Materials Transactions, Vol. 44, No. 9 (2003) pp.

1783 to 1789
#2003 The Japan Institute of Metals

The Kinetics of Isothermal Martensitic Transformation

of Zirconia Containing a Small Amount of Yttria
Jae-Hwan Pee1; * , Takahiro Akao1 , Shigeru Ohtsuka2 and Motozo Hayakawa1
1
Department of Mechanical Engineering, Tottori University, Tottori 680-8552, Japan
2
Department of Mechanical Engineering, Yonago National College of Technology, Yonago 683-8502, Japan

The high temperature tetragonal phase of zirconia containing 1.401.60 mol% Y2 O3 were successfully quenched in at room temperature
by rapid cooling of small spherical specimens. On these metastable specimens, the isothermal transformation behavior into the monoclinic phase
was studied by dilatometric method. The transformation start time exhibited a C-curve in a TTT diagram. The C-curve shifted toward short time
side as well as toward high temperature side with decreasing yttria content or increasing grain sizes. A study of the pre-aging eect during the
incubation period on the subsequent isothermal transformation suggested consecutive growth of embryos, but alternative interpretation was also
possible. The activation energy was evaluated to be
50 kJ/mol.

(Received May 22, 2003; Accepted July 22, 2003)

Keywords: zirconia-yttria alloy, martensitic transformation, isothermal transformation, time-temperature-transformation diagram, compo-
sition dependence, grain-size dependence, activation energy, dilatometric measurement

1. Introduction decreases almost linearly with increasing yttria content up to

1.75 mol% Y2 O3 , but beyond which no transformation takes
The phase transformation from the high temperature place not only during cooling to room temperature but also by
tetragonal to the monoclinic phase of zirconia has long been a subsequent cooling to the liquid nitrogen temperature.2)
considered to be a typical athermal type martensitic trans- This disappearance of the transformation is so sudden that it
formation. Historically, Wolten1) was the rst to suggest the is dicult to be accounted for by a reduction of Ms with
athermal nature of the transformation. He conducted a high increasing amount of yttria.
temperature X-ray experiment and observed a large hyster- On the other hand, as also shown in Fig. 1, Y-TZP (Yttria
esis between the forward and backward transformation as doped Tetragonal Zirconia Polycrystals), which contain 2.6
well as stagnation of the transformation when the temper- 3.0 mol%Y2 O3 , are well known to exhibit isothermal trans-
ature was halted during the transformation. These observa- formation when annealed at around 550 K causing a sever
tions led him to conclude that the transformation was an degradation in the mechanical properties.35) The isothermal
athermal type martensitic transformation. transformation takes place faster with decreasing yttria
Since zirconia doped with a small amount of yttria behaves content. Thus, it was suggested that if the athermal nature
similarly except for the decreasing transformation temper- of the transformation observed in the low yttria composition
ature with increasing yttria content, the transformation mode range is interpreted as a result of increased transformation
has also been considered to be the same. As illustrated in rate due to the reduced yttria content so that the C-curve
Fig. 1 after Ref. 2), the Ms (martensite start temperature) becomes intersected by the cooling curve in the TTT (Time
Temperature Transformation) diagram, the above mentioned
sudden disappearance of the transformation beyond
1500 1.75 mol% Y2 O3 can be accounted for.
Evidence for the validity of such interpretation, namely the
1300 isothermal transformation behavior in the lower yttria region,
Ms and A s , T/K

