See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/290488291

Introduction: What is Microwave Processing?

Article · January 1997

CITATIONS READS
10 2,730

2 authors, including:

Diane C. Folz
Virginia Polytechnic Institute and State University
40 PUBLICATIONS   653 CITATIONS   

SEE PROFILE

All content following this page was uploaded by Diane C. Folz on 07 July 2015.

The user has requested enhancement of the downloaded file.

What is Microwave Processing?

D.E. Clark and D.C. Folz

Introduction
The purpose of this book is to present a basic introduction to microwave
processing, with a particular emphasis on ceramic materials. The reader also is
encouraged to refer to Microwave Processing of Materials,1 published by the National
Academy Press in 1994, which provides an excellent overview of the subject and
includes materials other than ceramics. Some of the material in this chapter has been
adapted from Clark and Sutton2 which contains an extensive set of references up to 1996.
Applications of microwave energy can be divided into several categories: (1)
communications and information transfer; (2) processing/manufacturing; (3)
diagnostics/analyses; (4) medical treatment; and (5) weapons. By far, the largest uses fall
into the first two categories. In fact, most of us are familiar with microwaves primarily
through the use of our home microwave ovens and cell phones. Many of the microwave
applications involve the use of specialized ceramics for their successful operation.
However, the primary focus of this book is on how to use microwave energy to process
and manufacture ceramics. The principles and equations that govern the interaction of
electromagnetic energy with materials (which includes microwave energy) have been
known for over 50 years. In the early 1950s, these were used to develop equipment and
methods for processing food at the industrial level as well as within our homes. These
same principles and methods now are being used to guide the development of microwave
processing of ceramics in the laboratory and, to a more limited extent, in ceramics plants.
Microwave energy can revolutionize the way we, as ceramic engineers and
production managers, approach product manufacturing. While microwave energy alone
will not be the answer to every technical barrier in materials processing, it can give us an
alternative to the high energy consumption resistance heating techniques that are
commonplace in industry. This book will provide you with a more complete
understanding of the significant advantages microwave processing can offer and of some
of the barriers that have prevented more rapid, wide-spread industrial use of this
technology in the United States.
The question always arises as to the types of materials that are suitable for
microwave processing. As shown in the bar charts and tables that follow, there has been
significant interest in microwave processing of ceramics since the mid-1980s. These
figures present data based on the numbers and distribution of papers in the six
proceedings published by the American Ceramic Society for three international
microwave symposia and the first three World Congresses focusing on microwave and
radio frequency processing and applications3,4,5,6,7,8. As clearly indicated in Figure 1, out
of 383 total papers published, nearly half are focused on ceramics and glasses. The use
of microwaves for sintering accounts for a significant fraction of the research (Figure 2).
This point is interesting in light of the fact that most microwave ovens are designed to
operate at low temperatures.
Papers vs Materials

180
169

160

140

120

100
Papers

83
80

60

40
40
24
20 12 11 14
10
7 7 4
2
0
er
ic
al

al
te

s
ss

ic

ls

re
ria
er

al
am

ic
ia
et

si

tu
la

er
th

e
m
er
po

a
M

ly

ul
G

at
er

er

in
O

he
at
Po

r ic
om

m
C

M
-C

om

Ag
te
C

ss

Bi

as
la

&
W
G

od
Fo
Materials

Figure 1. Distribution of materials topical papers published by the American

Ceramic Society in the microwave symposia and conference proceedings from
1991 to 2003.
Papers vs Topics

60
54

50 47
44

40 38

31
Papers

30
30

22 22 22
20
13

8 9 8
10
6 6 5 5 6 5
2
0
od ent

ty

w
Sy ng

t & ing

l
es

ng
n

n
g

nt

z)
g

ca
si

in
ig
lin

tin
io
tio

tio
lin

ie
in
fe
e

H
av

si
he

i
es
ry

in
m

ur
at

ev
m

cl

ed
e

Sa
el
ea

ca

G
ac

es
w

Jo
od
D

re

iz

C
cy
re
nt

D
-M

45

om
ifi

er
n
ro

al

oc
su
su

re
M
An

2.
ss

nt
ci
ic

pr

Bi
ea
ea

nd
er

li
m

la

en

ot
&

a
ia
m

G
m

(n
of

ce

m
pm
g

er
m
s-
in

n
re

as
ls

es
fa

at
io
co
tie
er

ui
tu
ta

om Sur

pl
t

ci
Eq

ia
nt

ra
er
en

en

e
ed

e
Si

an
pe
op

av
m

av

qu
m
m
pr
a

ic

w
w
re

fre
nd

Te

ro
ro
ric
Fu

te

ic
ic

er
ct

on

M
as

th
le

Ec

O
ie
D

Topics

Figure 2. Distribution of papers with respect to research topics published by the

American Ceramic Society in the microwave symposia and conference
proceedings from 1991 to 2003.
 The information presented in Table 1 illustrates the distribution of interest in
microwave processing of ceramics throughout industry, academia and government labs as
presented in these six proceedings. Much of the work in microwave processing is being
conducted through collaboration between two or more of these research groups. It is not
uncommon to see interagency and interdisciplinary research teams working together to
attempt to work through some of the practical and theoretical issues associated with
implementing microwave processing.

Table 1. The distribution of ceramics (does not include glass or glass-ceramics) papers
according to researcher institution.
Topics Ceramics papers
G A I IA GA GI GIA Total
Fundamentals of microwaves 5 1 6
Sintering & annealing 7 29 4 4 1 2 47
Drying 1 1
Synthesis 1 14 4 19
Dielectric properties-measurement 2 8 3 3 1 17
Temperature measurement 1 3 4
Surface modification 3 1 4
Economic and commercialization 3 3
Modeling 15 2 17
Joining 1 7 2 2 1 2 15
Equipment & design 2 4 1 1 8
Microwave material interaction 1 12 6 19
Other frequencies (not 2.45GHz) 1 1 1 1 4
Microwave plasma processing 2 1 3
Review articles 2 2
Total 16 105 11 23 7 5 2 169
G=government laboratory; I=industry; A=academia

