
measurements at high temperatures are made during much
H i g h - T e m p e r a t u r e C r e e p in R e f r a c t o r y Ceramics 279

10 -I I0-:
b

10-2 20
I0-: 16"
,o-, -_
14
.d
l 0"'
12 ~ . E t . . . . 2 ~ o - ' - - ' ' ~

I0"s i i 10-4
4.6 4.8 5'.0512 5.4 5,6 4.s 510 5.2 5.4
104/r,K -~ 104/r, g-~
Fig. 4. Temperaturedependenceof creep flow rate in rnullite.The tests were
startedat (a) 15000Cand (b) 1700°I::;the loads were 0.9, 2.0, and 3.7 MPa for
1 - 3, respectively.
shorter time periods. If the tests are started at 1700°C, no 3 : 2
muIlite is formed and no anomalous region is observed.
These assumptions are verified by data o f x-ray phase
analysis. In specimens hardened from high temperatures
(1700°C) 2 : I mutlite is largely observed, while specimens
hardened from lower temperatures (1600°C) exhibit mixtures
of 2 : 1 and 3 : 2 compositions. Indirect data are obtained
from the creep activation energies. The curves in Fig. 4b cor-
respond to an activation energy o f about 545 k J/mole, which
is equal to the viscous flow activation energy o f quartz glass
(silica is freed during the formation o f the solid solution); the
creep activation energy o f very pure mullite specimens is
much higher and constitutes 1000 - 1100 kJ/mole.
The dependence between creep and load also verifies this
approach. At temperatures lower than 1600°C and in tests
starting from 1700°C the index n is the same and equals 1,
which is typical o f liquids and glasses and implies viscous
flow. In the range o f 1600 - 1650°C n increases (to about 2),
which is typical o f the deformations o f crystalline materials
(Fig. 5).
Solid solutions. As a rule, the formation of a solid solu-
tion is accompanied by considerable distortion o f the crystal
lattice and weakening o f the bonds between its elements (ex-
cept for the case o f replacement with an ion o f the same va-
lence or o f a close ionic radius). A t low concentrations the
lattice is deformed, so that when the concentration increases,
we observe the appearance o f another phase, namely, a con-
1C I f I
0,8 1.0 1.2 1.4 1,6
log
Fig. 5. Variationof log Z with log a for mullite in the temperature ranges
(1) 1650- 1850°C, (2) 1700- 18500C, and (3) 1550- 1650°C.
tinuous one or one in the form o f individual inclusions. In its
chemical composition this phase may be a double compound
or a solid solution.
We consider here a practically important case, namely,
creep in stabilized zirconium dioxide. Examples o f other
cases are given above and below in the text. In order to pre-
vent polymorphic transformations and the corresponding de-
struction of articles during use, zirconium dioxide is enriched
with stabilizing additions. The effect o f introduced calcium
oxide, which forms a solid solution o f substitution type that
has a lattice resembling a fluorite one, was studied in [8]. By
the condition o f conservation o f electric neutrality, one anion
vacancy is formed per C ~ + ion. Thus, an increase in the con-
centration o f the stabilizing addition results in a greater num-
ber o f point defects.
In order to determine the influence of the concentration
of the addition on the deformation rate we investigated creep
in zirconium ceramics with 8, 10, 12.5, and 15% (molar frac-
tions) additions o f CaO. The processes o f stabilization and
sintering were combined in one firing. The characteristics of
experimental specimens are presented in Table 1.
We established during the tests that zirconium dioxide
stabilized by a 10% CaO addition has the lowest deformation
rate in the investigated temperature and load intervals (1300 -
1500°C and 1 2 - 2 5 MPa, respectively). When the concen-
tration o f the stabilizing oxide is increased or decreased, the
creep resistance o f the specimens fails (Fig. 6). Compositions
with a deficit o f CaO are deformed faster due to distortions in

TABLE 1. Characteristicsof SpecimensofaZirconium Ceramics*

Composition Mole fraction Crystalsize, tam %er~, MPa Ti.m., *C
ofCaO, % Papp,~ crn3 Poo~,% dominating maximum 20"C 1000°C
1 8 5.46 3.5 3- 5 10 105 85 Not
determined
2 10 5.50 0 15 -20 30 245 170 2320
3 12.5 4.95 0.3 I 0 - 15 20 140 100 2300
4 15 4.86 7.1 10- 15 20 125 90 2280
" Pappis the apparent density, Porch is the open porosity, (rbcnd is the ultimate bending strength, Ti.m. is the temperature of melting
initiationat a load of 0.2 MPa.
280 V.S. Bakunov

