Materials Science and Engineering A266 (1999) 211220

Use of partially oxidized SiC particle bed for microwave sintering

of low loss ceramics
Peelamedu D. Ramesh
a,
*
,1
, David Brandon
a
, Levi Schachter
b
a
Department of Materials Engineering, Technion-Israel Institute of Technology, Haifa 32000, Israel
b
Department of Electrical Engineering, Technion-Israel Institute of Technology, Haifa 32000, Israel
Received 17 March 1998; received in revised form 17 November 1998
Abstract
A 1 kW hybrid microwave system was fabricated using a partially oxidized SiC powder bed and used to sinter small
components of low-loss insulating ceramics. Samples of 3% yttria stabilized zirconia/20% alumina (3YZA) and 99% alumina were
sintered to nal densities of 99%(3YZA) and 95%(99% alumina). Partially oxidized silicon carbide (b-SiC) powder was used as
susceptor (preheater). By comparison, unoxidised b-SiC powder, which couples well with microwaves at room temperature,
exhibited thermal runaway above 400C. It could be possible that at high oxidation levels the connectivity between SiC particles
in b-SiC powder bed might become depercolated, and a model similar to one proposed for silicon nitridation under microwaves
could be appropriate in understanding the microwave absorption phenomenon. Stable temperature measurements at various
positions in the system conrmed that the maximum temperature was at the center of the 3YZA sample. The plot of the relative
temperature difference between the sample and its surroundings as a function of sample temperature resulted in a bell-shaped
curve with a clear maximum at around 800C, associated with the rapid increase in radiation heat transfer above this temperature.
Experiments also conrmed that sintering occurred at lower temperatures in a microwave eld when compared to conventional
sintering. 1999 Elsevier Science S.A. All rights reserved.
Keywords: Hybrid microwave heating; Oxidized silicon carbide; Depercolation; Sintering
1. Introduction
Sintering of ceramics is an attractive area of mi-
crowave processing [1]. The advantages include rapid
heating rates, short processing times, low power re-
quirements and reduced reaction with the atmosphere.
Materials with a high loss tangent can couple with
microwaves at room temperature while less lossy ma-
terials need higher initial temperatures in order to
couple. Some ne powders, such as carbon [2], silicon
carbide [3] and vanadium oxide [4] couple efciently
with microwaves at room temperature, whereas others
such as zirconia [5] and alumina [6], only couple at high
temperatures. The dependence of dielectric constant (m%
r
)
and loss tangent (tanl) on temperature are needed to
predict the power absorption characteristics of materi-
als in a microwave eld.
Kitchen microwave ovens provide inexpensive multi-
mode cavities for experimental materials processing.
The modes generated within such a cavity result in a
complex electric eld distribution, so that the specimen
position within the cavity is an important variable in
the heating process. More uniform electric elds may be
achieved either by operating at higher frequencies or by
using mode stirrers. Larger specimens (a high lling
factor) absorb microwaves more efciently and result in
higher heating rates, but have the disadvantage of eld
non-uniformity and resonances within the specimen
(which may result in cracking of the sample). Heat
generation is also affected by the depth of penetration
(D
p
), in the sample. As the temperature of the material
rises, microwave penetration decreases, leading to local-
ized surface heating due to non-uniform power absorp-
tion [7,8]. Smaller workpieces experience a uniform
electric eld, but the heating efciency is then very low
* Corresponding author. Tel.: +49-721-6087922; fax: +49-721-
174263.
E-mail address: hr04@rz.uni-karlsruhe.de (P.D. Ramesh)
1
Now at Institu t fu r Keramik im Maschinenbau, Universitat Karl-
sruhe, Haid-und-neu-Str. 7, 76131 Karlsruhe, Germany.
0921-5093/99/$ - see front matter 1999 Elsevier Science S.A. All rights reserved.
