Advanced Ceramics

Advanced Ceramics 4th year Lecture notes
Dr. Saad B. H. Farid 2014
Course 1: Functional and Engineering Ceramics
Course 2: Bio-Ceramics
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Insulating// Thermal Conductive Ceramics

Semi-conductive Ceramics
Piezoelectric Ceramics
Dielectric Ceramics
Magnetic Ceramics
Opto-electro-ceramics
Strength Ceramics
High-Temperature High-Strength
Porous Ceramics for Filtration
Ceramic Bearing
Cutting Tools
Ceramic Materials for Energy Systems
Ceramics for Biomedical Applications
Ceramic-Matrix Composites
Introduction to Bio-Ceramics
Ceramics
Alumina and Zirconia in Surgical Implants
Bioactive Glasses - Materials
Bioactive Glasses - Clinical Applications
Glass-Ceramic - Clinical Applications
Machinable and Phosphate Glass-Ceramics
Glass
Hydroxyapatite Coatings
Porous Hydroxyapatite
Pyrolytic Carbon Coatings
Bioceramic Composites
Calcium Phosphate Cements
Radiotherapy Glasses
Dental Glass-Ceramics
1. Insulating Ceramics/High Thermal Conductive Ceramics

Materials for PKG
Because of its high thermal conductivity, high mechanical strength, good insulation characteristics, moderate
dielectric properties and high chemical durability, alumina (HTCC: high
high-temperature
temperature co-fired
co
ceramics) is the most
popular ceramics material for semiconductor packages.
However, for power devices like power amplifier for base station or for satellites, higher
hig
thermal conductivity
material is required to dissipate the heat generated in the devices. To meet this requirement, aluminum nitride (AlN),
(
which has high thermal conductivity (TC) and a low thermal expansion coefficient comparable to that of Si, has been
b
adopted for packages requiring high thermal dissipation.
Another market trend, toward higher power, higher working frequencies, and lower power consumption, requires
reduction of the resistivity of conductors in co
co-fired packages. To meet this requirement,
ent, glass ceramics (LTCC: lowlow
temperature co-fired
fired ceramics) with silver or copper conductors have been developed.
New materials have been developed such that a novel AlN that can co-fired
fired at low temperature to reduce cost.
The second is a novel LTCC that has a high thermal coefficient of expansion. The third is also a novel LTCC that has
low permittivity and low loss tangent at high frequency.
Process Flow
Figure 1 shows the process flow for a co
co-fired multilayer ceramic package. There are many steps to produce a
multilayer package; however, there are only a few differences among different materials. Of course, material
composition, metallize composition and process condition is different for each. Among these steps, metallizing is an
especially critical technology for package production.
Aluminum Nitride AlN: Material Properties
AlN has a characteristic dielectric dispersion at high frequencies. Figure 2 shows the frequency dependence of
the dielectric loss (tan ) of AN75W and AN242. The dielectric loss of AlN shows a maximum at a few gigahertz.
This phenomenon is due to the piezoelectricity
ectricity of AlN, and the peak frequency inversely depends on crystallite size.
As the crystallite size of AN75W is smaller than that of AN242, the peak (dispersion) frequency of AN75W is
correspondingly higher.
Expansion
LTCC with High Thermal Coefficient of Expan
Due to the ever-increasing
increasing I/O counts for IC devices, packaging trends have been changing to
surface mountable area array second-level
level interconnection, namely ball grid array (BGA
BGA) and chip
scale package (CSP).
BGA

The motivation for these types of second-level mounting
is described as follows:
1. Higher wiring density: smaller packages, thinner

packages, lighter packages,
2. Higher performance: electrical performance, thermal
performance, higher I/O counts,
3. Lower cost.
A surface mounting technology (SMT) package, such as
BGA, has low height interconnection between the substrate
and the printed wiring board PWB (also called printed circuit
board PCB).
When we have a big difference of TCE between the
substrate and the PWB, BGA and CSP packages receive
more severe shear strain, damaging the reliability of solder
joints, compared with Pin grid array PGA. This shear strain is
a big problem, since alumina ceramics has TCE of 7 ppm/C
while the TCE of a typical PWB is 1216 ppm/C.
The observations suggest that the reliability largely
depends on the TCE mismatch between the substrate and the
potting compound.
Figure 1: Process flow for multilayer ceramic

package fabrication.
A new ceramics is developed with TCE of 13 ppm/C,

which is in the range of PWBs (1216 ppm/C) and that of
the potting compounds (1030 ppm/C).
Hint: it is done by incorporating glass in a composite.
The dielectric constant is 5.3 at 1 MHz, which is lower
than 9.8 of alumina. The Youngs modulus is 110 GPa,
approximately one-third that of alumina. Also, copper
conductor is co-firable.
It is found that the equivalent plastic strain generated by
the TCE mismatch among Si-die, substrate, potting
compound and PWB drastically decreases as TCE of the
substrate increases from 11.5 to 13 ppm/C.
Figure 2: Frequency dependence of dielectric