-1

15

.~: -2

a:: 10
¢0
_o
.d 5 -3

10 15 20 -4 t ) i
Mole fractionofCaO, % 5.6 5.8 6.0 6.2 6.4
lo4/ r, K -~
Fig. 6. Deformationrate in a zirconiumceramicsas a functionof the amount Fig. 8. Temperatu~ dependence of the deformation rate in a zirconium ce-
of stabilizatingoxide(1400°C, 5 MPa). ramics of composition 3 from Table I before (I) and al~er(2) destabilization
(the load is 5 MPa).
10-1

Ceramics based on zirconium dioxide stabilized by CaO

.d I0"3 J u ~ ~ peratures below 900°C, completely and reversibly transforms
10-' 1 I ) I
5.6 5.8 6.0 6.2 6.4 6.6
104/T, K =I
Fig. 7. Deformationrate of a zirconium ceramicsas a function of tempera=
ture. The numbersat the straightlines indicatethe molefractionof CaO, %.
their lattices. Compositions with optimum amounts of addi-
tions needed to form a fluorite structure are most stable.
When the addition is in excess, the defects arising aLso in-
crease the deformation rate.
The dependence of the deformation rate in the investi-
gated zirconium ceramics on the temperature is given in
Fig. 7. The activation energies calculated from the slopes
of the lines of log ¢ versus 1/T constitute 350, 560, 560, and
620 kJ/mole for compositions 1 - 4 (see Table 1), respec-
tively.
Depending on the load, all compositions exhibited
viscous behavior, i.e., their index n was close to 1
(n = 1.1 - 1.4).
It is noteworthy that the creep activation energy in com-
position 1 is substantially lower than in the other three com-
positions. This may be explained by the presence of vacan-
cies in the phase oftbe transition structure (from tetragonal to
cubic), because 8% CaO is insu~cient for complete stabiliza-
tion of zirconium dioxide. It is possible that the activation en-
er~¢ of 560 - 620 Ll/mole can be referred to the fluorite type
of creep in cubic solid solutions. It is also possible that the
microstructure also has some effect, because the crystal size
in composition 1 is noticeably smaller.
are liable to destabilization during use at high temperatures,
i.e., to disintegration of the solid solution occurring in the
1200- 1400°C interval. The destabilization is accompanied
by evolution of a trigonal phase, which, when cooled to tem-
into a monoclinic phase. Disintegration of solid solutions
starts from crystal boundaries and penetrates their depth.
In order to determine the effect of destabilization on the
creep we tested specimens of composition 3 (see Table I)
that were first subjected to thermal treatment at 1200°C for
200 h. X-ray phase analysis showed that these ceramics had
5% of monoclinic zirconium dioxide. The temperature de=
pendence of creep for these specimens is compared with that
for the initial composition 3 in Fig. 8, where we can see that
the deformation rate after dcstabilization is somewhat higher
than in the initial ceramics. This may be associated with the
formation of new ~'ain interfaces. It should be noted that at
furthermost stabilization stages, when the content of the new
phase becomes substantial, the increase in the deformation
rate can be rather large.
Second crystalline phase. The effect of the presence of
the second crystalline phase was investigated within a wide
range for ceramic materials in a periclase-magnesium alumi,
hate system [9]. Even for small contents of the second com-
ponent the effect of the solid solution formed is also ob-
served.
The components of the M g O - M~A1204 system form a
eutectic with a composition o f 45o/82 MgO and 55% AhO3
and a melting temperature o f 1995°C (by other dam 2030°C).
The system exhibits regions of solid solutions o f aluminum
ions in periclase and magnesium ions in spinel. Periclase and
spinel solid solutions exist in considerable amounts at tem-
peratures exceeding 1500°C. They are formed by substitution
starting from temperatures of about 1200 - 1300°C, with ca-
tion vacancies arising in periclase solid solutions and anion
2 Hereand belowwe givemassfractions.
H i g h - T e m p e r a t u r e Creep in Refractory Ceramics 281