PII: S0921- 5093( 99) 00017- 9
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 212
Fig. 1. The microwave hybrid heating conguration. All dimensions are in mm. The temperature was measured at positions a, b, c, and d,
corresponding to the outer insulation, the inner insulation, the alumina ber board and the sample, respectively. Measurement of temperature on
the alumina berboard surrounding the sample c is a measure of susceptor temperature, since the sample is well-separated from the berboard.
due to the low mass [9] and can only be improved by
using a single mode cavity [10].
Since the dielectric loss properties increase with tem-
perature, low loss materials can be made absorptive by
raising their temperature. Most commonly, a room
temperature susceptor surrounds the specimen and sup-
plies thermal energy by heat transfer, simultaneously
immersing the specimen in both thermal and electric
elds
2
. Computer modeling of microwave heating indi-
cates that, despite a decrease in total electric eld
intensity, the eld at the specimen is not signicantly
screened by using a preheat susceptor [7].
Several preheating congurations have been sug-
gested. Deet al. [11] used a SiC-lined susceptor around
the specimen to sinter Al
2
O
3
compacts. An array of SiC
rods [12] has been used to sinter 8YZrO
2
(a picket
fence arrangement). Using this conguration, densities
as high as 99% have been reported for specimen sinter-
ing temperatures of 1100C, ca. 200C lower than the
conventional sintering temperature of the same powder.
Carbon [13] has also been tried as a preheating source,
while LaCrO
3
and mixtures of Al
2
O
3
+LaCrO
3
have
also proved to be suitable susceptor materials (Spotz et
al. [14]).
In this study, we report the use of a partially oxidized
b-SiC powder compact as a susceptor (pre-heater) to
sinter small components of low-loss ceramics (Al
2
O
3
and ZrO
2
). The susceptor powder surrounds the speci-
men cavity and heats the low-loss specimen to tempera-
tures of the order of 1250C.
2. Experimental
2.1. The hybrid microwa6e heating system
Various congurations [11,12] of hybrid heating have
proved successful for ZrO
2
and Al
2
O
3
compacts. Poor
microwave absorbers such as porous magnesia (MgO)
and quartz (SiO
2
), form the container walls of the
refractory cavity, and alumina ber board and brous
alumina are used as thermal barriers. A schematic of
2
In this study radiation heat transfer within the microwave oven
assembly is taken to refer to thermal radiation and not to the
externally imposed microwave radiation eld.
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 213
the present hybrid heating arrangement is shown in Fig.
1. The loss tangent values of MgO and SiO
2
are very
low and these ceramics remain transparent to mi-
crowaves even above 1000C. b-SiC powder (600 grit)
was used as the susceptor material. About 3040 g. of
the SiC powder was placed in the gap between the
alumina berboard inner cavity and the quartz wall.
The quantity of susceptor powder determines the elec-
tric eld at the sample and was selected to ensure that
the specimen was adequately exposed to the electric
eld at high temperatures, even though the microwave
penetration depth into the SiC powder bed decreases as
the temperature rises. Temperature measurements were
made at selected sites, labelled a, b, c and d in Fig. 1,
using a type R (Pt Pt13%Rh) thermocouple within an
alumina support tube. The specimen temperature T
d
was measured by inserting the thermocouple into a
small hole at the center. The temperature at the Al
2
O
3
ber board T
c
was taken as an estimate of the tempera-
ture of the silicon carbide susceptor. Temperatures were
also determined across the thickness of the porous
MgO crucible T
a
and T
b
. The present system was
designed to generate a moderate thermal gradient in the
central region: a critical consideration for uniform sin-
tering and crack prevention.
