MECHANICAL BEHAVIOR OF ZIRCONIUM DIOXIDE CRYSTALS PARTIALLY

STABILIZED WITH YTTRIUM OXIDE

G. A. Gogotsi, A. V. Drozdov, UDC 539.3/4:666.3

and V. G. Peichev

The results are given of a composite investigation of the mechanical behavior of

single crystals of zirconium dioxide partially stabilized with yttrium oxide and
ytterbium oxide at temperatures up to 1400~ It is shown that the elastic modulus
of these materials lies in the 150-350 GPa range and their tensile strengths may
reach 1,688 MPa. These materials have a nonincreasing relationship of the stress
intensity factor to crack length (flat R-curves). The stress intensity factors
determined on specimens with a sharp crack are significantly lower than on specimens
with a notch. The picture of fracture of single crystals in penetration of an
indentor, etc. differs significantly in relation to the stabilizing addition~

Recently there has been much interest in single crystals of partially stabilized zirco-
nium dioxide, the primary feature of which is a quite high strength and crack resistance and
also increased fracture toughness under 1500-1600~ temperature conditions [I], which is not
characteristic of other ceramic materials in heating in air. A series of investigations has
been made of such single crystals partially stabilized with oxides of yttrium and ytterbium,
gadolinium [2], and calcium and magnesium [3]. Various characteristics of this type of mate-
rials have also been studied [4].
In investigation authors have attempted to analyze in detail the elastic anisotropy
of zirconium dioxide crystals [5], to explain their possible high crack resistance by fer-
roelastic effects [6], etc. As far as it is possible to judge from the results of published
works, the greatest attention has been devoted to crystals partially stabilized with yttrium
oxide [4], which is most promising for production use.
This investigation was made for the purpose of assembly of new information on the mecha-
nical behavior of this type of materials and of revealing features of the physicomechanica!
properties of some of them developed in the USSR. The materials for the study were obtained
by the known method of withdrawal of crystals from molten material [4] formed in induction
heating of a charge in a cold crucible. In preparation of them the Donets unit of Verkhnedne-
provsk Mining and Metallurgical Combine, which was designed for experimental production of
cubic zirconium dioxide crystals, was used [7].
Two materials were investigated, crystals of Y containing 6 wt.% yttrium oxide as a
stabilizing addition and crystals of Y-Yb containing a stabilizing addition in the form of
1.5 mol.% yttrium oxide and 1.5 mol.% ytterbium oxide.
To obtain a fuller picture more than one lot of specimens of each material was used in
the tests (to distinguish them the letters "a-d" were added to the designations of the mate-
rial). The specimens of the first lot differed from one another primarily in uncontrolled
features of the method since they were prepared at different times. The lot of Y-a crystals
corresponded to the material studied earlier in [7] while for the remaining lots of specimens
of this material the accuracy in maintaining the technological parameters in preparation of
them was increased somewhat. The specimens of the second material were withdrawn from the
molten material at different rates (the letters "a" and "b" disignate lower and higher rates,
respectively).

Institute of Strength Problems, Academy of Sciences of the Ukrainian SSR, Kiev. The
All-Union Scientific-Research Institute for Power in Nonferrous Metallurgy, Sverdlovsk. Trans-
lated from Problemy Prochnosti, No. i, pp. 73-77, January, 1991. Original article submitted
July 27, 1990.

86 0039-2316/91/2301-0086512.50 9 1991 Plenum Publishing Corporation

 @, 4Pa
O

O 9 O 9
~8
o 9

800

d0 Fig. i. Results of study of the

elasticity and strength of Y-e
o~
200 crystals: i) static elastic
e2
modulus Est; 2) dynamic elastic
0 R I I modulus E d.
180 T80 E s t , Ed, G P a

Fig. 2. Sources of fracture of specimens in bending: a) Y-a

crystal, o = 626 MPa; b) Y-b, o = 1,290 MPa; c) Y-b, o = 451
MPa; d) Y-b, o = 1,247 MPa.