1100 As can be found in the literature.2,6,7) Among all, Hayakawa et

al.2) found not only that the transformation temperature was
900 dependent on the cooling rate but also the parent phase could
Ms
be fully retained at room temperature for a certain compo-
700
sition range below 1.75 mol% Y2 O3 by a rapid cooling. The
Isothermal
500 Transformation metastable tetragonal phase obtained by such a fast cooling
readily transformed into the stable monoclinic phase by
300
heating at around 550 K as expected from the isothermal
0.0 1.0 2.0 3.0 nature of the transformation. More interestingly, the
Y 2O3 content, x/mol% quenched metastable tetragonal phase underwent a burst
type martensitic transformation into the monoclinic phase
Fig. 1 The variation of Ms and As (reverse transformation start temper- during a subzero cooling to the liquid nitrogen temperature.
ature) with Y2 O3 composition for bulk specimens measured with a
continuous cooling and heating of 200 K/h2) along with the region of the
The occurrence of both isothermal and athermal modes of
isothermal t  m transformation4) after Ref. 2). transformation in an alloy of a composition is very rare and
no other system is known to transform at so dierent
*Graduate Student, Tottori University.
1784 J.-H. Pee, T. Akao, S. Ohtsuka and M. Hayakawa

temperatures as in the present case.

The isothermal nature of zirconia doped with a small
amount of yttria has been recognized only recently.2,6,7) Even
though it may be regarded as similar to the isothermal
transformation of TZP, the essential nature of the trans-
formation is not fully understood. In fact some researchers
consider the isothermal transformation of TZP is bainite-
like.8,9) In order to identify the rate controlling thermally
activated process and clarify the transformation mode,
quantitative measurements of the kinetics are necessary. In
the present study, the kinetics of the isothermal transforma-
tion is studied with special interests in its dependence on the
composition and grain size.

2. Experimental Procedures

Series of specimens of dierent compositions, ZrO2 1.30

1.55 mol%Y2 O3 (1.301.55Y) were prepared from pure
zirconia and ZrO2 3.0 mol%Y2 O3 powders (TZ-0 and TZ-
3Y, TOSOH, Japan), both having 99.9% purity. Weighed
powders for a given composition were mixed in a zirconia
ball mill with ethanol for 50 h. After being dried, the mixed
powder was lightly ground with a mortar and pestle and
passed through a 100 mesh screen.
Small spherical specimens were prepared from the mixed
powders so that a fast cooling was possible to retain the high
temperature tetragonal phase after sintering. A mixed powder
was uniaxially pressed into a 1 mm-thick disk of 20 mm
diameter in a steel die under 200 MPa. The sheet was diced
with a knife-edge into cubes of 1 mm size. The cubes were
granulated in a rotating cylinder whose inner walls were lined
with emery paper. In about 24 h, beads of uniform diameter Fig. 2 SEM micrographs of a dense spherical specimen of ZrO2 1.6 mol%
were obtained. They were placed in a platinum crucible and Y2 O3 prepared for rapid quenching experiments: (a) low magnication
and (b) high magnication.
sintered at 17231873 K for 1 h in the ambient atmosphere.
To avoid isothermal transformation of the specimens during
cooling, they were taken out of the furnace when the furnace thin quarts rods; the specimen cell welded on one end of the
temperature reached 1273 K and rapidly cooled by immers- supporting rod was heated by focused infrared gold image
ing the outer surface of the crucible in water. Figure 2 shows furnace (Shinku-Riko, Model MR-55W, Yokohama, Japan)
SEM micrographs of a sintered specimen. and the displacement of the push rod was measured by a
The retention of the tetragonal phase after quenching was capacitance type transducer (MTI Accumeasure System,
examined by X-ray diraction method using Cu K
radiation. Model AS-2021SAI, USA). The maximum heating rate up to
For the specimens sintered at 1723 K, a full retention of the several hundred degree K was approximately 1000 K/min,
tetragonal phase was possible with the specimens containing but cooling rate was somewhat lower. Only specimens of
1.40 mol% yttria and more. Specimens sintered at higher good spherical shape and diameter between 600 and 700 mm
temperatures were less stable, but only specimens of fully were used for measurements.
tetragonal phase were used for the subsequent kinetic
measurement. The densities of successfully quenched speci- 3. Results
mens were higher than 98% as measured by the Archimedes
method. An average grain size of a sample was measured Dilatometric data obtained from the isothermal holding of
using the linear intercept method; the conversion factor 1.54 1.50Y specimens sintered at 1723 K are shown in Figs. 3(a)
was multiplied to the average intercept length measured over (f). To avoid overlapping of the dilatation curves, the data are
500 grains on the SEM micrographs taken from the cross- plotted in three separate temperature ranges ((a)(c)), and for
section of a sample. As seen in Fig. 2, equiaxed grains were each temperature range the early stage up to 300 s is re-
uniformly distributed. The average grain sizes increased with plotted with an expanded time scale ((d)(f)). Specimens
increasing sintering temperature but nearly independent on temperature reached a preset temperature within a time
the composition. For 1.55Y specimens, the grain sizes of between 30 and 50 s depending on the preset temperature. A
0.51, 0.63, 0.80, and 1.00 mm were obtained by sintering at small dilatation during this period was primarily due to the
1723, 1773, 1823, and 1873 K, respectively. thermal expansion of the specimen, which increased with the
A handmade micro-dilatometer2) was used for monitoring holding temperature. Then dilatation due to the transforma-
the transformation behavior. It was a push rod type made of tion followed a sigmoidal curve saturating at about 10 mm up
 The Kinetics of Isothermal Martensitic Transformation of Zirconia Containing a Small Amount of Yttria 1785

