Int. J. Appl. Ceram. Technol.

, 12 [5] 909–920 (2015)

DOI:10.1111/ijac.12305

Development of Silicon Nitride-Based Ceramic Radomes — A

Review
Kishore Kumar Kandi,* Nagaveni Thallapalli, and Surya Prakash Rao Chilakalapalli
Department of Mechanical Engineering, National Institute of Technology, Warangal 506 004, Telangana, India

Radome is an aerodynamic structural part attached to the fore-end of a missile. It transmits electromagnetic signals with
minimum attenuation and also protects radar communication system, and thus, the radomes are made of ceramics as they have
desirable properties required by the radomes. The flexural strength, dielectric constant, and loss tangent values of various ceramic
materials used in the development of radomes are important in the selection of radome materials. Different nose cone shapes of
missile radomes are also important. Ceramic materials show variational properties with sintering time, temperature, and other
additives. The existing different near-net shape fabrication techniques for manufacturing of ceramic radomes are discussed and
compared. Gelcasting is one of the manufacturing techniques to produce radomes with homogeneous and high green strength.
Gelcast parts of silicon nitride ceramics are hard, tough, brittle, and wear-resistant and are difficult to machine using conven-
tional methods of machining. Therefore, laser-assisted machining is used for fine finish of ceramic radomes with excellent surface
integrity and productivity. This paper deals with a review of development of ceramic radomes, manufacturing methods for variety
of applications.

Introduction antennas, and radar dishes to protect radar antenna from

Ceramic radomes are typically used for missiles
intended to operate at speeds of Mach 4 or higher, also
called hypersonic regime.1 Numerous investigations are
going on for the development of radomes with ceramic
materials for high-speed missiles. Radome must have suf-
ficient structural strength and fracture resistance to with-
stand the aerodynamic forces and foreign object
impingement and also it should offer minimal aerody-
namic resistance. The radome should have minimal
attenuation and distortion of the outgoing and incoming
radar energy.2 The materials used for construction of
radomes for high-speed missile applications should pos-
sess high flexural strength, low dielectric constant, low
loss tangent, high thermal shock resistance, high rain
erosion resistance, etc.3
A radome (the word is a contraction of radar and
dome) is a light weight structural, weatherproof enclo-
sure that protects a microwave or radar antenna. The
radome is made of some material that minimally attenu-
ates to the electromagnetic signal transmitted or received
by the antenna. In other words, the radome is transpar-
ent to radar or radio waves.4 A radome is often used to
prevent ice and freezing rain from accumulating directly
onto the metal surface of the antennas. Radomes can be
manufactured into desired shape and are widely used in
marines, naval shipboard, aircraft, missiles, stationary
*kishorekumar01@gmail.com
© 2014 The American Ceramic Society
wind, blowing sand, snow, ice, rain, ultraviolet sun light,
temperature, fungus, and corrosion. Radomes are widely
made of ceramics as they were light in weight and have
good mechanical and electronic properties.
Ceramic material properties strongly depend on the
ceramic powder morphology, impurity, sintering aids and
their composition, and forming and sintering parameters.5
The two most important parameters to evaluate the
dielectric properties of a material are its dielectric con-
stant e and loss tangent d (also called as dissipation fac-
tor). To obtain excellent wave-transparent properties for
high-speed radome materials, e and tan d should be less
than 4.0 and 0.01, respectively. Near-net shape ceramics
are commonly produced through forming techniques
such as tape casting,6 slip casting,7,8 pressure casting,9
freeze casting,10 cold isostatic pressing,11 direct coagula-
tion casting, electrophoretic casting, hydrolysis-assisted
solidification,12 injection molding,13,14 and gelcast-
ing.15,16 In each of these techniques, the ceramic powder
is suspended in liquid-binder system for shaping and all
these forming methods start with a suspension where the
ceramic particles are mixed with solvent, proper disper-
sant and possibly further additives such as binders,
plasticizers, and antifoaming agents so as to produce well-
dispersed, nonagglomerated ceramic slurry.17 Upon form-
ing, the component is solidified by gelling, drying, or
cooling and finally any remaining liquid present is
removed, organic binders are burned out, component is
sintered, and further may be machined if necessary.
910 International Journal of Applied Ceramic Technology—Kandi, Thallapalli, and Chilakalapalli Vol. 12, No. 5, 2015