Historical Perspective
The possibility of processing ceramic materials with microwave energy was
known by the 1950s and had been investigated by Tinga et al9, Levinson10, and Bennett et
al11 on a limited basis by the 1960s. In 1975, while investigating microwave drying of
high alumina castables, Sutton12 observed that, in addition to removing water,
microwaves heated the ceramic. Using an industrial microwave oven lined with non-
microwave-absorbing refractories, temperatures in excess of 1400°C were attained. This
study demonstrated that microwave energy could be used for processing full-scale
ceramic products (low- and high-temperature). It also showed microwave energy to be
faster and more cost effective, as well as capable of producing products with equal or
superior performance when compared with products resulting from conventional gas
heating. It was fortuitous that the particular ceramic used by Sutton was a good
microwave absorber at 2.45GHz (the most commonly used microwave frequency), as
many ceramic materials are transparent to microwave energy at this frequency. On the
other hand, it was unfortunate that, comparatively, the low cost of fossil fuels at the time
limited implementation of microwave energy for industrial applications.
By the 1980s, quite a number of researchers in North America were investigating
microwave processing of ceramics, most likely due to three factors: 1) many laboratories
were equipped with inexpensive home-model microwave ovens that could be modified
for high-temperature research, 2) researchers at national and foreign laboratories were
reporting successes and unusual effects with microwave processing, and 3) an
international symposium on microwave processing was held in 1988. As a consequence
of factor (1), most of the studies have been and still are performed at 2.45GHz. This fact
has resulted in some creative engineering in developing microwave-conventional hybrid
heating techniques and microwave-absorbing additions to compositions in order to
overcome the issue of low microwave absorption by many ceramics at room temperature.
Regarding factor (2), scientists in the Ukraine and Russia used high frequency (37 and
84GHz) microwaves to achieve very rapid heating and processing for applications, such
as plastic coating of oil piping; glazing ceramics; soldering and brazing; treatment of
polymers, composites and semiconductors; and, synthesis of materials. Researchers at
Los Alamos and Oak Ridge National Labs used 2.45GHz and higher frequencies (28 and
60GHz) to prepare ceramic-glass seals; sinter Al2O3, ZrO2, B4C and TiB2; heat treat
Si3N4; fabricate composites; and, form ceramic joints. The laboratories also developed
unique microwave susceptors and casketing techniques. Scientifically, one of the most
important discoveries was reported by Janney et al13 at Oak Ridge National Laboratory.
They demonstrated that alumina (Al2O3) could be sintered at much lower temperatures
with microwave energy than with electric resistance heating. This phenomenon is
referred to as a “microwave effect” and has been reported by numerous investigators.
Enhancements in the rates of activated processes involving material transport (e.g.,
sintering, ion exchange and chemical reactions) are considered to be microwave effects
because a reduction in the activation energy appears to be required, and investigators
have been unable to provide a scientific basis for this behavior. In addition to enhanced
rates, reaction pathways and reaction products found in microwave processes, but not in
conventional processing, also are considered as microwave effects.
As microwave processing becomes more widely used, it also will be necessary to
understand the differences in heating schedules, reaction pathways and phase
transformations that occur in a microwave processing field. It is anticipated that new
diagnostic/analytical tools, such as microwave thermogravimetric analyzers (MTGAs)
and microwave differential scanning calorimeters (MDSCs) will need to be developed to
provide this understanding. One such tool, scanning dielectric analysis (SDA), is
described by Hutcheon et al in this book.
Since 1988, the Materials Research Society (MRS) and The American Ceramic
Society (ACerS) have held seven major symposia in the United States on microwave
processing. The Microwave Working Group (MWG) (www.microwave-rf.org) was
formed in 1993 to foster microwave research and manufacturing in the United States. In
addition to being active in the MRS and ACerS symposia, the MWG has organized four
World Congresses on microwave processing.
Other professional societies worldwide (the International Microwave Power
Institute, the American Chemical Society, the Institute of Electromagnetic Wave
Application – Japan, the Association of Microwave Power in Europe for Research and
Education) regularly sponsor microwave processing conferences, short courses and
workshops. These symposia have brought together internationally recognized experts in
materials processing, microwave technology and equipment designers, and provided an
excellent forum for exchanging information, sparking fresh ideas and stimulating new
interest. As a result of the increased interest among scientists and engineers, many
advances are being made in dielectric property measurements, modeling and processing.
A better understanding of microwave-material interactions and the economics of
microwave processing is evolving that will provide the basis for future industrial
applications. In parallel, new equipment with variable frequencies, high-temperature
capabilities, and better temperature monitoring and control systems are being designed
and manufactured.

The Basics
Microwaves (frequencies of 0.3GHz to 300GHz and wavelengths of 1 m to 1 mm)
lie between radio wave frequencies (RF) and infrared (IR) frequencies in the
electromagnetic (EM) spectrum (Figure 3). Microwaves can be reflected, transmitted
and/or absorbed. The absorbed microwave energy is converted into heat within the
material, resulting in an increase in temperature. Gases, liquids and solids can interact
with microwaves and be heated. Under certain conditions, gases can be excited by
microwaves to form plasmas that also can be useful for processing.

Figure 3. The electromagnetic (EM) spectrum and the microwave range. The
most commonly used frequency is 2.45GHz with a wavelength of 12.2 cm.