12 12
(a) (d)
10 10

Dilatation, L/m
Dilatation, L/m

8 8
653
6 6
573 533 493 613 573
4 653 4

2 613 533
2

0 0
0 1000 2000 3000 0 100 200 300
Time, t/s Time, t/s

12 12
(b) (e)
673
10 10
673
Dilatation, L/m

Dilatation, L/m
683
8 693 8 683
703
6 6 693

4 4
703
2 2

0 0
0 1000 2000 3000 0 100 200 300
Time, t/s Time, t/s

12 12
(c) (f)
10 10
Dilatation, L/m
Dilatation, L/m

8 8

6 713 6 733
753
733
4 753 4
713
2 2
0 0
0 1000 2000 3000 0 100 200 300
Time, t/s Time, t/s
Fig. 3 Dilatation curves of the isothermal transformation at various temperatures for the rapidly cooled specimens of 1.50Y sintered at
1723 K. (a) data for 493653 K, (b) data for 673703 K, (c) data for 713753 K; (d), (e) and (f) show the expanded early stage of (a), (b)
and (c), respectively.

to 653 K. Note that a complete transformation of a 700 mm increase of the holding temperature, the transformation
diameter specimen would yield an 11.7 mm linear expansion diminished. As seen in Fig. 3(c), transformation seemed to
assuming the lattice volume expansion was 5%. A well be still in progress at 713 and 733 K. On the contrary, the
dened plateau was observed at low temperatures. But this curve at 753 K appeared to show a gradual shrinkage of the
became shorter and eventually disappeared when the dilata- specimen. At rst sight, this phenomenon might appear
tions due to the transformation and thermal expansion merge suggesting a partial transformation by intersecting the nose of
at higher temperatures, say 653 and 673 K. With further C-curve during heating and a subsequent reverse trans-
increase of the temperature, the plateau tended to reappear formation at the holding temperature. However, this was
indicating a delay of the beginning of the transformation (at veried not the case by the fact that a heating of the same
temperatures 683 and 703 K in Fig. 3(b)). At these temper- specimen up to 1173 K with the same heating rate showed no
atures, the transformation behavior was no longer sigmoidal sign of reverse transformation around the expected As point
shape and was quite dierent from those observed at lower (
1073 K) in case a partial transformation had occurred
temperatures (see 693 and 703 K in Fig. 3(b)). With further during the heating.
1786 J.-H. Pee, T. Akao, S. Ohtsuka and M. Hayakawa

6 800 800
1.40Y
1.45Y

Temperature, T/K
Temperature, T/K
4 600 700
Dilatation, L/m

1.50Y
1.55Y
2 400 600
493
0 200 500
733
-2 400
0 500 1000 1500 10 100 1000 10000

Time, t/s Time, t/s

Fig. 4 Blank tests of the dilatometer at two dierent temperatures: 493 and Fig. 6 A TTT diagram showing C-curves for the transformation start time
for specimens with dierent yttria contents and sintered at 1723 K.
733 K.