Recently, Zou et al.18 prepared wave-transparent effect of nose shape on drag becomes highly significant.
porous Si3N4 ceramics by gelcasting and gas-pressure sin- The factors influencing the pressure drag are the general
tering, and the effects of solid loading on microstructure, shape of the nose cone, its fineness ratio, and its bluff-
mechanical, and dielectric properties were investigated. ness ratio. The ratio of the length of a nose cone com-
Microstructures with interlocked elongated b-Si3N4 pared with its base diameter is known as the fineness
grains and uniformly distributed pores were observed, ratio. At supersonic speeds, the fineness ratio has a very
while both the b-Si3N4 phase content and grain aspect
ratio reduced as the solid loading increased due to the
restrained anisotropic growth of b-Si3N4 grains. b-Si3N4
is stable at high temperatures and increases the toughness High Blunt
of the matrix. As the solid loading increased from 30 to
45 vol.%, the porosity of ceramics reduced from 57.6%
to 36.4%. The flexural strength increased linearly from
108.3 to 235.1 MPa, and the dielectric constant and loss
tangent of ceramics increased from 0.00263 and 0.00285 Blunt Cone
to 0.00368 and 0.00356 (10 GHz), respectively. This
technique is considered to be an efficient way to prepare
high-performance porous Si3N4 ceramics.

Drag
There is a need to prepare porous Si3N4 ceramics,
which can improve the wave-transparent properties. Cone
There are several factors involved in manufacturing
radomes right from selection of material, manufacturing
process, and further machining of radomes to its desired
shape and size.
Ogive
Different Shapes of Missile Radomes

The most common nose shapes are conical, tangent Low Parabola
or secant ogive, elliptical or hemispherical, power series,
parabolic series, haack series, or Von Karman. Some of
the nose cone shapes are shown in Fig. 1.
Fig. 2. Performance of drag on various nose shapes.
Below Mach 0.8, the nose pressure drag is essentially
zero for all shapes and the pressure drag increases dra-
matically in the transonic region and beyond, where, the
Tangent Ogive r

x=0
y

y=0
Conical 3/4 Power
x
x=L
L y=r

Tangent Ogive Ellipsoid

Secant Ogive LV-Haack

1/2 Power Von Karman

Fig. 1. Different types of radome nose shapes. Fig. 3. Tangent ogive formed from the segment of a circle.
www.ceramics.org/ACT Development of Si3N4 Based Ceramic Radomes
significant effect on nose cone wave drag. Fineness ratio
of 5 is critical as the fineness ratio increases, and the wet-
ted area and the skin friction component of drag
increases.19 Sharp tips are ideally formed in most of the
nose cone shapes and are often blunt to some degree for
ease of manufacturing, resistance to handling, flight dam-
age, and safety. This blunt is most often specified as a
hemispherical “tip diameter” of the nose cone. The term
bluffness ratio is often used to describe a blunt tip and is
equal to the tip diameter divided by the base diameter.
Fortunately, there is little or no drag increase for slight
blunt of a sharp nose shape. In fact, there is a decrease
in drag for bluffness ratios upto 0.2, with an optimum
of 0.15 for constant overall lengths. Most commercially
made tangent ogive nose cones are blunt to a bluffness
ratio of about 0.1. Comparison of drag for different nose
shapes of the radomes is shown in Fig. 2.20
For airborne radomes, the shape is chosen to be tan-
gent ogive to withstand the aerodynamic drag.21 The
ogival shape has several advantages such as slightly
greater volume for a given base and length, a blunter
nose, providing structural superiority and slightly lower
drag.22 The profile of tangent ogive is formed by a seg-
ment of a circle such that the rocket body is tangent to
the curve of the nosecone at its base; and the base is on
the radius of the circle as shown in Fig. 3.
The radius of the circle that forms the ogive is
called the ogive radius, R, and it is related to the length
and base radius of the nose cone, r:
r 2 þ L2
R¼
2r
The radius y at any point x, as x varies from 0 to L is:
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
y ¼ R 2  ðx  LÞ2 þ ðr  RÞ
The nosecone length, L, must be equal to, or less
than the ogive radius. If they are equal, then the shape is
a hemisphere. The fore-end of missile shell radius is
equal to the base radius (r) of radome.
Selection of Materials for Radome Structure
As shown in Fig. 4, the radome wall structure
greatly determines the use of the defined frequencies or
broadband (1–18 GHz) wave transmissions23 and for the
defined frequency application half-wave wall structure is
used.24
The most commonly used and reported broadband
radome wall structure includes A-sandwich, C-sandwich,
and multilayer. However, these structures are not suitable
911
Half-wave wall
Thin wall
A-Sandwich
B-Sandwich
Broadband
C-Sandwich
Multilayer
Graded
Fig. 4. Schematic diagram of radome wall structure.
for high-temperature environment, due to the big mis-
match of the thermal properties (namely the ultrahigh
residual thermal stress) of each layer, which may restrain
their application in the high-speed missile radome.25 The
structure is designed to be composed of an odd multiple
of five or more layers with no central matching layers at
the design frequency. Investigations indicate that the
multilayer structure exhibits multiband transmission
property. The central-layer thickness can be chosen in
the range of 0.1–6 wavelengths, so as to provide suffi-
cient mechanical strength and structural rigidity for the
whole radome structure. The multilayer structure at a
design frequency of 65 GHz turns to be a broadband
radome wall structure in the 16–100 GHz frequency
range for both centimeter and millimeter waves applica-
tions.26 To relieve the thermal stress between the layers,
specially designed functionally graded materials have
been developed and are used for ultrahigh temperature
application.27
Modern ground-based and ship-based radomes are
manufactured using composite materials such as fiber-
glass, quartz, and aramid fibers held together with poly-
ester, epoxy, and other resins. Materials for developing
ceramic radomes include fused silica (SiO2),28 silicon
nitride–barium aluminum silicate composites (Si3N4/
BAS),29,30 aluminum phosphate–mullite composites
(AlPO4/3Al2O3.2SiO2),31 silica–aluminum nitride
composites (SiO2-AlN),32 silica fiber reinforced silica–
boron nitride composites (SiO2f/SiO2-BN),33 aluminum
borate whisker/aluminum phosphates composites
(9Al₂O₃.2B₂O₃/AlPO4),34 liquid-phase silicon nitride,35
Si2N2O composites,36 reaction-bonded silicon nitride,37
b-Si4Al2O2N4,38 b-Si4Al2O2N4-SiO2,39 b-SiAlON,40,41
few of these materials with efficient properties with con-
siderable importance are shown in Table I.
Fused silica can be used only for low-speed radomes
because of its low strength (40–50 Mpa) but has an
912 International Journal of Applied Ceramic Technology—Kandi, Thallapalli, and Chilakalapalli Vol. 12, No. 5, 2015