t2 '51 +1 6Y°r
3 .$ 4
o 340~ ~ c
170
N
I I I I
.Ul

+t
0 10 20 30 40 50 60 70

MgO Mass fraction,% AI203

-4 5
I Fig. 10. Variationof creep activationenergy Q as a functionof the compo-
2
-5 I 0 --
4+5 5.0 5.5 --0.5 o 0.5
104/ T, K-1 log cr (MPa)
Fig. 9. Deformationrate in specimensof the periclase-magnesiumaluminate
systemas a functionof temperature(a) at 0.6 MPa and load(b). The numbers
at the lines denote the compositions of the specimens in accordance with
Table2.
vacancies arising in spinel solid solutions. Maximum solubi-
lity of aluminum oxide in periclase is observed within 8 2 -
83% MgO contents, which corresponds to dissolution of
nearly 9.5% of A13÷. The greatest solubility of magnesium
oxide in spinel occurs at 39% MgO, which corresponds to
dissolution of about 6% of Mg 2÷ [ 10].
The characteristics of experimental specimens are given
in Table 2.
The change in the creep rate with temperature is pre-
sented in Fig. 9a and its change with load is given in Fig. 9b.
Within the studied range of the variables in both cases we ob-
tained linear dependences (in the chosen coordinates) for all
specimens, which verifies that the empirical creep law is ap-
plicable to the given bicomponent system.
The lowest deformation rate for a given temperature and
load is exhibited by pure components. A small addition of
aluminum oxide to periclase affects its creep only slightly
(compare lines 1 and 2 in Fig. 9a). A large content of the
second component (up to 8%) leads to a sharp increase in the
deformation rate (by 1 - 2 orders of magnitude). Specimens
with composition 4 show the largest rate of the process.
Specimens with intermediate compositions behave in virtu-
ally the same way.
sitionof a ceramicsin the perielase- magnesiumaluminatesystem.
15
- - 13 1600°C fl
1700°C ,,r'
j
12 I 1 . I I I
0 10 20 30 40 50 60 70
MgO Mass fraction,% AI203
Fig. 11. Isothermsof effective viscosity(rl ~ I/e) of a ceramics in the peri-
clase- magnesiumaluminatesystem.
The activation energies calculated from the slope of the
dependence of log ~ versus 1/T are shown in Fig. 10. It
should be noted that the activation energies of compositions
close to periclase and spinel have minima and the quantities
Q for intermediate compositions are virtually the same. The
formation of solid solutions upon introduction of small addi-
tions o f MgO into spinel and o f aluminum oxide into MgO
leads to the appearance o f excess structural vacancies and
lowering of the activation energ3'. A further increase in the
share of the second component ensures the appearance of
crystals of the other phase and increases the activation ener-
gy. The virtually identical values o f creep activation energy
of intermediate compositions can be regarded as a conse-
quence of like structures of the specimens, where the spinel
and periclase grains have approximately equal sizes. It seems
that here we are dealing with the behavior of a eutectic mix-
ture whose crystals contain a certain number of structural va-
cancies.