2.2. Temperature measurement
Simultaneous temperature measurement in a continu-
ous electromagnetic eld using a thermocouple is usu-
ally impossible as the thermocoupleeld interaction
leads to gross errors. A very thin metal sheath sur-
rounding the thermocouple could be used to overcome
this problem, but contact between the thermocouple tip
and the metal sheath must be avoided, while, shielding
reduces the response of the thermocouple. In this work,
the microwave energy was pulsed and an alumina cov-
ered thermocouple, with the tip uncovered, was used
for calibrating temperature measurements. Tempera-
tures were measured using a Pt Pt 13% Rh thermocou-
ple (type R, 0.5 mm wire). The stable temperature
readings agreed with readings obtained with a platinum
sheathed thermocouple. While the temperature readings
are judged to be reliable, they are still average readings
which do not necessarily reect the energy conversion
processes associated with the microwave power absorp-
tion. In particular, the relation between the measured
temperature and the effective temperature in the sinter-
ing process may not be linear.
2.3. Absorption characteristics of SiC, ZrO
2
and Al
2
O
3
Polar substances absorb microwaves to convert mi-
crowave energy to thermal energy. The generalized
equation for the absorbed power is written as
P
mw
=P
inc
(1p
2
)(1e
2hd
) W m
3
(1)
where P
mw
is the total power absorbed by the material.
The reection coefcient, p, and attenuation constant,
h, mainly determine the total power absorbed in the
material. Low values of p and h correspond to insulat-
ing materials, in which a limited microwave absorption
results. Metals reect microwaves and have high values
of p and h.
For a homogeneous material, reection constant [15]
can be written as
p=
1m
r
*
1+m
r
*
(2)
and attenuation constant h,
h=
2yf
c
m
0
m
r

1/2
!
1+
|
2yfm
0
m
r
%

2
n
1/2
1
"
1/2
(3)
where m
r
* is the RMS value of the complex dielectric
constant, | is the electrical conductivity of the material,
f =2.45 GHz, c=310
8
m s
1
, and m
0
and m
r
% are the
free space permittivity and the relative dielectric con-
stant of the material, respectively.
At a xed microwave frequency, only the material
properties m
r
=m
0
m
r
% and tanl determine the total power
dissipated within the sample. Both these parameters
depend strongly on temperature [16].
Experimental time versus temperature curves for
fresh powders of SiC, Al
2
O
3
and ZrO
2
are given in Fig.
2 for increasing power loadings. Experiments were con-
ducted with 50 g. of each powder sample in an alumina
crucible without any preheating powders. The gure
clearly indicates the strong absorption of the SiC pow-
der in comparison with the other powders. A few
minutes exposure, even at low power levels (450 W),
raises the temperature of fresh SiC powder above
1600C, with thermal runaway occurring after 90 min
of irradiation. More unexpectedly, after three successive
runs of the now partially oxidized SiC powder the
microwave heating curve exhibits much better coupling
at the lower temperatures with no runaway at high
temperatures.
All subsequent hybrid sintering experiments were
performed with a partially oxidized SiC powder suscep-
tor for two reasons: (1). Repeated runs generated nearly
identical power/temperature/time conditions. (2) The
controlled coupling of the electric eld together with
the moderate temperature maximum ($1250C at 1
kW) fullled the basic prerequisites for a hybrid pre-
heating system.
2.4. Penetration depth
Microwave absorption for planar thick samples can
be characterized by a parameter termed the penetration
depth, D
P
. The primitive equation to calculate the
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 214
depth of penetration for microwaves in a homogeneous
material is given by
D
P
=
u
o
2y tanl m%
r
(4)
At a frequency of 2.45 GHz, the free space wavelength
u
o
=122.4 mm. The temperature dependence of D
p
was
calculated from the data of m
r
% and m
r
for Al
2
O
3
and SiC
available in the literature [16]. At 1350C, 2.45 GHz
microwaves penetrate 1 mm in SiC and 93 mm in solid
alumina. Alumina only absorbs microwaves signi-
cantly above 800C, SiC absorbs at room temperature
but at high temperatures heat generation is limited to
the surface layer and the susceptor will screen the
sample. It follows that both the thickness and the
temperature of the susceptor layer must be limited.
In general, if the penetration depth exceeds sample
thickness, the material behaves transparent. Volumetric
heating results, if the penetration depth is comparable
with the sample thickness. Otherwise, if the sample is
too thick, absorption limits to the surface.