Table I. Characteristics of Commonly Used Radome Materials

Materials Flexural strength (Mpa) Dielectric constant e Loss tangent tand References
Fused silica 40–50 4.01 <0.01 28
40
b-SiAlON 266 7.34 0.003–0.004
36
Si2N2O 190 4.80 0.0025
AlPO4-mullite 168  7.6 3.42 0.00475 31
33
SiO2f/SiO2-BN 58.9 3.22 0.0039
Si3N4-BAS 420 8.16 – 29
5
Si3N4 600–1000 8.59 0.013
b-Si4Al2O2N6 226 7.72 – 38

b-Si4Al2O2N6 –SiO2 199 6.32 0.002 39

18
Porous Si3N4 57–176 2.35–3.39 0.0035
40
Reaction-bonded Si3N4 180 4–6 0.002–0.005
34
9Al₂O₃.2B₂O₃/AlPO4 215.3 4.23 0.0024

excellent dielectric constant of 4.01 and has loss tangent
<0.01 at 1000°C.28 Preparing Si2N2O composites
repeatedly with consistent properties is not possible
because of its final chemical composition as it depends
on the extent of oxidation of a-Si3N4 materials that
occur upon calcinations in atmospheric air and does not
depend on the initial precursor material compositions
although the dielectric properties of these materials are
good.42 Preparing radome structure was quite difficult
using Si3N4/BAS, although it poses high flexural strength
(420 Mpa).29 b-SiAlON material can be shaped into
radome structures and can be sintered to full density
without disturbing the structure, but fixing the best
chemical composition based on the required properties
and processing of these materials is quite difficult.40,41
Si3N4 ceramic can be shaped into radome structures
using near-net shape forming techniques, and the major
drawback of dense sintered silicon nitride materials is its
poor sintering ability although it possesses exceptionally
high flexural strength (600–1000 Mpa)5 and it can with-
stand high temperatures and has well-acceptable dielec-
tric properties. Low-density porous silicon nitride
ceramic has been used as radome materials owing to its
rather low dielectric constant and loss tangent, high
chemical stability, high melting point and extremely low
coefficient of thermal expansion. The existence of the
pores in the silicon nitride ceramic will lower the dielec-
tric constant and the dielectric loss tangent according to
Bruggeman theory.43
Silicon nitride ceramics have great demand for high-
temperature applications such as radomes and turbine
rotors, as it posses high flexural strength, high fracture
resistance, high thermal shock resistance, high chemical
resistance, good oxidation resistance, and low thermal
expansion coefficient.44,45 Si3N4 has strong covalent
chemical bond and two forms, a and b phases. Nowa-
days, various processing techniques have been developed
to prepare both the porous and dense Si3N4 ceramics for
structural and functional applications.25 These materials
can be densified under pressureless sintering conditions
by adding certain amount of sintering aids at high tem-
peratures (1750–2000°C). Si3N4 may be well stabilized
electro-statically against agglomeration in aqueous slips
either at pH of <5 or >9, having either a positive charge
or negative charge, respectively.46
Addition of certain oxides in the sintering of nitrides
is a well-known technique for producing dense ceramics
for engineering applications.47 Many of the oxide materi-
als such as magnesium oxide (MgO),48 yttria (Y2O3) and
alumina (Al2O3),49–51 beryllia (BeO),52 zirconia
(ZrO2),53 calcium oxide (CaO),54 ceria (CeO2),55 hafnia
(HfO2),56 yttria and hafnia (HfO2),57 lutetium oxide
(Lu2O3) and silica (SiO2),58 ytterbium oxide (Yb2O3) and
silica (SiO2),59 yttria and neodymium oxide (Nd2O3),60
lanthanum oxide (La2O3)61 are used as sintering aids.
Diffusional mass transport by solid-state diffusion is
very slow as there is a high degree of covalent bonding
crystal structure in silicon nitride and hence by liquid-
phase sintering the silicon nitride powders are converted
into a dense body. Generally 1–5 wt% silica (SiO2) is
contained by the Si3N4 as a surface oxidation layer as an
oxide additive at certain high temperatures reacts with
the SiO2 to form silicate liquid that aids densification.62
During sintering of silicon nitride ceramics, silica
naturally acts as a sintering aid, which reacts with other
sintering aids and plays an important role in determining
the final mechanical properties of silicon nitride ceram-
ics.63
To densify Si3N4 ceramics the first sintering additive
used was Magnesium oxide (MgO) and among all oxide
www.ceramics.org/ACT Development of Si3N4 Based Ceramic Radomes 913