Nearly all microwave ovens operate at 2.45GHz due to the fact that they were
designed to process foods and the water in the foods is a good absorber at this frequency.
Unfortunately, at room temperature, many ceramics do not absorb 2.45GHz microwave
energy appreciably. Their absorption may be increased by adding absorbing constituents
(e.g., silicon carbide, carbon, organic binders), altering their microstructures and defect
structures, changing their form (e.g., bulk vs. powder) or changing the frequency of the
incident radiation. The latter often is not feasible due to the relative unavailability of
equipment. Fortunately, absorption of poorly absorbing ceramics also can be improved
by increasing their temperatures. This phenomenon has led to the development of hybrid
heating, where the ceramics are heated initially using conventional methods. Once the
ceramic is heated to its critical temperature, Tc, microwave absorption becomes sufficient
to cause self-heating. This hybrid method can yield more uniform temperature
distributions than those resulting from stand-alone microwave or conventional processing
methods. This uniformity is the result of microwave volumetric heating and minimized
heat losses. Hybrid heating can be achieved either by using an independent heat source,
such as a gas or electric furnace in combination with microwaves, or through the use of
an external susceptor that couples with the microwaves. In the latter, the material is
exposed simultaneously to microwave energy and radiant conventional heat produced by
the susceptor.
Microwaves can be absorbed by ceramics either through polarization or
conduction processes. Polarization involves short-range displacement of charge through
formation and rotation of electric dipoles (or magnetic dipoles, if present). Conduction
requires long-range (compared to rotation) transport of charge. Both processes give rise
to absorption losses in certain frequency ranges, as illustrated in Figure 4. In this figure,
the absorption losses (also referred to as dielectric losses), ε˝, are due to ionic conduction,
dominant at low frequencies, and rotation of permanent dipoles at higher frequencies.
The ionic conduction losses are due to the well-known ohmic losses that occur when ions
move through the material and collide with other species. Ionic conduction decreases
with increasing frequency because the time allowed for transport in the direction of the
field decreases with increasing frequency. Increasing the temperature increases the
kinetic energy of the dipoles, making it easier for them to respond to the oscillating field
and shifting the absorption curves to higher frequencies.
 A (v)

X (m)
Dielectric Material

Ionic Dipole
Conduction Rotation

HT
RT HT

RT
ε˝eff

2.4
f (GHz)

Figure 4. This figure illustrates two absorption mechanisms that can contribute
to ε˝eff: ionic conduction, which can be important at low frequencies; and, dipolar
rotation, which can be important at high frequencies. The absorption curves shift
to higher frequencies for both of these as the temperature is increased. Note that
a material may be poorly absorbing at room temperature and 2.45GHz and highly
absorbing at high temperature and 2.45GHz (adapted from Metaxas14). Terms: x
≡ distance; A ≡ amplitude of the electric field; ε˝eff ≡ effective dielectric loss; f ≡
frequency; RT ≡ room temperature; HT ≡ high temperature.
 Figure 5. Frequency dependence of the polarization mechanisms in dielectrics:
(a) contribution to the charging constant (representative values of ε´); (b)
contribution to the loss angle (representative of ε˝).

In addition to dipole rotation, other widely recognized polarization processes

include interfacial, ionic and electronic polarization. These processes are discussed in
detail by Hench and West15 for typical ceramics. Because several processes can
contribute to the losses, and it is not always easy to differentiate experimentally between
the loss mechanisms, losses typically are reported as effective losses, ε˝eff. To adequately
characterize the response of ceramics to the electromagnetic spectrum, measurements
should be made over a broad frequency range. Frequency ranges, where each of these
can contribute to losses, vary considerable over the EM spectrum, depending on the
ceramic (Figure 5). It is because of the frequency dependence of absorption that a single
frequency, such as 2.45GHz, cannot be used easily to heat all ceramics at room
temperature. To efficiently heat a material that does not have an absorption mechanism
close to 2.45GHz requires changing either the frequency of the radiation or the
composition of the material, or the use of hybrid heating. Likewise, ceramics can be
designed to be microwave safe, such as with microwave cookware. These materials have
insufficient absorption to be self-heating at the operating frequency of the microwave
oven.
Whether or not a ceramic can be heated by microwave energy depends on how
much and how fast that energy can be absorbed. The rate of energy absorption is
expressed in terms of power per unit volume as

Pa = ω εo ε˝eff E2rms + ω µo µ˝eff H2rms (watts/m3) (1)

where, the terms on the right side of the equation refer to electric and magnetic losses,
respectively. Generally, the magnetic losses are negligible and only the electric losses
contribute to the absorbed power. Here

ω = angular frequency = 2πf (f=operating frequency in hertz);

εo = permittivity of free space = 8.85 x 10-12 farads/m;
ε˝eff = effective relative dielectric loss (dissipation) factor (unitless); and,
Erms = root mean square of the internal electric field (volts/m).

ε˝eff = ε˝c + ε˝s + ε˝d + ε˝i + ε˝e (2)

where, ε˝c is the loss due to dc conductivity and is negligible at microwave frequencies
for most ceramics, as shown in Figure 414. The last four terms represent dielectric losses
due to polarization mechanisms, where ε˝s = space charge or interfacial; ε˝d = dipolar; ε˝i
= ionic, and ε˝e = electronic. For ceramic materials in the microwave frequency range, ε˝s
and ε˝d are the most important. Since these terms are dependent on both frequency and
temperature, they must be measured in order to know how well the ceramic will heat at a
specified frequency (i.e., 2.45GHz and room temperature). Sometimes, ε˝eff is replaced
by tanδε΄, where δ is the loss angle, tanδ is the dissipation factor and ε΄ is the dielectric
constant. Values of dielectric properties are provided in Table 2 for a few ceramics. A
rule of thumb is that ceramics with loss factors between the limits 10-2 < ε˝eff < 5 are
good candidates for microwave heating. Ceramics with ε˝eff < 10-2 would be difficult to
heat, while those with ε˝eff > 5 would experience most of the heating in the surface and
not the bulk16.
The rate of temperature rise (∆T/∆t) in a ceramic when microwave energy is
absorbed is given by16
∆T Pa
= (°C/sec) (3)
∆t ρ (C p )

where, ρ = density of the ceramic (kg/m3),

Cp = specific heat (kJ/kg-°C).
Table 2. Dielectric properties, penetration depths and critical temperatures (Tc) for some typical
ceramics and other commonly used materials. The dielectric properties can be very sensitive to
the purity and phase of the material. Therefore, the data shown should be used only as a guide.

CERAMIC MATERIALS FREQUENCY TEMP. ε´ ε ´´ tan δ DEPTH OF CRITICAL TEMP.