TABLE 2, Characteristicsof CeramicSpecimensinthe MgO- MgAI204System

Deformationtemperature
Dominatingcrystal size, pan ob~d, MPa at 0.2 MPa, *C
Spinel Relative
Composition fractionin
total mass, % density,% MgO MgAI204 20°C 1450°C melting 4%
initiation compression
1 0 96.5 30 - 50 -- 105 40 2300 2410
2 5.3 98.0 30 -60 2- 5 127 40 2050 2200
3 10+2 98.5 20-45 2-5 145 50 2020 2180
4 t9.1 99.0 15 -30 3-5 180 62 1950 2040
5 55.1 98.5 5- 7 5- 8 222 66 1800 1850
6 76.7 98.2 4- 5 10-20 238 73 1820 1880
7 87.5 98.0 65 10-25 230 69 1850 1925
8 100 95.5 -- 10-20 150 48 1960 2040
282
2800
2400 ~
2000
! ! ! ! ~
0 I0 20 30 40 50 60 70
MgO Mass fraction, % AI20~
Fig. 12. Change in some parameters of a ceramics in the periclase-rnagne-
slum aluminate system as a function o f the composition. Temperatures:
1) of the liquidus; 2) of melting initiation under load; 3) of a viscosity of
3 × 1012 Pa. sex (with respect to creep).
-5 I
4.6 5.0 5.4
104/r,K -~
Fig. 13. Creep (at 2 MPa) in a densely sintered ceramic based on yttrium
oxide without (I) and with additionsof 2.7% zirconium dioxide (2) and 0.5%
alumina (3).
For all compositions the index n is close to 1, which cha-
racterizes the observed determation process as a viscous flow.
Isotherms of effective viscosity are presented in Fig. 1 I. In-
termediate compositions have virtually the same viscosities,
which are about one and a one-half orders of magnitude less
than the viscosities of periclase and spinel. As the tempera-
ture changes by 100°C, the viscosity changes by half an order
of magnitude, while the nature of the curves is preserved.
Curve 3 in Fig. 12 shows the dependence between the
temperature corresponding to an apparent viscosity of about
3 × 1012Pa. sec (calculated from the creep) and.composition.
It virtually corresponds to the nature of the temperature
change during the initial melting under loading. It is notewor-
thy that curves 2 and 3 do not follow the liquidus tempera-
ture; in the region of intermediate compositions the deforma-
tion characteristics are slightly dependent on the composition
of the components. This implies that creep is determined by
the behavior of most high-melting (and fine-crystal) part of
the microstructure, namely, the eutectic mixture, which prob-
ably formed by diffusion during high-temperature firing of
the specimen.
Vitreous phase. Figure 13 presents experimental data
[I 1] on creep in ceramics based on yttrium oxide without and
with additions of aluminum dioxide and zirconium oxide.
Zirconium dioxide does not form low-melting compounds
V.S. Bakunov
-I
-2
-3
-4
-5
0 5.0 5.5 6.0
1041 T, K "I
Fig. 14. Temperature dependence of the deformation rate in a densely sin-
tered muIlite ceramics loaded to 2.5 MPa. The numbers at the curves indicate
the total amount o f additiom, %.
with yttrium oxide but gives a dense free-grain structure. The
introduction of alumina leads to the formation of a second
phase that supposedly consists of yttrium aluminate with a
lower melting temperature. This phase is mainly exhibited as
fine intergrain layers. The dominating crystal size in speci-
mens 1 - 3 is 50 - 60, 5 - 7, and 50 - 55 ~m, respectively.
It can be seen from Fig. 13 that the lowest deformation
rates are found in ceramics without additions. Next come
specimens with zirconium dioxide additions. In this case the
increase in the deformation rate is explained by smaller crys-
tal sizes. The formation of a low-melting compound causes a
substantial increase in the deformation rates of A1203 speci-
mens despite the considerable size of their crystals. This is as-
sociated with the fact that at the test temperatures the cera-
mics exhibits a liquid phase. Thus, even a small amount of
additions, if they lead to the formation of low-melting com-
pounds, sharply increases the high-temperature deformation
rate provided that these compounds are distributed continu-
ously. Such deformation occurs as a viscous flow (the index n
in the power dependence of creep versus stress is close to 1).
A more complex case of creep was investigated for a
densely sintered synthetic mullite ceramics [6]. In their ther-
momechanical, chemical, and other properties such ceramics
are close to the materials made of pure oxides. The use of
clays and kaolins containing large mounts of impurities in
manufacturing mullite refractories affects the properties of
articles negatively. At high temperatures the additions cause
formation of a large amount of vitreous phase, which notice-
ably lowers the operating temperature of such materials.
We prepared the specimens from experimental mixtures
based on pure preliminarily synthesized mullite and mullite
contaminated by LT1 Latnensk clay. The composition of the
mixtures and some characteristics of the specimens are given
in Table 3. X-ray analysis and petrographic examination
show that the crystalline phase in all specimens consists of
multite. A vitreous phase is observed near the crystal bounda-
ries and its content ~ o w s with the amount of introduced clay
with a continous distribution.
High-Temperature Creep in Refractory Ceramics 283