sintering aids the best-known system is the yttria–alu-

References
mina (Y2O3–Al2O3). The addition of yttrium or alumi-
num oxide is due to their sintering qualities at high
temperature and their high stability in reductive atmo-

47
67
51

35
68
69
70
71
72

73
18
3
spheres.64 Y2O3 and Al2O3 sintering aids65 are most

Increase in strength, fracture toughness and wear rate

widely used for preparation of Si3N4 ceramics possessing

High fracture toughness and high flexural strength

High flexural strength and low dielectric constant
high strength at temperatures higher than 1000°C
shown in Table II. On cooling, the liquid phase crystal-
lizes to an yttrium–aluminum garnet phase. The fabri-
cated Si3N4 shows improved high-temperature creep

Table II. Characteristics of Commonly Used Si3N4 Sintering Aids, Process, and Temperatures

improvement in dispersion properties

resistance as well as better oxidation resistance.62 Scan-

High fracture resistance and strength

ning electron micrograph of silicon nitride densified with

Observations

Increase in mechanical properties

Improved mechanical properties

Y2O3 and Al2O3 showed an elongated rod-like b-silicon

High density is obtained and

nitride grains surrounded by a Y-Si-Al-O-N glass

High temperature strength

phase.66

Increase in densification
Increase in bulk density
Higher green density

High densification
Selection of Sintering Process

As the properties of a material strongly depend on

the fabrication method, different sintering techniques
have been developed.74 The most common sintering
methods to densify Si3N4-based ceramics are: reaction
bonding (RBSN),75 hot pressing (HPSN),76,77 sintering
Pressure
(MPa)

(SSN), sintering reaction bonding (SRBSN), hot isostatic

0.225
2.63
pressing (HIPSN),78 gas-pressure sintering (GPSN),79,80

0.1

0.5
0.1

0.6
48
30

10
–

1
and pressureless sintering (PLS).7,48 The thermomechan-
ical properties of Si3N4 materials are shown in Table III.
Time (h)

Pressureless sintering of Si3N4 occurs by a liquid-

HP, Hot pressing; PLS, Pressureless sintering; S, Sintering; GPS, Gas-pressure sintering.
phase sintering process.81 Pressureless sintered silicon
–
1
2

4
6
1
1–4
2
2
1–2
1
1
nitride has several favorable features and properties
which make it a promising candidate for radome materi- N2/Ar
used
Gas

als. Pressureless sintering provides relatively unlimited

N2
N2
N2

N2
N2
N2
N2

N2
N2
N2
N2
shape forming capabilities, and the process can be con-
trolled for reproducing and parts can be made relatively
temperature (°C)

inexpensive. Pressureless sintered silicon nitride provides

Sintering

some excellent physical and mechanical properties which

1750–1950

1800–2000

1700–1800

1600–1800

approach hot-pressed silicon nitride and posses excellent

oxidation resistance above 1350°C. It provides high
1750

1750

1650
1850

1725

1750

1800
1750

strength from room temperature to above 1250°C has

excellent thermal shock resistance due to low thermal
expansion and high strength provides opportunities to
Process
used

wide applications.35 For pressureless sintering, consider-

GPS
GPS

GPS
PLS

PLS
PLS
PLS
HP
HP

HP

able amount of oxide additive should be used, which

S

may tend to decrease the high-temperature strength of

Al2O3

the sintered body.82 An alternate to pressureless sintering

Sintering aids (%)