In the case of an oxide layer surrounding the suscep-
tor powder particle, such as SiC powder particle sur-
rounded by silica, the above Eq. (4) can not be
applicable. For a compositionally changing ceramic
system, a more complex equation involving terms for
connectivity and percolation, is needed to describe the
microwave penetration depth.
2.5. Materials and methods
Specimens with two different compositions and of
various shapes (see Fig. 8) were used for the sintering
studies. The compositions used were 3Y
2
O
3
ZrO
2
/20
Al
2
O
3
(YZA) and 99% Al
2
O
3
. The nominal particle size
of the YZA powder was 20 nm. All YZA samples were
prepared by gelled tape-casting [17] as shown in the
owchart (Fig. 3). Cylindrical pellets of YZA 15 mm in
diameter and 45 mm in thickness were obtained from
the gelled tape by uniaxial pressing. The measured
green density of these samples was 5055% of theoreti-
cal. Al
2
O
3
green samples were supplied in the form of
small cylinders (16 mm height and 3 mm diameter). A
maximum of three YZA pellets (approx. 15 gm.) and 15
Al
2
O
3
specimens (ca. 5 g) were placed separately in the
ber-board specimen cavity (Fig. 1).
A kitchen microwave oven was used (multimode
cavity, Sanyo Super Showerwave, 1000 W maximum
power). The microwave power was pulsed at a constant
rate, but with the pulse duration adjusted for different
power levels (at maximum power the power supply was
continuous). Stable temperatures were recorded in-situ
between pulses.
No sparking associated with microwavethermo-
couple interaction was observed. The hybrid pre-heat-
ing system (Fig. 1) was placed at the center of the
microwave oven cavity and insulated by alumina ber-
board. Even at high specimen temperatures the heat-
losses due to convection from the insulated system were
low and no overheating of the oven was observed.
3. Results and discussion
3.1. Oxidation of SiC powder
When the SiC powder bed is microwave heated to
temperatures above 1000C in ambient atmosphere,
oxidation phenomena takes place. The oxidation phe-
nomena [18] that takes place in SiC is briey discussed
below. The possible oxidation reactions for SiC could
be
Fig. 2. Effect of power-dependent microwave absorption on the heating of SiC, Al
2
O
3
and ZrO
2
powders without any preheater (susceptor).
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 215
Fig. 3. Flowchart for YZA pellet formation by tape-casting.
where i is the mass gain per unit volume of SiO
2
.
Values of K
p
h were calculated for oxidation of silicon,
based on oxygen diffusion through a silica layer, and
compared with the experimental SiC oxidation data.
From a thermodynamical point of view, various pos-
sible reaction rate limiting steps in the SiC oxidation
reaction are discussed in detail elsewhere [18]. These
steps include (i) inward O
2
diffusion through SiO
2
layer
(ii) reaction at the SiC SiO
2
interface and (iii) outward
diffusion of CO molecules. On observation of a higher
oxidation rate of silicon compared to SiC, it was sug-
gested that more than one rate-limiting step is involved
in SiC oxidation, i.e. a mixed interface-reaction/diffu-
sion controlled oxidation takes place in the case of SiC.
3.2. Absorption by different materials
Some attempt has been made to understand the
absorption characteristics of powders as opposed to
solid samples. An amount of 15 g of sample powder
was placed in an alumina crucible which was sur-
rounded by 50 g of fresh SiC powder (as susceptor).
The heating curves for different sample powders at a
constant power level of 650 W are shown in Fig. 4. The
measured temperatures reect both the microwave ab-
sorption by the powder sample (the sample temperature
was measured using a Pt Pt13%Rh thermocouple
which was covered by a thin alumina tube in order to
avoid the thermocouple tip touching the sample pow-
der) and mixed mode heat transfer from the SiC suscep-
tor powder: rstly, if microwave absorption by the
powder sample were negligible, at all temperatures,
then all the heating curves should be similar, with the
sample temperature only dependent on heat transfer
through the sample powder. Secondly, the lower ther-
mal conductivity of ZrO
2
as compared to Al
2
O
3
should
result in a higher Al
2
O
3
temperature at a given time.