To clarify the origin of this negative slope, a blank test was line at 743 K represents an approximate upper limit of the
conducted with the dilatometer at some temperatures. The isothermal transformation of the present sample. Although
results at 493 and 733 K are shown in Fig. 4. At 493 K the the low temperature data were limited by the time of
initial expansion due to the heating of the holder was measurement, a partial transformation to the monoclinic
maintained at constant. But at 733 K, after the initial phase was observed even at room temperature during an
expansion, gradual shrinkage was observed for quite an extended period of time. The isothermal transformation of
extended time. This seems to be caused by the gradual this sample proceeds quite fast and the usual cooling rate
temperature redistribution through the measuring system, employed for a bulk ceramic sample should have intersected
where only specimen cell was heated by a focused beam. the C-curve resulting in transformation, which seems to have
Since the apparent shrinking behavior of 753 K curve in Fig. been mistaken as athermal type transformation.
3(c) is the same as 733 K curve in Fig. 4, the former was Similar dilatometric measurements were conducted for
interpreted as showing neither forward nor reverse trans- specimens of dierent compositions and grain sizes to see the
formation. eect of the composition and grain size on the transformation
The transformation-start times as well as the times for 10% kinetics. The results are summarized as the transformation
and 50% transformation obtained from the above dilatomet- start time in TTT diagrams. Figure 6 shows the eect of yttria
ric curves were plotted in a TTT diagram in Fig. 5. The content on the C-curve for the specimens sintered at 1723 K.
transformation start time was read from the point of a denite Because the average grain sizes were essentially the same,
increment (roughly 2% of transformation) from the plateau. the eect of grain size could be ignored. The C curves shifted
But this criterion became more or less uncertain when a at toward the long time side as well as toward low temperature
plateau was absent. These times read from Fig. 3 were with increasing yttria content. Although this trend is
corrected for the time expended for heating to the preset qualitatively well expected from the stabilizing eect of
temperature for isothermal holding. yttria, it is worth noting that only 0.05 mol% addition of
The temperature dependence of the transformation kinetics Y2 O3 content resulted in a signicant delay in the trans-
was represented by typical C-curves: atter top and signi- formation start time. It is also noted that the reduction in the
cant temperature dependence below the nose. The horizontal nose temperature between 1.45Y and 1.55Y in Fig. 6 is
comparable with the reduction in the Ms (transformation
temperature during a continuous cooling) between the same
800 compositions plotted in Fig. 1.
2% Figure 7 shows the eect of grain size on the C-curve for
specimens of 1.55Y sintered at dierent temperatures. The C-
Temperature, T/K

700 10%
50% curves shifted toward the short time side as well as toward
higher temperature with increasing grain size. The behavior
600 is consistent with often reported un-stabilizing eect of grain
coarsening.1016) As an Ms point is inuenced by both T0
500 (equilibrium temperature between the chemical free energies
of the parent and martensite phases) and a critical driving
400 force (dierence in the chemical free energies to trigger the
nucleation of martensite), the position of a C-curve in a TTT
10 100 1000 10000
diagram can be considered to be inuenced by the same
Time, t/s parameters. Although the stabilizing eect due to yttria
Fig. 5 A TTT-diagram showing C-curves for 2% transformation, 10%
content is expected through the reduction of T0 and that due
transformation and 50% transformation for 1.50Y specimen sintered at to grain renement must be through the increased driving
1723 K. force required for triggering the transformation, these eects
 The Kinetics of Isothermal Martensitic Transformation of Zirconia Containing a Small Amount of Yttria 1787

800 tion start times for the subsequent aging as seen from the
0.51m shifted C-curves in Fig. 8(a). The result seems to imply that
0.63m some sort of preparation toward transformation or even
Temperature, T/K