1.5
1.5

is the gas-pressure sintering which owns the advantages

0
5
6

4
2
5
5
3
2
3

of hot pressing, pressureless sintering, and hot isostatic

pressing. Full dense Si3N4 parts can be produced by
adding relatively large amount of sintering additives such
Y2O3

as yttrium oxide and alumina and using high gas pres-

4.5
5
5
14

6
5
10
2
6
6
5
8

sure above 30 MPa. In contrast, relatively low gas pres-

914 International Journal of Applied Ceramic Technology—Kandi, Thallapalli, and Chilakalapalli Vol. 12, No. 5, 2015
Table III. Thermomechanical Properties of Si3N4 Materials (After Greil46 with Permission. Copyright Elsevier.)
Oxygen Porosity Elastic
Material content (wt%) (vol.%) modulus (GPa)
RBSN 1–2 8–25 80–220
SRBN 2–8 1–8 100–300
SSN 3–12 1–5 140–320
GPSN 2–10 1–5 200–320
HIP/HPSN 2–6 0.5–2 250–340
RBSN-reaction bonded; SRBN-sintered reaction bonding; SSN-pressureless sintered; GPSN-gas-pressure sintered; HIP/HPSN-hot pressed.
sure will lead to high-performance porous Si3N4 ceram-
ics.30
Selection of Near-Net Shape Fabrication Technique
Material processing techniques are continuously
expanding with respect to development of new materials,
and new processing methods are to be investigated and
refined for efficient processing. Ceramic engineers have
attempted many of the forming techniques for the near-
net shape fabrication of ceramic materials. Near-net
shape ceramics are commonly produced through forming
techniques such as tape casting, slip casting, pressure
casting, freeze casting, cold isostatic pressing, direct coag-
ulation casting, electrophoretic casting, hydrolysis-assisted
solidification, injection molding, and gelcasting.
Tape casting is used to produce thin sheets only.
Slip casting is a low-pressure filtration method where
capillary suction provides the driving force (0.1–
0.2 MPa) for liquid removal and formation of a cast
layer at mold surface. It is generally a slow process,
because the casting rate decreases parabolically with
thickness of the cast layer. Pressure casting is a modifica-
tion of slip casting that has been developed to obtain a
higher green density, and in this method, an external
pressure below 4 MPa substantially higher than the cap-
illary suction pressure is applied to the ceramic suspen-
sion.83 The traditional drain-casting methods are plagued
by some generic problems as the liquid flow affects the
suspension microstructure and tends to orient nonspheri-
cal constituents, such as whiskers. The stress gradient
may cause mass segregation because of differences in par-
ticle size and density84 and also leads to nonuniform
densities of the green body.85 Freeze casting offers excel-
lent rheological properties and provides high green
strength, but the major drawback is the volume expan-
sion of water which causes cracks in the component.
Cold isostatic pressing (CIPing) is probably the most
important forming technique for industrial production
Fracture toughness Modulus of Weibull
(MPa m1/2) rupture (MPa) factor (m)
2–4 50–350 6–15
4–6 300–700 10–15
5–7 400–900 5–15
5–12 600–1200 10–20
5–8 600–1400 10–25
of ceramic materials. But problems associated with this
technique are density gradients, inhomogeneous micro-
structures, and the need to machine complex-shaped
objects. Solidification is obtained by coagulation in direct
coagulation casting. Excellent rheological properties and
high green density are obtained, and the major draw-
backs are expensive additives and poor green strength.
The electrophoretic casting is considered to be a power-
ful forming technique as it is extremely versatile, low
cost, and reliable process. Problems that could be faced
during this process are: unwanted water electrolysis, gal-
vanic reactions, and water electro-osmosis. The benefits
of this process are excellent rheological properties, fast
solidification, and high degree of density. The drawbacks
include limited time and temperature stability, heat
transfer during solidification, and need of additional
equipment to collect and neutralize ammonia. Addition-
ally, the process is not suitable for all types of ceramics.
Forming methods, such as injection molding and gelcast-
ing have the potential to avoid the aforementioned prob-
lems. Injection molding has proved to be an excellent
forming technique for small objects although there are
potential problems related to the die-filling process.
Abrasive wear of screw-driven injectors for high-pressure
injection molding can also lead to metallic inclusions
and poor reliability. The major problem confronting
injection molding is the removal of the binder. Binder
burnout must proceed at a slow rate to avoid problems
with slumping and crack formation.17
Gelcasting, a ceramic forming process was developed
at Oak Ridge National Laboratory by Janney and Omat-
ete to overcome some of the limitations of other com-
plex-shape forming techniques such as injection molding
and slip casting.15,86 During gelcasting, ceramic powders
are dispersed in an aqueous solution containing a mono-
mer, cross-linker, free radical initiator, and catalyst to
form a fluid and castable slurry is poured into an appro-
priately designed mold and polymerized in situ to form a
polymer–water gel that immobilizes the dispersed cera-
mic powder particles in the shape of the mold cavity.
www.ceramics.org/ACT Development of Si3N4 Based Ceramic Radomes 915