However, in Fig. 4, the ZrO
2
samples reach higher
temperatures conrming that ZrO
2
powder absorbs mi-
crowaves much more efciently than Al
2
O
3
.
The vast difference in the heating curves between
unoxidized SiC powder bed and oxidized SiC powder
bed clearly suggests that in these two materials, the
microwave absorption nature is not identical. When a
SiC powder compact is microwave heated to tempera-
tures above 1000C in an ambient atmosphere, the
surface of SiC particle starts oxidizing leading to for-
mation of a SiO
2
layer. This system can now be viewed
as a compositionally changing ceramic system, which is
similar to nitridation of silicon under microwaves,
where a conducting silicon phase continuously gets
converted to a non-conducting silicon nitride phase. A
nite difference model developed by Skamser et al. [19]
gives a deeper insight into the microwave absorption
nature in a compositionally changing ceramic system.
Indeed, the model was successful in predicting the
SiC (s) +O
2
(g)USiO
2
(s) +C (s) (a)
and
SiC (s) +3/2O
2
(g)USiO
2
(s) +CO (g) (b)
The reaction rate constant, K
p
, can be written as
K
p
=
(Dx)
2
t
=
2D
O
2
0,*
(p
O
2
g
p
O
2
i
)
h
(5)
where D
0,*
O
2
is the tracer diffusion coefcient in silica, h
is the number of moles of oxygen required to form one
mole of silica and p
g
O
2
and p
i
O
2
are the oxygen partial
pressures at the oxygen silica and SiC silica interfaces,
respectively. Dx is the SiO
2
layer thickness through
which oxygen diffusion takes place. Depending on the h
value, one of the above described reactions ((a) or (b))
is chosen.
The above Eq. (5) shows a parabolic behavior, which
can also be expressed in terms of SiO
2
mass gain, K
m
,
K
m
=K
p
i
2
(6)
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 216
temperature and composition distributions inside a re-
action bonded silicon nitride specimen [20]. During the
nitridation reaction, silicon was gradually converted to
silicon nitride, and at the intermediate stage, the mate-
rial was two phasic nature. Despite an insulating layer
formation, their experiments revealed the existence of
silicon connectivity at low conversion levels. At around
25% conversion, the electrical conductivity was maxi-
mum, thereafter started decreasing with more and more
conversion, and reached below the detection limit be-
yond 70% conversion. At this region, the silicon parti-
cles lost their connectivity and became completely
depercolated, clearly indicating that there was a neck
formation due to sintering of silicon particles, occurred
at the initial stages of reaction. As long as the connec-
tivity among silicon particles persisted, silicon behaved
like a conductor, reecting most of the microwave
energy. But, when the silicon particles lost their connec-
tivity and became depercolated, the system behaved like
an insulator, absorbing more microwave energy. This
led to non-uniform local heatings in the specimen,
where the more nitrided regions heated to higher tem-
peratures compared to the less nitrided ones. Thomas et
al. [20] have obtained a reasonably accurate empirical
model of the microwave heating characteristics of the
RBSN system by assuming it as a homogenous conduc-
tor at low conversion levels and like a conductor loaded
dielectric (CLD) at high conversion levels.
Let us consider the microwave heating process of
fresh SiC powder bed. At the initial stage, the unoxi-
dized silicon carbide powder is homogeneous, having a
characteristic dielectric behavior. At the initial stages of
Fig. 4. Heating curves for various ceramic powders surrounded by fresh SiC susceptor powder (constant power loading).
Fig. 5. Experimental time-temperature proles at various sites within the cavity (see Fig. 1) on a YZA sample.