TABLE. 3. Characteristicsof Specimensofa Mullite Ceramics efficient of viscosity is structure-sensitive and depends on the
Total Amountof Cbend, Ti.m, structural state of the phases, i.e., the distortion o f the lattice
amount of Papp- Popen, vitreous MPa, *C and the size of the crystals. The presence of crystalline inclu-
g/cm ~ %
additions, % phase, % at 20"C sions in a viscous matrix o f a low-melting phase raises the
0 3.02 0.3 0 130 1760 coefficient of viscosity.
0.5 2.96 0.2 5 210 1670
1.0 2.96 0.I 10 200 1630
2.0 2.95 0 20 175 1610 REFERENCES
Calculated. 1. V. S. Bakunov, "High-temperature creep in refractory ceramics.
Kinetics and the effect of experimental conditions," Ogneupory,
No. 6, 2 - 8 (1994).
It is seen from Table 3 that at room temperature speci- 2. V. S. Bakunov, "High-temperature creep in refractory ceramics.
Moving forces and mechanisms," Ogneupory, No. 7, 1 2 - 17
mens containing fusing agents have greater strength, which (1994).
may be explained by better bonding of the mullite phase by 3. D. N. Poluboyarinov, E. Ya. Shapiro, V. S. Bakunov, and
the vitreous phase. The temperatures at which the specimens F. A. Akimov, "Change in electrical conductivity and creep rate
start to deform under load are correspondingly lowered upon in a CeO2 ceramics during reduction," Izv. Akad. Nauk SSSR,
Neorganicheskie Materialy, 2(2), 336 - 3 4 2 (1966).
introduction of the impurities.
4. P. Kofstad, Nonstoichiometry, Diffusion and Electrical Conduc-
Figure 14 presents the temperature dependence o f creep tivity in Binary Metal Oxides, Wiley, New York (1972).
in the mixtures studied. The introduction o f even 0.5% fusing 5. F.A. Akopov and D. N. Poluboyarinov, "Some properties of a
agents sharply increases the deformation rate. In clay- and si- sintered ceramics of cerium dioxide," Ogneupory, No. 4,
lica-based mullite specimens the deformation rates at a given 37-41 (1965).
6. V. S. Bakunov, Wu Ngok Kyong, D. N. Potuboyarinov, et at.,
load and temperature are 2 - 3 orders of magnitude higher "Investigation of some properties of a densely sintered mullite
than in fluxless specimens. It should be noted that the afore- ceramics," Ogneupory, No. 4, 32 - 39 (1974).
mentioned 2 : 1 ~ 3 : 2 transition o f the mullite composition 7. E. B. Kroll and D. N. Poluboyarinov, "Sintering and properties
is also observed in specimens containing clay. In this case an of a mutlite ceramics," in: Proceedings of the Research Institute
of Structural Ceramics, NIIstroykeramiki, Moscow, Issue 24,
increase in the total amount of fluxes increases the content of 133 - 157 (1964).
the vitreous phase in the specimens, which affects the defor- 8. I. M. Demonis, R. Ya. Popilskii, E. Ya. Shapiro, and
mation rate and gradually eliminates the role of the indicated D. N. Poluboyarinov, "Investigation of creep in a ceramics
transition. based on zirconium dioxide," in: Proceedings of the Mendeleev
For all mullite compositions studied the exponent o f the Chemical and Technological Institute, MKhTI ira. Mendeleeva,
Moscow, Issue 54, 146- 150 (1967).
power dependence o f creep versus stress is close to 1, which 9. D. N. Poluboyarinov, R. Ya. Popilskii, I. P. Galkina, and
indicates that the deformation occurs as a viscous flow. V. S. Bakunov, "On creep in ceramic materials in the M g O -
MgA1204system," Izv. Akad. Nauk SSSR, Neorganicheskie Ma-
terialy, 2(6), 1115 - 1118 (1966).
CONCLUSIONS 10. A. M. Alper, R. N. McNally, P. H. Ribbe, and R. C. Doman,
"The system MgO-MgA1204," J. Am. Ceram. Soc., 45(6),
HigJa-temperamre creep in multiphase ceramics can be 263 - 268 (1962).
11. L. B. Borovikova, E. S. Lukin, D. N. Poluboyarinov, and
controlled either by diffusion flow of polycrystalline materi- V. S. Bakunov, "Creep in a ceramics based on yttrium oxide,"
als or by viscous flow in the presence a continuously distri- lzv. Akad. Nauk SSSR, Neorganicheskie Materialy, 10(5),
buted vitreous or low-melting phase. In diffusion flow the co- 29-31 (1974).