The gel part with uniform chemistry and density is few percent of organic components making binder
removed from the mold while still in wet condition and removal much less critical compared with injection
then dried in controlled conditions to get green body molding.87 Gelcasting has more advantages such as the
which is strong enough to be machined. Binder removal products produced are consistently defect free, uniformly
and sintering takes place as in other ceramic processes, dense and very strong, and able to form very large parts
and the details of gelcasting process are shown in Fig. 5. compared with other forming processes shown in
In gelcasting, the gel parts are more homogeneous and Table IV. Gelcasting is attractive for fabricating complex
have a much higher green strength in contrast with slip shapes such as radome shown in Fig. 6, respectively.
casting and pressure casting. Gelcast parts contain only a It is important to understand the role of particle
interactions in determining the slurry rheology shown in
Fig. 7 to control the parameters such as pH, dispersant
CERAMIC
amount, monomer content, and solid loading which
POWDER
have a strong effect on mechanical properties of green
ORGANIC WATER
body and also have influence on process viability for
MIXING/MILLING
MONOMERS
(BINDERS)
(SLURRY)
DISPERSANT
manufacturing. Therefore, it is necessary to understand
DEAIR
how an optimum suspension of ceramic particles can be
CATALYST INITIATOR
created.17 The influence of dispersant addition on the
interaction among particles in Si3N4 aqueous suspension
CASTING
can be observed via zeta potential measurements,88 and
GELATION some of the dispersants used for Si3N4 slurry stabiliza-
tion are listed in Table V.
MOLD REMOVAL The heart of gelcasting technology is use of an
GREEN
organic monomer solution that can be polymerized to
DRYING
MACHINING form a strong and cross-linked polymer–solvent gel, and
the macromolecular gel network resulting from the in
BINDER BURNOUT
situ polymerization holds the ceramic particles in the
SINTERING MACHINING given mold shape. The monomer solution consists of the
solvent (typically water), a chain forming monomer, a
Fig. 5. Flowchart of gelcasting process. chain branching (cross-linking) monomer, and a free rad-

Table IV. Comparison of Near-net Shape Fabrication Techniques (After Janney et al.86.)
Property Gelcasting Slip casting Injection molding Pressure Casting
Molding time 5–60 min 1–10 h 10–60 sec 10 min–5 h
Strength (As-formed) Moderate to high Low High Low
depending on
gel system
Strength (Dried) Very high Low N/A Low
Mold materials Metal, glass, Plaster Metal Porous plastic
polymer, wax
Binder burnout 2–3 h 2–3 h Up to 7 days 2–3 h
Molding defects Minimal Minimal Significant Minimal
Maximum >1 m >1 m ~30 cm, one dimension ~0.5 m
part dimension must be ≤1 cm
Warpage during Minimal Minimal Can be severe Minimal
drying/binder
removal
Thick/thin sections No problem Thick section increases Problems with binder Thick section increases
time of cast removal in thick sections time of cast
Particle size Viscosity goes up Casting time goes up Viscosity goes up Casting time goes up
as size goes down as size goes down as size goes down as size goes down
916 International Journal of Applied Ceramic Technology—Kandi, Thallapalli, and Chilakalapalli Vol. 12, No. 5, 2015

Repulsive forces (dispersed systems)

Liquid-like
microstructure of
individual
particles.
Usually no yield
stress

Weak attractive forces (Weak flocculation)

Particles form
loose flocs which
flow as units.
Shear thinning is
observed

Fig. 6. Si3N4-based radome. (After Ganesh and Sundarara-

Strong attractive forces (coagulation)
jan.40.).

ical initiator. Gel formation is shown in Fig. 8; here, the Interconnected

chain building monomer is depicted as “M”, and the
chain branching or cross-linking monomer is depicted as
“X”. Upon the addition of free radicals to the solution,
the “M” monomers react to form long chains that are
occasionally caused to branch by the incorporation of
the “X” monomers. The result is a very high molecular
weight polymer that fills space and traps the solvent mol-
ecules among its branches and the macroscopic result is
a polymer–solvent gel.89
The influence of ratio of monomers on flexural
strength of green body and sintered body is shown in
Figs. 9a and b, respectively. The flexural strength first
increases and reaches maximum value with an increase of
the ratio of monomers and then decreases which indicate
that the ratio of monomers has an optimum value where
fractal networks
are formed with a
measurable yield
stress
Fig. 7. Illustration of the connection between suspension micro-
structure, interparticle forces, and rheological behavior. (After Sig-
mund et al.17).
the flexural strength of green body is highest. The varia-
tion of flexural strength of sintered body and green body
with the ratio of monomers is similar, and high-perfor-
mance sintered body can be achieved by high-perfor-
mance green body. The high strength of green body has
a great advantage for handling and machining before sin-