(GHz) (OC) PENETRATION (TC)
Dp (cm)
Alumina1 2.45 +25 8.9 0.009 0.00010 1.2 800o C
(3.89-3.61GHz)5
Silicon carbide2 2.45 +200 105 110 1.048 0.28

Mullite3 0.001 +25 5.8 0.012 0.002 3674.4

Fused Quartz 1 2.45 +25 3.8 0.0001 0.00003 1.9
4
Soda Lime Glass 2.45 +20 6.0 1.20 0.20 1.5
Pyrex 1 2.45 +25 4.0 0.005 0.0013 1.8
Boron Nitride 5
8.52 +25 4.37 0.01311 0.00300 0.5 750-800o C
(5.17-4.96 GHz)5
Aluminum Nitride6 2.45 +100 9 0.008 0.000889 1.18
8.52 +25 5.54 0.01994 0.00360 0.44
Silicon Nitride5
2.45 +25 0.68 0.015 0.022059 8.13
4
Water (Distilled) 2.45 +25 78.0 12.00 0.1565 0.39

Lithium Disilicate 2.45 +25 7.5 0.17 0.023 1.30

glass7
Lithium Disilicate 2.45 +25 5 0.02 0.004 1.63
glass-ceramics7
Teflon 1 2.45 +25 2.1 0.0003 0.00014 2.73

Natural Rubber4 2.45 +25 2.2 0.01 0.005 2.65

Polyethylene4 2.45 +20 2.3 0.001 0.0004 2.57

Beef(cooked)4 2.45 +30 30.5 9.6 0.31 0.62

5
Frozen Beef 2.45 -20 4.4 0.53 0.12 1.74
Potato(Mashed)4 2.45 +30 72.5 24.0 0.33 0.40
1: Data provided by J. Gerling, Gerling Applied Engineering, Inc., Modesto, CA
2: Leiser, K., “Microwave Behavior of Silicon Carbide/High Alumina Cement Composites,” Doctoral
dissertation, University of Florida (2001)
3: www.accuratus.com
4: Schiffmann, F. R “Principles of Industrial Microwave and RF Heating,” Microwave: Theory and
Application in Materials Processing IV, Ceramic Transactions, American Ceramic Society, 80 (1997).
5: Metaxas, Industrial Microwave Heating, Peter Peregrinus Ltd., London, United Kingdom (1988).
6: Committee on Microwave Processing of Materials: An Emerging Industrial Technology, Commission
on Engineering and Technical Systems, National Research Council, Microwave Processing of Materials,
National Materials Advisory Board, National Academy Press, Washington, D.C. (1994).
7: Dielectric data provided by Dr. R. Hutcheon, Microwave Properties North, Canada
 It can be seen from equations 1 and 3 that, in addition to the dielectric properties,
the internal electric field also must be known in order to predict the power absorbed and
heating efficiency of the ceramic. It is not trivial to determine the internal electric field,
since it can vary from point to point within the ceramic. The internal field is less than the
external field and is controlled by the dielectric constant, ε΄, as shown by 2,

⎡ N (ε ′ − 1) ⎤
Eint = ⎢1 − ⎥ E ext (V/m) (4)
⎣ 1 + N (ε ′ − 1) ⎦

where N is a depolarization factor that depends on shape or geometry. For an alumina

sample sandwiched between parallel electrodes, N=1, ε΄=9 and Eint = Eext/9. Thus high
values of ε΄ can reduce the internal field and rates of absorption and heating. The internal
electric field for a given point within the material can be estimated by measuring ∆T/∆t
and knowing Cp and ε˝eff by 16

1
⎛ ρC p ∆T ⎞ 2
Eint (rms) = ⎜⎜ ∆t ⎟
⎟⎟ (V/m) (5)
⎜ ωε eff′′
⎝ ⎠

From this, the Eext (rms) can be estimated using equation (4). It should be pointed out
that the external electric field is not uniform in most multimode microwave ovens, hence
neither is the internal electric field. This is why many home microwave ovens require
turntables or mode stirrers. The field uniformity can be improved by increasing the size
of the oven cavity. The cavity should be much larger than the wavelength of the
microwaves.
At the macroscopic level, the dielectric properties control the microwave
processibility of a wide range of non-magnetic materials through the quantitative
relationships of absorbed power per unit volume (Pa) and depth of penetration (Dp,
defined as the distance from the surface into the material at which Pa drops to e-1 (~37%)
of the surface value)16

−1
⎡ 1
⎤ 2

λo ⎛ ε ′
⎢⎜ ⎛ eff ⎞ ⎟′ ⎞
2 2
⎥
DP = ⎢⎜1 + ⎜⎝
1 ε ′ ⎟⎠ ⎟ − 1⎥ (cm) (6)
2π (2ε ′) 2
⎢⎣⎝ ⎠ ⎥⎦

where, λo = free space wavelength of the microwave radiation (λo= 12.2cm for 2.45GHz).
The penetration depths given in Table 2 were calculated using equation (6).
The depth of penetration has important consequences when processes are scaled
up to manufacture components with large cross-sections or multiple samples where
stacking is required. As an example, the depths of penetration for many ceramics in the
microwave range usually are much greater (many cm) than their cross-sections. Thus
multiple samples stacked inside a microwave furnace will all “see” the microwaves and
uniform heating can occur. On the other hand, most of the radiant (IR) heat in
conventional furnaces is absorbed in the first few microns of the outer most samples,
producing shielding effects for samples that are not directly exposed to the radiation.
Therefore, long times are required to bring all the samples to the same temperature and
each sample experiences a different thermal history. This phenomenon increases
production times and can reduce product consistency.
In some materials, the magnetic dipoles may be able to couple with the magnetic
component of the electromagnetic field and provide an additional heating mechanism.
Similar to the dielectric properties, the magnetic permeability, µ΄, and loss, µ˝, must be
considered. There have been relatively few investigations on microwave processing of
magnetic materials and this area appears sufficiently promising so as to warrant further
investigation.
Historically, there has been a serious lack of data on dielectric properties of most
materials as a function of temperature over the microwave range. The data that are
beginning to emerge indicate that there is a complex interdependence of these properties
on temperature and frequency. The microwave processing community has begun to
address these complexities through improved dielectric measurement techniques and
processing equipment design. Several groups have established laboratories for measuring
the dielectric properties over broad ranges of microwave frequency and temperatures.
Many ceramics exhibit an abrupt increase in ε˝eff with increasing temperature, as
shown in Figure 6. Since Pa is directly proportional to ε˝eff, there is a corresponding
increase in the power absorbed and the heating rate of the ceramic as the temperature is
increased. The reason for this abrupt change in ε˝eff most likely is due to easier dipole
rotation that allows the peak shown in Figure 4 to move closer to the microwave
frequency being used. The temperature where the abrupt change in ε˝eff occurs is referred
to as the critical temperature, Tc. Below Tc, an external energy source is required to heat
the ceramic. Above Tc, the sample becomes self-heating in the microwave field. Very
few Tc values have been reported for ceramics thus far. Collection of more Tc values for
these materials would be very useful. There is no equation relating Tc to fundamental
materials values, thus the critical temperature values must be measured. For all
calculations and measurements, it is important to identify specifically the materials
characteristics (i.e., composition, phase, form) and assumed or measured process
parameters (i.e., temperature, pressure, atmosphere). For example, 99% alumina differs
from 96% alumina and α-SiC differs from β-SiC.
 Sample material
ε˝eff 1 2
or
Pa
Tlow Thigh