700
0.80m subtle transformation below detection limit was in progress
1.00m during the incubation period; certainly not a stage of simple
600 waiting for a nucleation event governed by a statistical
probability. It was then examined if such a change during the
500 incubation period proceeded linearly with time until it
reached the critical state at the transformation start time. If
this hypothesis is correct, the eect of pre-aging for a certain
400
period (300 or 600 s) at 523 K can be regarded as equivalent
10 100 1000 10000
to the aging for tT0 at temperature T. That is:
Time, t/s
300 or 600
tT0 T 1
Fig. 7 A TTT diagram showing C-curves for the transformation start time 523
for 1.55Y specimens with dierent grain size.
where 523 and T are the incubation times (in unit s) at 523 K
and TK, respectively. Thus, the eective transformation start
800 time at T, tTtotal , for the specimens pre-aged at 523 K can be
(a) 0s evaluated by adding the eective contribution by the aging,
300s namely:
Temperature, T/K

700
600s tTtotal tT tT0 2
600 where tT is the observed transformation start time at T for the
specimen pre-aged at 523 K for 300 or 600 s.
500 The corrected transformation start times are plotted in Fig.
8(b), where we see that the eective time expended before
the transformation started after the pre-aging agreed well
400 with those for the as sintered specimens at all temperatures.
10 100 1000 10000 The result supports the initial hypothesis, namely a change
Time, t/s toward transformation proceeded linearly with time during
the incubation period.
800 Finally, activation energies were evaluated from the
(b) 0s presently obtained C-curves. Figures 9(a) and (b) show
300s Arrhenius plots of the reaction rates, which are taken as the
Temperature, T/K

700
600s inverse of the transformation start time in Figs. 6 and 7. An
activation energy was evaluated from the slope of the linear
600 portion of the Arrhenius plot which corresponds to the data
well below the nose temperature of C-curve.17,18) The data
500 presented by open symbols which denote the data near and
above nose of the C-curve were not used for the linear t.
400 Activation energies were about 50 kJ/mol, irrespective of
yttria content and grain sizes.
10 100 1000 10000
Time, t/s 4. Discussion
Fig. 8 (a) C-curves of the transformation start time for 1.55Y specimens
pre-aged at 523 K for 300 and 600 s in the incubation period as compared Isothermal nature of the tetragonal to monoclinic phase
with that of no pre-aging. (b) Same as (a) but the transformation start times transformation was clearly shown for zirconia doped with
were corrected for the pre-aging eect (see text). 1.401.55 mol% Y2 O3 . The isothermal nature is the same as
those observed in Y-TZP, which contains 2.53.0 mol%
on the C-curves were indistinguishable. Y2 O3 . The isothermal nature seems to extend to pure zirconia
As seen in Fig. 3(a), the isothermal transformation as veried by the time dependence of the transformation
behavior at lower temperatures was characterized by a well observed through the transformation temperature.6) The
dened incubation period before a detectable amount of reason why the t-m transformation of this composition range
transformation was observed. To see if any signicant change had long been considered to be typical athermal martensite
was occurring during this incubation period, the eect of pre- seems to be due to its fast reaction. In fact, the time intervals
aging on the subsequent isothermal transformation was of X-ray measurement used for monitoring the transforma-
studied. Figure 8(a) shows the eect of the aging treatments tion by Wolten1) were longer than 30 min, by which time the
at 523 K for 300 and 600 s on the subsequent transformation amount of transformation must have well saturated to the
start times. Although these aging treatments were well within value prescribed by the temperature. When the specimens
the incubation stage, they denitely shorten the transforma- temperature was reduced by a step, the amount of the m-
1788 J.-H. Pee, T. Akao, S. Ohtsuka and M. Hayakawa

2 At a temperature well below the nose, the transformation

(a) Q 1.45Y = 50.1kJ/mol behavior is well characterized by a long incubation period
0 where essentially no transformation was observed. In some
Q 1.50Y = 51.1kJ/mol
-2 theories of isothermal martensitic transformation,20,21) the
Q 1.55Y = 51.1kJ/mol
incubation time is interpreted as the time before a rst
ln(1/t)