Specimens of the materials studied were cut from crystals grown in the form of rods
with an average diameter of -10-30 mm and length of 30-70 mm. The surfaces of the specimens
were ground parallel to their axis and the faces rounded. The direction of the axis of the
specimens in relation to the axes of the cubic matrix of the crystals was not identified.
All of the crystals (as for those investigated in [7]) had a milk-white color and in
some of them dark veins probably perpendicular to the axis of growth of the crystal were
observed. The crystals were made up of a cubic matrix with finely dispersed tetragonal pre-
cipitates (the method of their preparation is described in detail in [7]).
The investigations were made using known methods developed in the Institute of Problems
of Strength of the Academy of Sciences of the Ukrainian SSR [8] and which were used earlier,
including those for study of zirconium dioxide-base polycrystalline materials ([9, 10], for
example).
In the initial stage of the work the values of the dynamic and static elastic moduluses
were investigated and then an attempt was made to reveal the relationship between them and
the strength of the materials (Fig. I).
For the most representative lot of specimens of Y-b material (88 specimens) the variation
coefficient of the dynamic elastic moduluses was 21% with a minimum value of 168 GPa and a

87
 1/2
Kzc ' MPa"m

~, M P a i

80O

40O

20~
I i _
500 ~ODO T,~ 500 ;000 T."C

Fig. 3 Fig. 4
Fig. 3. Temperature relationships of strength for Y-b (i), Y-Yb-a (2), and
Y-Yb-b (3) crystals.
Fig. 4. Temperature relationships of the critical stress intensity factors
Kic. (Designations the same as in Fig. 3.)

maximum of 346 GPa. In the latter case the three-point bend strength was 1,335 MPa, for the
lot of specimens of Y-d material with E d = 352 GPa it was 1,244 MPa, and for the lot of speci-
mens of Y-a material with E d = 339 GPa 626 MPa. For Y-Yb-a material the variation coeffi-
cients obtained were the same. However, for the specimen having a dynamic elastic modulus
of E d = 350 GPa (maximum value in the lot) the four-point bend strength to a base of 20[40 mm
was 903 MPa and in subsequent three-point bend testing of the remainder of this specimen to
a base of 20 mm 1,668 MPa.
In general it was observed that for specimens of the same lot basically the relationship
of an increase in strength with an increase in elastic moduluses is observed. However, in
different lots different strengths correspond to the same elastic moduluses. This is caused
by structural defects of the single crystals not recorded in measurement of the rate of travel
of the ultrasonic wave from the values of which are calculated the dynamic elastic moduluses
and in measurement of the deflections of the specimens from which are determined the static
elastic moduluses.
The difference in elastic moduluses of specimens of materials of the same lot is probably
related to the different orientation of the axis of the specimens relative to the axis of the
single crystal. For example, the axis of the above mentioned specimen of Y-a material coin-
cided with the <100> direction. Let us recall that in [5] the highest (-360 MPa) values of
the elastic moduluses were obtained in the <100> direction and the lowest (-170 GPa) in the
<iii> direction, which approximately corresponds to the spread in results of our measurements.
Taking into consideration the significant spread in properties in the lots of specimens,
to determine the strength and crack resistance specimens with average values of the elastic
moduluses (>190 GPa and <220 GPa), which corresponds to the average value of the elastic
modulus given in the literature for single- and polycrystalline ZrO 2 ceramic of about 200
GPa, were selected.
Strain curves of the studied crystals were considered. All of them were linear with
X = 1 (we should note, looking ahead, that for these materials and in further high-temperature
tests they remained linear).
The sources of fracture of the test specimens were either surface defects (Fig. 2a, b)
or stress raisers on the faces of the specimens (Fig. 2c, d). It was characteristic that the
stronger the specimen, the rougher the fracture surface for it. Pore-type defects were ob-
served in the fractures of Y-a material specimens.
In high-temperature tests a more significant reduction in strength was observed (Fig. 3)
than in the case, for example, of the materials studied in [I] but at the same time the values
of strength were more than those recorded in investigation of a zirconium dioxide-base poly-
crystalline ceramic containing yttrium oxide [ii]. The picture of the temperature changes

88
 F /2
/<I ,MPa" m i

P, Ni P, N 5 21//
30 30

20

5
10

] I I L 0
5 fO 15 20~,,pm 0 5 5 9 12N,IOs 0,5 1,0 t,5 2,0~ c r , uan
a b
Fig. 5 Fig. 6
Fig. 5. Force P-deflection ~ (a) and force P-total acoustic emission count N (b)
relationships for Y-Yb-a crystals.
Fig. 6. R-curves of single crystals. (Designations the same as in Fig. 3; ~cr
is the length of a sharp crack.)