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 217
Fig. 6. Plot of [1T
c
/T
d
] versus sample temperature [T
d
] (YZA specimen).
the heating process (i.e. before oxidising), nevertheless
the Eqs. (1) (3) can be used to calculate the reection
coefcient, the attenuation constant and the power
absorption. The temperature dependence of conductiv-
ity for yellow green coloured SiC shows a semiconduc-
tor behavior with an increased conductivity on heating
from room to high temperatures. This dielectric loss
factor increases sharply at temperatures beyond 400C,
which makes the material to show a thermal runaway
behavior beyond this temperature. As the SiC powder
bed gradually oxidize to SiO
2
(see section 3.1), the
system gradually slips away from homogeneity, consist-
ing of two different solid phases coexisting with poros-
ity. With the continuous increase in SiO
2
volume
fraction during microwave heating, in a normal sce-
nario, it can be assumed that the semiconducting SiC
particles are gradually isolated by an electrically insu-
lating layer of SiO
2
. This would cause a gradual de-
crease in the tangent loss of the SiC, as their volume
fraction decreases during the oxidation phenomenon.
Since the above case is somewhat analogous to sili-
con nitridation under microwaves, we believe that a
similar modelling procedure could be possible. On the
same basis, we speculate that at the intermediate stage
(partially oxided), the conductivity of SiC could be of
the same order of magnitude as that of unoxidised SiC,
which might suggest that the silicon carbide particles
sintered partially and still remain well connected. But,
the silicon carbide phase would become completely
depercolated at higher oxidation levels resulting in a
very low conductivity. This could mean that at low
conversion levels, SiC might behave like a semiconduc-
tor and at high conversion levels, it might transform to
a semiconductor loaded dielectric (SLD) material.
The microwave absorption behavior of such a mate-
rial is more complex and a mathematical treatment
similar to nitridation of silicon reaction could be help-
ful in understanding the microwave absorption nature
of this material. The above given Eqs. (2) (4) for
reection coefcient, attenuation constant and the pen-
etration depth respectively, becomes invalid at high
conversion levels and a new set of equations similar to
the one proposed by Neelakanta and Park [21] might be
more appropriate. More importantly, in the energy
balance equation, the SiC depercolation, and chemical
phenomena of oxidation should properly be accounted
in order to get accurate temperature distributions in the
powder bed. This discussion is purely speculative and
no conductivity measurements were made in order to
conrm the percolation phenomenon.
3.3. Temperature proles
Temperature versus time proles measured as a func-
tion of power input for the different sites in the hybrid
system of Fig. 1 are shown in Fig. 5. The highest
temperatures were recorded at the center of the YZA
sample T
d
, (1340C), whereas the highest temperature
measured in the alumina ber board T
c
, was 1250C.
Curve T
d
diverges increasingly from curve T
c
above
400C, consistent with increasing microwave coupling
of the YZA specimen. This divergence reaches a maxi-
mum at 800C and then decreases, consistent with
increasing radiation heat transfer. The relative tempera-
ture divergence was plotted as [1T
c
/T
d
] against the
sample temperature [T
d
], Fig. 6 and can be qualitatively
explained as follows. At low temperatures (B400C)
there is no YZA specimen-microwave coupling, and the
measured temperature at the center of the sample is
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 218
Fig. 7. Radiant heat transfer from a YZA specimen calculated from the experimental temperature values.
predominantly the result of heat transfer from the
susceptor powder. Above 400C [1T
c
/T
d
] increases as
the sample starts to couple and absorb microwave
energy. As heat transfer due to radiation, proportional
to T
d
4
, increases, above 800C the temperature differ-
ence again decreases, leading to the observed bell-
shaped curve in the [1T
c
/T
d
] versus T
d
graph.
Heat transfer due to radiation can be calculated from
the appropriate values for the parameters in the radia-
tion equation. The radiant heat loss from the sample
calculated from experiments as a function of the sample
temperature [T
d
] is shown in Fig. 7. As predicted, the
radiation loss increases rapidly above 800C, but then
saturates as the temperature difference (T
d
T
c
) de-
creases at the highest temperatures.