Table V. Dispersants Used for Si3N4 Slurry Stabilization

Dispersant Manufacturer Chemical basis
Dolapix CA Zschimmer & Schwarz, Lahnstein, Germany Synthetic polyelectrolyte
Dolapix PC21 Zschimmer & Schwarz Synthetic polyelectrolyte
Dolapix PC33 Zschimmer & Schwarz Poly(acrylic acid) — aminomethyl propanol
Dolapix PC75 Zschimmer & Schwarz Poly(acrylic acid) — ammonium salt
Dolapix CE64 Zschimmer & Schwarz Carboxylic acid preparation
Dolapix A88 Zschimmer & Schwarz Amino alcohol
Duramax D-3007 Rohm and Haas, Philadelphia, PA Sodium salt of an acrylic copolymer
Vanisperse CB Borregaard, Sarpsborg, Norway Sodium lignosulphonate
Darvan C-N R.T. Vanderbilt, Norwalk, CT Ammonium polymethacrylate
Darvan 821A R.T. Vanderbilt Poly(acrylic acid) — ammonium salt
www.ceramics.org/ACT Development of Si3N4 Based Ceramic Radomes 917

Monomers in solution Polymer-Solvent Gel (a) 90

M M
M M M 85
X M M X M MC=40 wt% Solid loading=40 wt%
M M M M
M M M 80
M M
M M

Flexural strength (MPa)

M M M
M M 75
M M M
X
M M 70
M Free Radical M
X M
M M X
M M 65
M
M
M
M
X M M
M M M 60
M M X M
M M M
M X 55
M
Liquid solution Solid Gel 50

45
Fig. 8. Formation of polymer–solvent gel.
40 4 6 8 10 12 14 16 18 20 22
Ratio of monomers
tering. Both green body and sintered body have a maxi-
mum value at the optimum ratio of monomers. Fig- (b) 155

ure 10 shows the influences of monomer content on the

flexural strength and porosity of Si3N4 sintered body. 150
The porosity monotonically increases with increase of Flexural strength (MPa)

monomer content and the flexural strength decreases.

145
The pores of sintered body mainly originate from the
residual microspace of the organic processing aids in the
green body during organic binder burnout. Therefore, 140
the porosity monotonically increases with increase of
monomer content.90 MC=40 wt% Solid loading=40 wt%
135

Selection of Machining Technique and Tool 130

0 5 10 15 20 25
For machining of gelcast radomes, various machin- Ratio of monomers

ing techniques can be used such as green ceramic
machining (before sintering), direct laser machining, and
laser-assisted machining (after sintering).
Advanced ceramic materials such as silicon nitride
are hard, tough, wear-resistant, and chemically stable,
even at high temperature. These properties which are
desirable make very difficult in machining of these cera-
mic materials.91 Green ceramic machining (GCM) has
been investigated as an alternative method for the mold-
free fabrication of complex-shaped ceramics. Machining
of ceramics in the unfired state is called green ceramic
machining. Recent advancement of CNC machining
technology makes GCM a potential alternative for the
rapid fabrication of ceramics.
In any machining process, a wear-resistant cutting
edge separates material from the workpiece because of
the velocity of the cutting tool edge relative to the work-
piece. When cutting metals, intense heat causes plastic
deformation, producing chips or a curl of material.
Green ceramic is different; it is machined by a process of
fracturing the material rather than a plastic deformation.
Fig. 9. (a) Influence of ratio of monomers on flexural strength of
green body. (b) Influence of ratio of monomers on flexural strength
of sintered body. (After Yu et al.90 with kind permission of
Springer Science + Business Media.).
The cutting edge crushes the ceramic just ahead of the
tool edge as it moves through the material. This forms
small particles, resulting in ceramic powder as an end
product rather than chips or a curl, as when cutting
metal. The ceramic cutting process does not generate
high temperatures. Attention must be paid to the avoid-
ance of chipping at the edge of a workpiece and develop-
ment of internal cracking caused by compressive stresses.
Coolants or compressed air is needed to wash away the
swarf. When cutting green ceramic, most tool wear is
caused by the abrasive nature of the ceramic particles
rather than by material temperature or cutting speed.
This places emphasis on selecting the most abrasion-
resistant tool surface material, specifically, diamond.
Shrinkage and warping of the ceramic part occurring
during its sintering does not allow achieving tight
918 International Journal of Applied Ceramic Technology—Kandi, Thallapalli, and Chilakalapalli Vol. 12, No. 5, 2015

Laser-assisted machining is a new and innovative

240 Solid loading=40 wt% RM=15 62
way of machining hard-to-wear materials, which are dif-
ficult to machine using conventional methods. The
220 60
description of LAM process is shown in Fig. 11. LAM
Flexural strength (MPa)