-4 nucleation to occur which is governed certain statistical

-6 probability under a given activation energy and driving force.
If this is the case, the probability of nucleation during a given
-8 period is constant and thus an interruption of aging before
nucleation should have no eect on the following aging. But
-10
this is not the case observed in the present experiment,
1.0 1.5 2.0 2.5 3.0
-1 -3 -1
instead the eect of aging during incubation time was
T /10 K cumulative. This seems to suggest a continuous growth of
embryos during incubation period. This may appear to
2 support the embryo growth model proposed recently by
(b) Q1.00m = 48.0kJ/mol
0 Borgenstam and Hillert.22) However, the present method of
Q0.80m = 51.3kJ/mol
monitoring the transformation was not very sensitive. Thus, a
-2 Q0.63m = 51.0kJ/mol
small amount of martensite may have already occurred even
ln(1/t)

Q 0.51m = 51.1kJ/mol
-4 in the stage which we thought as an incubation period.
Further study is necessary on this point.
-6 We have obtained
50 kJ/mol for the activation energy of
the nucleation of the isothermal transformation of the present
-8
specimens; the value was the same within the accuracy of
-10 measurement irrespective of the composition and the grain
1.0 1.5 2.0 2.5 3.0 sizes of the present specimens. Activation energy of 92 kJ/
-1
T /10 K
-3 -1 mol was obtained for the isothermal transformation of 3Y-
TZP under water vapor pressure of 3350 Pa;19) the value was
Fig. 9 Arrhenius plots of the data (a) from Fig. 6 for dierent yttria interpreted as corresponding to the chemical reaction
contents and (b) from Fig. 7 for dierent grain sizes. between water absorbed on the surface and ZrOZr bonds.
On the other hands the activation energy of O2 ions in Y-
phase increased gradually but soon saturated to a level FSZ was reported to be
120 kJ/mol.23) The presently
prescribed by the temperature. This behavior suggests that obtained activation energy 50 kJ/mol is considerably lower
the transformation is more like martensite rather than bainite. than the other two values. However, we cannot identify the
The isothermal transformation behavior looked consider- corresponding rate controlling step for the isothermal trans-
ably dierent at temperatures below and above nose temper- formation.
ature. Below nose temperature it is characterized by a long
incubation period followed by a well dened sigmoidal 5. Conclusions
curve, while above nose temperature there was essentially no
incubation period and the transformation proceeded more or The kinetics of isothermal martensitic transformation of
less linearly with time. Although it was veried that no zirconia doped with small amounts of yttria was studied
transformation took place during the heating of a specimen quantitatively. The transformation behavior at temperatures
above the nose of C-curve, the continuous heating up to the below the nose of C-curve is characterized by a long
holding temperature might have resulted in the apparent incubation period followed by a sigmoidal curve. On the
absence of the incubation period. The marked dierence in other hand, at higher temperatures there was little incubation
the transformation rate, however, seems arise from the time and the transformation proceeds more steadily with
dierences in the driving force and the degree of autocatal- time. The amount of yttria and grain size gave signicant
ysis at temperatures below and above the nose temperatures. inuence on the location of the C-curve, namely the stability
As seen from the position of the C-curves in Fig. 6, the against the transformation. The eect of aging during the
transformation start time is sensitively dependent on the incubation period was found to be cumulative. However, a
yttria content. With decreasing yttria content, not only the C- caution is necessary to properly interpret this because of the
curve shifted toward short time side but it shifted toward limited sensitivity of the measurement of the transformation.
higher temperature side. Although the latter shift was small, The activation energy of 50 kJ/mol was obtained for the
the shift becomes evident if we compare with the nose nucleation of the isothermal transformation of the present
temperature of 3Y-TZP (473K).9,19) The position of C-curve specimens; they are considerably lower than those corre-
was also dependent on the average grain size of specimen; sponding to the chemical reaction between H2 O and ZrO2 on
with increasing grain size the C-curve shifted toward short the specimens surface and the diusion of O2 ions in Y-
time side and toward higher temperature side. The un- FSZ.
stabilization eect due to the variation of the grain size from
0.5 to 0.8 mm was nearly equivalent to that caused by the
composition change from 1.55 to 1.45 mol% Y2 O3 .
 The Kinetics of Isothermal Martensitic Transformation of Zirconia Containing a Small Amount of Yttria 1789

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