in the critical stress intensity factors obtained on specimens with a notch was approximately
the same as that found by other authors [i] (Fig. 4).
In addition to evaluate the crack resistance the relationships of the stress intensity
factor to length of the growing crack (R-curves of these materials) were determined, which is
of special interest for zirconium dioxide-base ceramics.
First a relatively short crack (0.2-1 mm) was formed in specimens with a notch and then
they were cyclically bent, causing in each load cycle an increase in crack length, which was
measured on the force P-deflection ~ diagram (Fig. 5a). The crack length was calculated from
the pliability of the specimen (the method was described earlier [12]). The results of such
measurements for certain specimens are shown in Fig. 6. From a comparison of the data shown
in Figs. 4 and 6 it follows that in testing specimens of Y and Y-Yb materials with cracks
formed they had lower values of stress intensity factors than simple notched specimens. Con-
sequently for these materials there is a barrier to fracture, which is characteristic of other
brittle (X = i) ceramic materials [12].
In connection with the results obtained the question arises of to what degree brittle
(in this case single crystalline) zirconium dioxide-base materials may be assumed to be duc-
tile? We should note that under real conditions fracture of a ceramic part normally occurs
as the result of formation of a sharp crack and not a notch, using which the crack resistance
of a ceramic is traditionally determined.
In this work the total acoustic emission count in development of a crack in zirconium
dioxide-base crystals was recorded (Fig. 5b). Since the acoustic emission process is charac-
teristic in fracture of heterogeneous materials, a possible reason for acoustic emission in Y
and Y-Yb crystals may be the presence of the tetragonal precipitates in the cubic matrix,
which leads to interrupted emission of elastic waves in crack development.
In investigation of the resistance of the surface of the ceramic considered to penetra-
tion of a Vickers indentor as by other authors [i, 3, 4] it was established that the hardness
of all of the materials is practically the same and is primarily 12-14 GPa. The critical
stress intensity factors were determined in relation to the force applied to the indentor,
which was varied from 50 to 500 N. For Y-b and Y-Yb-b materials it was within limits of
10-4.3 and 13.7-5.7 MPa'm89 respectively.
We should note that when the crack resistance of one material or another is determined
from the resistance to development of a sharp crack preference belongs to a Y-Yb-a crystal.
It is characteristic that crystals with the addition of ytterbium and without it fail dif-
ferently under the action of an indentor (Fig. 7). In the Y-b material lateral (Hertz)cracks
perpendicular to penetration of the indentor:appear (Fig. 7a) while in the case of Y-u
material on the faces of the impression there may be seen light zones where there occurred
a phase transformation (Fig. 7c) similar to that observed in [13] for a tetragonal polycrys-
talline material of zirconium dioxide with addition of 2% yttrium oxide.

89
 Fig. 7. Portions of the surface of specimens indented with a load of 50 N: a) Y-a
crystal (light photograph); b) the same (electron photograph of the surface of a
specimen coated with a thin electrically conducting layer); c) Y-Yb-a crystal (light
photograph).

In general the data obtained indicates the promise of creation of crystals stabilized w i t h
ytterbium oxides since in this case the strength and actually the crack resistance of materials
of such a type may be increased.
LITERATURE CITED
i. "Temperature dependence of strength and fracture toughness of ZrO 2 single crystals,"
J. Am. Ceram. Soc., No. 9, 150-152 (1983).
2. D. Michel, L. Mazerolles, and M. Jorba, "Fracture of metastable tetragonal zirconia
crystals," J. Mater. Sci., 18, No. ii, 26-28 (1983).
3. R. P. Ingel, D. Hevis, B. A. Bender, and R. W. Rice, "Physical, microstructural and
thermomechanical properties of a ZrO 2 single crystal," Science and Technology of Zir-
conia, Vol. 12 (1984), pp. 408-414.
4. D. J. Creen, R. H. J. Hannink, and M. V. Swain, Transformation Toughening of Ceramics,
CRC Press, Florida (1989).
5. R. P. Ingel and D. Lewis, "Elastic anisotropy in zirconia single crystals," J. Am. Ceramo
Soc., 71, No. 4, 265-271 (1988).
6. A. V. Virkar and R. L. K. Matsumoto, "Ferroelastic domain switching as a toughening
mechanism in tetragonal zirconia," ibid., iO, No. 3, 224-226 (1986).
7. K. Strelov, V. G. Peichev, S. Yu. Pliner, et al., "The properties of partially stabilized
zirconium dioxide," Ogneupory, No. 8, 5-6 (1988).
8. G. A. Gogotsi, "Problems of certification of machine building ceramics for their strength
indices," Vestn. Mashinostr., No. 18, 50-52 (1989).
9. G. A. Gogotsi, A. V. Drozdov, and M. V. Svein, "The strength, crack resistance, and
acoustic emission of ZrO2-base ceramic," Probl. Prochn., No. i, 34-44 (1991).
i0. I. F. Usatikov, E. I. Zoz, R. E. Vol'fson, et al., "Partially stabilized zirconium
dioxide-base ceramics," Ogneupory, No. 5, 17-20 (1990).
ii. G. A. Gogotsi, Yu. I. Komolikov, D. Yu. Ostrovoi, et al.~ "The strength and crack resis-
tance of a zirconium dioxide-base ceramic," Probl. Prochn., No. I, 50-52 (1988).