1 Tc 2

T
Figure 6. The effect of temperature on ε˝eff and Pa. Points 1 and 2 in the sample
material represent positions in or on the sample with different electric field
strengths. The electric field is greater at point 2.

A potential consequence of the rapid increase in ε˝ with temperature (dε˝/dT) is

that, unless the sample is heated uniformly by an external source, localized hot spots as
indicated by point 2 in Figure 6, can develop. The development of hot spots usually is
referred to as “thermal runaway” (unstable accelerated heating). This terminology is
unfortunate since it suggests a process that cannot be controlled. In fact, it is this very
property (large dε˝/dT) that permits the microwave heating of many materials that are
poor absorbers at ambient temperatures, as long as the entire sample is heated uniformly
by an external source and the internal field is fairly constant.
Some excellent quantitative models of thermal runaway have been developed in
the last few years. The models incorporate thermal conductivity, dielectric properties and
their nonlinear dependence on temperature. The effects of the electric field intensity,
sample size and insulation were evaluated thoroughly by Johnson et al using various
purities of Al2O3 as a model system. These investigators delineated regions of stable and
unstable heating and demonstrated that insulation normally used to contain the heat inside
the cavity exacerbates the problem of thermal runaway. However, the data also
suggested that thermal runaway could be minimized by hybrid heating (heating the article
with radiant heat at the same time that microwave energy is deposited into the sample)
and with proper control of the electric field. This is consistent with the experimental
results of many investigations using hybrid heating and controlling the electric field with
various techniques.
Many different aspects of the microwave process have been modeled: drying and
heating rates, temperature profiles, electric field distributions, power absorption and
hybrid heating. Most research has been focused on modeling the electric field inside a
loaded cavity, and then coupling these data with equation (1) and various heat transfer
equations. Huang et al used a variable mesh Finite-Difference-Time-Domain (FDTD)
analysis of electromagnetic power deposition in combination with a 3-D heat transfer
program to model sintering in a multimode cavity. This model accounts for external
stimuli, such as SiC heating rods (hybrid heating) and insulation effects. When the
dielectric and thermophysical properties are known as a function of temperature, the
model can accurately predict the heating rate of the sample, as shown in Figure 7.
Modeling can greatly help to understand the quantitative effects of microwave-material
interactions and will play an increasingly important role in the automation and control of
processing parameters.

Figure 7. Comparison between experimental and numerical results of a zirconia

sample’s temperature while heating in a multimode microwave cavity.

Equipment
A microwave system typically consists of a generator to produce the microwaves,
a waveguide to transport the microwaves and an applicator (usually a cavity) to
manipulate microwaves for a specific purpose and a control system (tuning, temperature,
power, etc.). Until recently, only fixed frequency single-mode or multimode systems
(home microwave ovens) were readily available. Single-mode systems have had limited
(but successful) applications in industry because of a limited processing volume over
which the electric field is useful, but have been particularly effective in plasma
processing, joining and fiber curing. In a multimode system, the fixed frequency
microwaves yield resonant modes over a narrow frequency band around the operating
frequency. The modes result in regions of high and low electric fields (i.e., non-
uniformity) within the cavity. In general, the uniformity of the field increases as the
cavity size increase, but the uniformity also is dependent on the overall cavity
dimensions.
Magnetrons, klystrons, gyrotrons and traveling wave tubes (TWTs) are used to
generate microwaves. Each has its advantages. For example, klystrons offer precise
control in amplitude, frequency and phase. Gyrotrons offer the possibility of providing
much higher power output (megawatts) and beam focusing. The TWTs can provide
variable and controlled frequencies of microwave energy. Magnetrons are by far the
most widely used microwave source for home microwave ovens and industrial
microwave systems, due to their availability and low cost. Solid state devices also are
available for generating microwaves, but typically have been limited in power (few tens
of watts).
The total cost of microwave processing equipment usually is greater than
conventional equipment designed to perform the same tasks. However, it is not easy to
do a one-to-one comparison between conventional and microwave processing equipment
because, in some cases, a hybrid system may be best. Certainly, as microwave energy
becomes more widely used for manufacturing ceramics, the costs will come down.
Shown in Figure 8 is a microwave furnace designed by Cober Electronics, Inc. for
manufacturing ceramics. In addition to the substantial amount of microwave power, the
equipment includes a hot air mode to provide high efficiency heating in conjunction with
the microwave power. The control systems are highly automated and precise with
minimum operating labor. Equipment of this type costs approximately $500,000
installed. Panasonic manufactures a microwave kiln that will achieve 1250°C and may
be used for both bisque and final firing of traditional ceramic ware. The system sells for
about $15,000 in Japan (Figure 9). Additional systems cost and efficiency information is
provided in Table 3. While the costs have changed significantly since Sheppard’s table
was produced, the relative data remains the same.

Table 3. Capital and operating costs of microwave equipment. Adapted from Sheppard, 1988.
COMPONENT TYPICAL COSTS
Complete System $1,000 – 5,000/kW
Generator < 50% system cost
Applicator > 50% system cost
Power Transmission $1,000 – 3,000; < 5% system cost
Instrumentation $1,000 – 3,000; < 5% system cost
External Materials Handling $1,000 – 3,000; <5% systems cost
Installation, Start-up 5 - 15% system cost
Magnetron Replacement $0.01- 0.12/kWh
Electric Energy $0.05 – 0.12/kWh
Plug-to-Product Efficiency 50 – 65%
Routine Maintenance 5 – 10%
 Figure 8. Hybrid microwave oven manufactured by Cober Electronics, Inc. for
drying technical ceramics (0.915GHz; 200kW).