200 58
combines laser technology with traditional machining

180
160
140
12020 25 30 35 40 45
Monomer content (%)
Fig. 10. Influence of ratio of monomers on flexural strength and
porosity of sintered body. (After Yu et al.84 with kind permission
of Springer Science + Business Media.).
dimensional tolerances and high quality surface finish in
the presintered state.
Green ceramic machining is performed whenever
possible as the machining of ceramics after firing is very
costly. GCM offers several distinct advantages compared
with other technologies currently used for the fabrication
of net shape ceramics in terms of the cost-effectiveness
and surface finishing.92
Direct laser machining has also been studied as a
means of shaping hard materials. However, it involves
melting or evaporating the material, which can cause sur-
face cracks and undesirable changes to the surface micro-
structure.93 For machining ceramic materials, laser-
assisted machining (LAM) has recently been considered
as an alternative process.94 Residual stresses and micro-
cracks may form at the cut edge as a result of the shrink-
age of the solidified molten material. Some of the
machining processes that are compared with respect to
the parameters influencing the economy are shown in
Table VI.
Porosity (%)
methods such as turning and milling. Laser is used as a
56 heat source with the beam focussed on the unmachined
section of the workpiece directly in front of the cutting
54 tool. The addition of heat softens the surface layer of the
material, so that ductile deformation rather than brittle
52 deformation occurs during cutting.93 LAM’s most
important advantage is its ability to produce much better
50 55 60 50 workpiece surface quality than the conventional machin-
ing, together with larger material removal rates and mod-
erate tool wear.96
To machine tough ceramics such as silicon nitride,
diamond tools are typically used. Ductile machining of
silicon nitride is possible at higher speeds, but with an
increase in the force components above a speed of
250 m/min using polycrystalline diamond tools. As the
depth of cut increases, the machining forces also increase
and there is a maximum value of negative rake angle for
the tool above, which the machining changes from duc-
tile to brittle.97 Figure 12 shows the chip formation pro-
cess in LAM with each chip segment shown to contain
multiple cracks.98
The SEM image shown in Fig. 13 suggests that
LAM does not change the microstructure of the bulk
silicon nitride workpiece beneath the thin-smeared
layer. No microcracks were found on the smeared sur-
face produced by the plastic flow of the softened glass
phase and the redistribution of Si3N4 grains on the sur-
face. Promising experimental results are achieved in
LAM of silicon nitride experiments, in terms of long
tool life, good surface finish, thermal damage-free sur-
face, excellent subsurface integrity, moderate compres-
sive residual stress, and preservation of the silicon
nitride microstructure.99

Table VI. Comparison of Different Machining Processes Influencing Economy (After Samant and Dahotre95
with permission. Copyright Elsevier.)
Capital Toolings/ Power Removal
Machining process investment Fixtures requirements efficiency Tool wear
Conventional machining Low Low Low Very low Low
Ultrasonic machining Low Low Low High Medium
Electrochemical machining Very high Medium Medium Low Very low
Chemical machining Medium Low High Medium Very low
Electrical-discharge machining Medium High Low High High
Plasma arc machining Very low Low Very low Very low Very low
Laser machining Medium Low Very low Very high Very low
www.ceramics.org/ACT Development of Si3N4 Based Ceramic Radomes 919

Laser

Heat affected
zone

Chip

Tool

Ceramic
Workpiece

Rotation Fig. 13. SEM image of machined surface of a Si3N4 part pro-
Pyrometer duced by laser-assisted machining. (After Tian and Shin99.).
Fig. 11. Schematic description of laser-assisted machining.

weight and possess good green strength and may further

require finish machining operations.
Si3N4 radomes after sintering have high hardness
Ceramic and thus difficult to machine using conventional machin-
Workpiece ing processes. However, the finish machining with good
surface integrity is achievable using laser-assisted machin-
Chip ing process, and also, the process is very economic and
highly productive.

Rotation
Cutting tool
Fig. 12. Chip formation process in laser-assisted machining of
Si3N4.
Conclusions
After a thorough review, it is observed that: The
most desirable shape of airborne radomes is tangent
ogive with bluffness ratio of about 0.1. This shape pro-
vides minimum aerodynamic drag with low drag pres-
sure. Alumina (Al2O3) and yttria (Y2O3) are added to
Si3N4 materials in the gelcasting of ceramic radomes to
attain excellent mechanical and electronic properties at
high sintering time and temperature. These ceramics will
have stability in reductive atmosphere, and up on cool-
ing, the liquid phase crystallizes to an yttrium–aluminum
garnet phase.
Gelcasting is envisaged as the best near-net shape
fabrication process for manufacturing ceramic radomes
to the close tolerances. Such gelcast radomes are light in
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