3.4. Sintering
In most reports on microwave sintering of Al
2
O
3
or
ZrO
2
ceramics, researchers have observed a microwave
eld effect. Janney et al. [22] have sintered Al
2
O
3
+
0.1% MgO compacts to densities of ca. 98% at 1200C
using a 28 GHz microwave furnace, a temperature
nearly 300C lower than that required for conventional
sintering. Using the picket fence SiC susceptor ar-
rangement, the same authors have reported [23] sinter-
ing of ZrO
2
8% Y
2
O
3
compacts to densities above 99%
at 1195C, ca. 150C lower than the conventional ring
temperature. Fang et al. [24] have reported much re-
duced sintering times for hydroxyapatite ceramics
heated in a multimode cavity compared to conventional
sintering [25]. They showed that the same soaking time
and sintering temperature in the microwave eld gave
higher densities and ner microstructures, and that this
effect was the same at all temperatures. Enhanced
densication in a microwave eld was also observed for
ZrO
2
3% Y
2
O
3
compacts by Nightingale et al.
[26].Even though there is still much to explain in mi-
crowave-eld assisted densication, the effect appears
real and signicant.
In the present work, specimen densities of 99% of the
theoretical value were achieved for YZA and about
95% for Al
2
O
3
samples. Example of the various green
and sintered samples are given in Fig. 8. Uniform size
reduction (density) was observed when a batch of 15
Al
2
O
3
samples were sintered together. The microstruc-
ture of the sintered YZA samples showed a uniform
distribution of the two phases (the Al
2
O
3
grains are
dark, Fig. 9a). The grain size of the Al
2
O
3
samples in
Fig. 8. Sintered and unsintered samples of different composition used
in the present work.
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 219
Fig. 9. Scanning electron micrographs of (a) YZA, z=99%, (Al
2
O
3
grains appear dark) and (b) Al
2
O
3
, z=95%.
samples with different soaking times are shown in Fig.
10. The sintering temperature for YZA was 1340C
(Fig. 5) with soaking times from 5 to 60 min. The
temperature of the Al
2
O
3
sample was not recorded.
The faster sintering of the YZA samples is attributed
to greater microwave absorption in ZrO
2
as compared
to Al
2
O
3
.
4. Conclusions
Room temperature microwave absorption by silicon
carbide powder was utilised to construct a microwave
hybrid heating conguration. Partially oxidized SiC
powder proved a very satisfactory room temperature
preheater, generating reproducible power/time/temper-
ature conditions. Since the SiC powder bed was conti-
nously oxidizing at high temperatures generated by
microwave energy, it could be considered as a compo-
sitionally changing ceramic system. It is suggested that
a model similar to the one proposed for silicon nitri-
dation could be appropriate in explaining the observed
difference in the microwave absorption nature between
pure and partially oxidized SiC powder compacts.
Temperature measurements indicated that a zirconia
sample reached the highest temperature in the hybrid
system. The temperature increase of zirconia at low
temperatures ( B800C) is primarily by thermal radia-
tion from the susceptor. At higher temperatures radia-
tion cooling of zirconia occurs, while the continuing
temperature increase is due to microwave power ab-
sorption by the zirconia. Using this simple hybrid
heating unit, it was possible to sinter small samples of
yttria stabilized zirconia and 99% alumina to densities
above 95%.
Fig. 9b was about 1 mm, with no exaggerated grain
growth but some porosity at the triple junctions.
Microwave sintering curves for Al
2
O
3
and YZA
Fig. 10. Density change with sintering time for YZA (at 1340C) and Al
2
O
3
specimens.
P.D. Ramesh et al. / Materials Science and Engineering A266 (1999) 211220 220
Acknowledgements
The authors acknowledge the Wolfson Centre for
Interface Science for providing a research fellowship
(PDR) and the Faculty of Materials Engineering for
providing the experimental facilities. The research was
supported by AFIRST. L. Schachters research on mi-
crowave ceramic sintering was supported by the Israeli
Ministry of Science.
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