Figure 9. Microwave kiln manufactured by Panasonic for firing ceramics

(2.45GHz, 6kW).

Certain features of microwave equipment have most likely hindered more

widespread use of microwave energy for industrial processes;(i.e, limited and fixed
frequencies, low temperature capabilities, field non-uniformity and complexity, and
inability to monitor or control the internal temperatures). Although microwave energy
covers a broad frequency range, in the United States, the Federal Communications
Commission (FCC) allocates frequency bands centered at 2.45GHz and 0.915GHz for
industrial, scientific and medical (ISM) use. These two frequencies provide a good
compromise between penetration depth, absorption and equipment costs for food
processing. Water and other polar molecules couple well with these frequencies.
Unfortunately for the rest of the materials processing community, they are not always the
optimum frequencies for heating polymers, ceramics, composites and other materials.
Most of the equipment is designed for low- temperature (few hundred °C) cooking and
drying. Consequently, the equipment is not designed or properly insulated for the high
temperatures (>1000°C) required to process most ceramics and composites. Field
uniformity also has been a problem, especially for the lower frequency microwaves (2.45
and 0.915GHz), where the wavelengths are several inches. As discussed previously, the
power absorbed by the material is strongly dependent on the internal electric field. In
turn, the internal field is controlled by the field inside the cavity, which can vary widely
in most cavities. Mode stirrers and moveable platforms provide some improvement in
the field uniformity as “seen” by the sample, through time averaging.
Potential users and equipment suppliers have, in many cases, avoided
implementing microwave technologies dues to (1) the complexity of the equipment, (2)
the need to perform expensive feasibility studies, and (3) the requirement for custom
designs. In the last few years, microwave equipment and component companies have
begun to more fully address these obstacles. Many equipment companies are alleviating
some of the complexities and research costs by allocating facilities and technical
assistance for customers to use for feasibility studies and prototype stage evaluations. If
prototyping proves successful, the equipment manufacturers are prepared to construct,
install and service the equipment, and to provide technical assistance during product
manufacture. As an example, Lambda Technologies, Inc. is commercializing variable
frequency microwave (VFM) equipment under exclusive license from Oak Ridge
National Laboratory for materials processing. This new generation of microwave oven is
computer controlled and takes advantage of broadband microwave sources (TWTs) to
tune the incident frequency to the materials to be processed. Furthermore, the VFM
system can sweep over several frequencies to achieve uniform distribution of the EM
field. These applicators are available now for research and industrial applications.
Many researchers use home microwave ovens that have been modified to suit
their needs. For example, when sintering ceramics, the oven must be well-insulated to
protect the interior from high temperatures. In most cases, granules or rods of highly
absorbing materials are attached to or embedded in the insulation to create susceptor
caskets. The ceramics to be heated are put into these caskets and then placed inside the
microwave oven. The microwaves heat the susceptors which, in turn, heat the ceramics.
Using this hybrid system, the ceramics are heated by both the radiant energy from the
susceptor and the microwave energy from the oven. In order to control and monitor the
temperature, shielded thermocouples as well as radiation pyrometers are used. These
devices provide feedback information to the control panel that controls the power to the
magnetron (Figure 10). Most home microwave ovens provide “power level” control
through a variable duty cycle. For example, a power level setting of 50 for a 1000 watt
oven might result in the magnetron being on “full power” for 50% of the specified
“cooking” time. The magnetron is cycled on/off using a specified time base (i.e., 15
seconds on/15 seconds off) to essentially achieve a 500 watt power level. In more
expensive industrial microwave ovens, the power level can be controlled without pulsing.
You can build as complex or as simple a system as you like. However, the real key to
success is to understand the basics with respect to microwave heating.

Figure 10. Schematic of a research system using a multimode microwave oven17.

(The SALI is transparent to microwave, but is a thermal insulator. To make the
SALI into a susceptor casket, it is lined with a microwave absorber, such as SiC.)

Why Use Microwave Energy?

Based on research performed by many engineers and scientists, a list of the
potential benefits as well as challenges and needs associated with microwave processing
has been compiled (Table 4).

Table 4. Benefits, challenges and needs of microwave processing18.

Benefits
Cost savings (time and energy, reduced floor space)
Rapid heating of thermal insulators (most ceramics and polymers)
Precise and controlled heating (instantaneous on/off heating)
Selective heating
Volumetric and uniform heating (due to deep energy penetration)
Short processing times
Improved quality and properties
Synthesis of new materials
Processing not possible with conventional means
Reduction of hazardous emissions
Increased product yields
Environmentally friendly (clean and quiet)
Self-limiting heating in some materials
Power supply can be remote
Clean power and process conditions
 Challenges
Heating low-loss poorly absorbing materials
Controlling accelerated heating (thermal runaway)
Exploiting inverted temperature profiles
Eliminating arcing and controlling plasmas
Efficient transfer of microwave energy to workpiece
Compatibility of the microwave process with the rest of the process line
Reluctance to abandon proven technologies
Timing
Economics

Needs
Availability of affordable equipment and supporting technologies
Kiln furniture, thermal insulation, and other processing support hardware
Development of compositions and processes tailored specifically for
microwave processing
Better fundamental understanding and modeling of microwave-material interactions
Better process controls, electronic tuning and automation (smart processing)
Better communication among equipment manufacturers,
technology developers, researchers and commercial users
More emphasis on microwave processing of magnetic materials

Cost Savings
A Canadian study has shown there can be considerable energy savings when
ceramics are manufactured with microwaves. Table 5 compares conventional drying and
firing with microwave drying and firing for a wide range of ceramic products. It can be
seen that there is a factor of about two in energy savings for microwave drying and about
a factor of ten in energy savings for microwave sintering. Similar savings have been
reported by E.A. Technologies for microwave hybrid heating, as discussed in more detail
in Wroe’s paper in this book.