90
12. G. A. Gogotsi, V. P. Zavada, A. I. Fesenko, et al., The Crack Resistance of a Zirconium
Dioxide-Base Ceramic [in Russian], Deposited in the All-Union Institute for Scientific
and Technical Information 4/25/89, No. 2690 V-89.
13. T. R. Lai, C. L. Hogg, and M. V. Swain, "EvaluatiOn of fracture toughness and R-curve
behavior of Y-TZP ceramics," ICIJ Intern., No. 3, 240-245 (1989).

EVALUATION OF THE INFLUENCE OF THE SCALE FACTOR ON THE

FRACTURE OF RODS

V. N. Yuzevich UDC 539.3:539.4:532.6

On the basis of the energy criterion of fracture a method of calculation of the

relationship of the strength of quasibrittle rods in uniaxial tension and bending
of rectangular and round cross section to their geometric dimensions was devel-
oped. With use of the analytical relationships obtained and known experimental
data it is shown that with an increase in loading rate of the bodies being deformed
the influence of the surface layer simulated by a physical surface on the strength
of glass specimens first drops to a minimum value and then steadily increases.

An important problem in the mechanics of solids is calculation of the strength properties

of surface and interphase layers in structural elements of complex composition [i]. During
deformation their boundary areas influence the volumetric portion of the material and the
service characteristics of the specimens as a whole.
In this work with use of the energy criterion of fracture [2] and based on the mechanical
properties of the surface layer relationships are developed for evaluation of the influence
of the scale factor on the change in strength of solids in uniaxial tension, bending, and
compression in relation to geometric dimensions.
Let us consider a specimen of a quasibrittle material with a length of s a width of b,
and a thickness of h uniformly in tension by a stress of o in the direction of length. Let
fracture consist of rapid separation of the specimen into two parts. In this case the area
of projection of the surface which was formed after fracture on the plane perpendicular to
the axis of the rod (the axis parallel to ~) is equal to bh.
Let us simulate the body being deformed by a composite medium consisting of a uniform
core and a surface area with an effective thickness of x, which is taken as constant for the
given material of the rods and independent of deformation [3]. Subsequently we will take
into consideration the smallness of x in comparison with the dimensions of the test specimens,
which makes it possible to replace the boundary layer not resisting bending with a physical
surface [4] with characteristics inherent in it reflecting the mechanical and other physico-
chemical properties of the surface area. In should be noted that the properties of the bound-
ary layer differ from those of the core [5].
The elastic energy accumulated in the body U = 0.5 o2bhs [2], where E is the modulus
of longitudinal elasticity in the direction of tension and o is the tensile stress, parti-
cularly the tensile strenth.
Let us present the work for fracture of the specimen in the form

A : kV + ? S f + ~S e 4- q~L, (I)
where Sf = bh is the projection of the area of the fracture surface, S e is the area of the
external surface of the body, L is the projection of the perimeter of the cross section of
the rod, L = 2(h + b), k is a parameter characterizing the loss of energy in the volume V
of the body, ~ is a parameter characterizing the loss of energy in the surface layer, the
volume of which is approximately equal to Sex (~ is per unit area of the external surface),
.... institute of Applied Problems of Mechanics and Mathematics, Academy of Sciences of the
Ukrainian SSR, L'vov. Translated from Problemy Prochnosti, No. i, pp. 77-79, January, 1991.
Original article submitted June 21, 1990.

0039-2316/91/2301-0091512.50 9 1991 Plenum Publishing Corporation 91