Table 5. Comparison of energy savings for conventional and microwave drying and
firing of ceramics19.

A few examples of other benefits in ceramic processing are discussed below.

Many other examples can be found throughout this book.
Selective and Self-Limiting Heating
As discussed previously, many factors can influence the rate at which ceramics
heat in the microwave field (i.e., dielectric loss, sample volume). Leiser20 observed that
other factors, such as particle size and particle size distribution, sample geometry, and
material phase(s) present can influence the heating rate significantly. Leiser loaded an
alumina cement (microwave transparent) matrix with varying amounts of silicon carbide
(absorber) to determine the effects of the range of composite composition on heating
rates. The cement alone could not be heated much above room temperature. In contrast,
pure SiC could be heated rapidly and to very high temperatures. This research showed
(1) that the ratio of microwave-absorbing material to microwave-transparent materials
was significant when evaluating heating rate and maximum temperature, and (2) that self-
limiting heating also can be achieved by adjusting this ratio (Figure 11).

(a) (b)
Figure 11. Comparison of heating rates of susceptors as a function of particle
size and weight percent of silicon carbide: (a) 1000µm SiC; (b) 85µm SiC.

Volumetric and Uniform Heating

One of the most important characeristics associated with the use of microwave
hybrid heating is the potential to achieve uniform heating throughout the cross-section of
a material. In the late 1980s, De΄ et al showed that microwave hybrid heating could
result in samples with no significant density gradient throughout the cross-section and
that this phenomenon was enhanced with increased sample size (Figure 12)21. In
addition, he noted that the density was higher for the microwave hybrid heated samples
as compared to those processed with conventional fast firing techniques.
 Figure 12. Percent porosity versus sample thickness for alumina processed using
microwave hybrid heating and conventional fast firing methods.

Rapid Heating and Short Processing Times

As shown in Figure 13, microwave processing of materials offers the potential for
reducing production times for ceramic materials. The material for the study presented
was yttrium-barium-copper oxide superconductor and the sintering time was reduced
from over 900 minutes to under 200 minutes. Also note that the sintering temperature to
achieve 80% of theoretical density was reduced by over 100°C. This work, performed
by Ahmad et al, supported the data presented in Table 5, showing the potential for
significant cost savings in processing of ceramic materials22.

Figure 13. Typical sintering schedule for YBa2Cu3O7-x superconductors to

achieve 80% theoretical density.

Waste Treatment and Environmentally Friendly Technologies

In addition to offering the potential for advantages in ceramics fabrication,
microwave processing has been shown to reduce significantly the emissions generated
during processing operations. In a study by Earl et al presented in this book, it was
shown that microwave drying of tile resulted in an average reduction in flourine
emissions of approximately 33%. The possibility of significant emissions reduction
warrants further research.
In the 1990s, a large-scale research project conducted by the University of Florida
and Westinghouse Savannah River Company showed that microwave energy could be
used as a method for remediating waste materials (hazardous and nonhazardous) and
recycling precious metals. Schulz et al designed and built a tandem microwave system
that accomplished high-temperature incineration of composite feed stock (electronic
circuit boards), recycling of the valuable metal components and treatment of hazardous
emissions resulting from the incineration process. A schematic illustrating the basic
design of the system is provided in Figure 14.
While the value-added process of recovering recyclables during the volume
reduction experiments was a significant achievement, perhaps the most valuable results
were obtained in the emissions treatment portion of the work. As can be seen in Table 6,
hazardous emissions from the polymer incineration process were reduced by orders of
magnitude and, in some cases, were no longer detected using gas chromatography mass
spectroscopy (GCMS). This work indicates the value of microwave processing as a
“back end” technology as well as a “front end” production method.

Figure 14. Tandem microwave waste treatment and recycling system designed
and patented by the University of Florida and Westinghouse Savannah River
Company23,24.
 Table 6. Summary of GC Mass Sepctroscopy results of emissions resulting from
combusion of printed circuit boards (A = emission level before microwave treatment; B
= emission level after microwave treatment)25.

Frequently Asked Questions

As with any new technology, there always seem to be more questions than
answers. The list below contains many of the typical questions asked regularly of those
of us actively involved in microwave processing research and/or manufacturing*. Some
of the answers to these questions are provided in this Introduction, while others are
answered in the papers presented in this collection. You will most certainly have
additional questions that will not be answered in this book. For this reason, the contact
information for the first authors is provided in the appendices.

1. Can I use a home model microwave to perform research?

2. Can I get high temperatures in a low-power microwave oven?
3. What are the major components of a microwave oven?
4. How efficient is a microwave oven?
5. Can all materials be heated in a microwave oven?
6. What are the major safety issues with using microwave ovens?
7. How are microwaves generated?
8. What are the differences in microwave and radio frequency heating?
9. Why do some materials absorb and others reflect microwaves?
10. What is the difference between microwaves used in communications and in
processing?
11. How do you measure temperature in the microwave oven?
12. How do you measure electric field in a microwave oven?
13. What is the difference between single and multimode microwave cavities?
14. What is a susceptor?
 15. What is the microwave effect?
16. What are magnetrons, klystrons and gyrotrons?
17. Can microwaves be used for processes involving ceramics, other than drying?
18. What is the largest use of microwave energy for processing?
19. Can microwave ovens be scaled up to manufacture ceramics?
20. Is there an economic advantage in using microwave energy to manufacture
ceramics?
21. Are the properties of microwave and conventionally processed ceramics the
same?
22. What kinds of ceramics can be heated with microwave energy?
23. What is the cost of microwave equipment capable of manufacturing ceramics on
a large scale?
24. Why are the dielectric properties of ceramics important when microwaves are
being considered for heating them?
25. What is the operating frequency of a home model microwave oven and what are
some of the other frequencies that have been used to process ceramics?
26. What is the significance of an Industrial, Scientific and Medical (ISM) band?
27. Why do materials typically heat from the inside out in a microwave oven?
28. What is thermal runaway?
29. What are modes?
30. Why are some ceramics “microwave safe” and others not?
31. Where does all that energy go in an empty microwave oven when it is turned
on?

Recommendations
What needs to be done in order to generate more widespread use of microwave
energy in the ceramics industry? The National Materials Advisory Board convened a
committee in 1992 that heard presentations from a number of experts in the field. The
purpose of this committee was to recommend to the Department of Defense and the
National Aeronautics and Space Administration future directions for research and
development in microwave processing. While their recommendations do not specifically
address the question posed above, they do provide some specific direction for researchers
and manufacturers to move this technology forward. Following is a synopsis of the
committee’s recommendations as they pertain to ceramics2.

◊ Define the conditions under which microwaves provide uniform, stable heating
for ceramics. Hybrid heating schemes should be considered.
◊ Establish multidisciplinary teams to properly develop microwave processes and
procedures.
◊ Provide training and education in the fundamentals to ensure a knowledgeable
and sustainable workforce for the engineering technology.
◊ Compile existing ceramic property information in dielectric, magnetic and
thermal properties in the range useful for processing ceramics.
◊ Make better use of numerical modeling to design equipment and processes.
◊ Develop practical methods for monitoring and controlling microwave processing.
◊ Determine the validity of the “microwave effect.”
 The papers in this book are meant to help you to gain the insight that will lead to
successful evaluation of microwave energy as a solution to your processing needs. We
especially emphasize that you should read carefully John Gerling’s paper, “Equipment
Safety for Microwave and Radio Frequency Processing of Ceramics.” This overview of
safety issues will help prepare you to work with your microwave system and to separate
truth and fiction with respect to microwave oven safety.
If you prefer, there is a great deal of expertise in research on microwave
processing of a wide variety of materials that can be tapped into at academic and
government research laboratories. Many times it is better to work with an experienced
microwave research team than to “re-invent the wheel” in your own facility. However, if
you want to start the process from scratch, the information provided in this book should
be sufficient to get you started.

References
1 Materials Research Advisory Board, Microwave Processing of Materials, National Research Council,
Publication NMAB-473, National Academy Press (1994).
2 Clark, D.E. and Sutton, W.H., “Microwave Processing of Materials,” Annu. Rev. Mater. Sci., 26:299-331
(1996).
3 Ceramic Transactions - Microwaves: Theory and Application in Materials Processing, D.E. Clark, F.D.
Gac and W.H. Sutton, eds., American Ceramic Society, Inc., Vol. 21, Westerville, OH (1991).
4 Ceramic Transactions - Microwaves: Theory and Application in Materials Processing II, D.E. Clark,
W.R. Tinga and J.R. Laia, Jr. eds., American Ceramic Society, Inc., Vol. 36, Westerville, OH, (1993).
5 Ceramic Transactions - Microwaves: Theory and Application in Materials Processing III, D.E. Clark,
D.C. Folz and R. Silberglitt, eds., American Ceramic Society, Inc., Vol. 59, Westerville, OH, (1995).
6 Ceramic Transactions - Microwaves: Theory and Application in Materials Processing IV, Proceedings
from the First World Congress on Microwave and RF Processing, D.E. Clark, W. Sutton and D.L. Lewis,
eds., American Ceramic Society, Inc., Vol. 80, Westerville, OH (1997).
7 Ceramic Transactions – Microwaves: Theory and Application in Materials Processing V, Proceedings
from the Second World Congress on Microwave and RF Processing, D.E. Clark, J.G.P. Binner and D.A.
Lewis, eds., American Ceramic Society, Inc., Vol. 111, Westerville, OH (2001).
8 Microwave and Radio Frequency Applications, Proceedings from the Third World Congress on
Microwave and RF Processing, D.C. Folz, J.H. Booske, D.E. Clark and J.F. Gerling, eds., American
Ceramic Society, Westerville, OH (2003).
9 Tinga, W.R. and Voss, W.A.G., Microwave Power Engineering. 1968. New York: Academic
10 Levinson, M.L., 1971. U.S. Patent No. 3585258.
11 Bennett, C.E.G., McKinnon, N.A. and Williams, L.S., 1968. Nature 217:1287-88.
12 Sutton, W.H., 1988. Microwave Processing of Materials, 124. Reno: Mater. Res. Soc. 399 pp.
13 Janney, M.A. and Kimrey, H. 1988. Ceramic Powder Science II, Ceram. Trans. Westerville, OH: Am.
Ceram. Soc. 1:919-24.
14 Metaxas, A.C. 1993. See ref. 4.
15 Hench, L.L. and West, J.K. 1990. Principles of Electronic Ceramics. New York: Wiley & Sons. 546 pp.
16 Metaxas, A.C. and Meredith, R.J., Industrial Microwave Heating, Peter Peregrinus Ltd., London, United
Kingdom (1988).
17 Fathi, Z., Surface Modification of Sodium Aluminosilicate Glasses Using Microwave Energy. Doctoral
dissertation, University of Florida (1994).
18 Clark, D.E. and Sutton, W.H., “Microwave Processing of Materials,” Annu. Rev. Mater. Sci., 26:299-
331 (1996).
19 Sheppard, L.M., Ceramic Bulletin, 67 [10] 1988. 1656-61.
20 Leiser, K.S., Microwave Behavior of Silicon Carbide/High Alumina Cement Composites. Doctoral
dissertation, University of Florida (2001).
 21 De΄, A. Ultra-Rapid Sintering of Alumina with Microwave Energy at 2.45GHz. Masters thesis.
University of Florida (1990).
22 Ahmad, I., Chandler, G.T. and Clark, D.E., Microwave Processing of Materials Proceedings, W. Sutton,
I. Chabinsky and M. Brooks, eds., Vol. 124, Materials Research Society, Pittsburgh, 239-246 (1988).
23 Wicks, G.G., Schulz, R.L. and Clark, D.E., Tandem Microwave Waste Remediation and
Decontamination System, U.S. Patent # 5,968,400, issued 10/19/99.
24 Wicks, G.G., Schulz, R.L. and Clark, D.E., Microwave Waste Treatment and Decontamination System,
U.S. Patent # 6,262,405, issued 6/17/2001.
25 Clark, D.E., Folz, D.C., Schulz, R.L. Boonyapiwat, A., DiFiore, R.R., Darby, G. and Leiser, K., (1997)
See Ref. 6.

View publication stats