loss of AlN.
LTCC with Low Permittivity and Low Loss Tangent at High Frequency
The ceramic package used for microwave applications requires following properties;
(a) Lower dielectric constant and lower loss tangent in the radio frequency range;
(b) Lower resistivity conductor;
(c) Thermal expansion coefficient of the ceramic material close to that of semiconductor chips;
(d) High reliabilityof hermeticity (airtight).
A new LTCC material was designed to be able to sinter at less than 1000C because of co-firing with copper
conductor. The LTCC is composed of lead-free, SiO2Al2O3MgOZnOB2O3 system glass and ceramic fillers. In
order to satisfy electrical and thermal properties, the amount of crystalline phases precipitated after sintering is
adjusted.
The coefficient of thermal expansion is 7.5 ppm/C in the range of 40300C. This value is close to that of GaAs
chips that are mainly used for microwave applications. Thermal conductivity and flexural strength and volume
resistivity are as good as conventional LTCC material. The dielectric constant is 6.0, which is lower than that of
alumina in the range of 260 GHz. The loss tangent increases as frequency increases and close to that of alumina,
which is good for microwave applications.
2

Copper metallization
Copper was used for metallization material because of excellent migration resistance. It is important for co-firing
process to match the shrinkage behavior of copper metallization to that of LTCC material. Since the shrinkage of
copper starts at lower temperature than that of LTCC material, glass and ceramic fillers are added to copper paste to
control the shrinkage behavior of copper metallization. After co-firing, copper metallization is plated LTCC material
with nickelgold or coppergold.
Squares are the unit-less dimension of length
Adhesion strength of the metallization was measured,
divided by width. RH: Relative Humidity
and no change was observed after 1000 h aging at 150C.
Sheet resistance of the metallization was 2.5m/ (12m thickness), where and no increase was observed after
1000 h aging at 150C. The insulation resistance between lines separated by 100m space was more than 1012 after
1000 h of High Humidity Biased Test HHBT (semiconductor component reliability test) (85C, 85% RH, 5.5 V).
2. Semiconductive Ceramics
a- PTC Thermistors
Barium titanate (BaTiO3) is a ferroelectric material with a high dielectric constant and high insulation resistance.
Therefore, it has been widely used in the electrical industry for ceramic capacitors since its discovery in 1943. The
insulating BaTiO3 ceramic is converted into a semiconductor by adding a small amount of rare earth metal oxide such
as Sm2O3, CeO2, Y2O3, and La2O3. In 1955, unusual temperature dependence of resistance above the Curie
temperature of semiconductive BaTiO3 ceramics was discovered.
The resistance of this semiconductor called the positive temperature
coefficient (PTC) thermistor drastically increases above the Curie
temperature (TC), up to the temperature (Tn) where the resistance reaches
its maximum value. The characterized temperature is divided into three
regions (I, II, and III in Figure 4) according to the resistance behavior.
Conduction Mechanisms
The conduction mechanisms in the regions IIII are explained as
follows. In the temperature region I(T < TC), the resistivity of PTC
thermistor is in the range of 10106 cm. To produce semiconductive
BaTiO3, a small amount of rare earth metal ions (e.g. Sm3+ or La3+) are
substituted at the Ba2+ site, or Nb5+ and Ta5+ ions are substituted at the Ti4+
site. These ions provide conductive electrons.
Figure 3: Characterized temperature

regions of PTC ceramics
In the region II above the Curie temperature, resistance across the grain boundary increases exponentially with
increasing temperature. The increase of resistance corresponds to the decrease of spontaneous polarization (Ps) of
BaTiO3 due to the phase transition from the ferroelectric tetragonal phase to the paraelectric cubic phase. The gradual
decrease of Ps and dielectric constant cause the potential barrier height to recover. This recovery results in an increase
of resistance in region II.
In the temperature region III (T > Tn), the electrons that overcome the double Schottky barrier increase with
temperature, and resistance decreases from maximum resistance.
Manufacturing Process
Additives and their effects on PTC characteristics are
listed in Table 1. The transition temperature TC can be
lowered or elevated from its original value (120C) by
substitution of Sr2+ and Pb2+ at the Ba2+ site.
BaCO3, SrCO3, Pb3O4, TiO2 and donor dopant (e.g.
La2O3, Sm2O3, Y2O3 and Nb2O5) are used as starting
materials. Manufacturing processes of PTC thermistor are
almost the same as those in the electronic ceramics industry.
3
To control the resistance and the temperature coefficient

within the exact range, much attention is paid to the firing
temperature and ensuing cooling rate. The impurity of rare
materials and contamination in manufacturing process must be
decreased, because these increase the resistance at room
temperature. In particular, Fe and Al strongly affect the resistivity
of PTC thermistor.
Non-precious metal electrodes such as Ni, Zn, and Al provide
ohmic contact with PTC thermistor, which is n-type
semiconductor ceramics. InGa alloy also makes ohmic contact,
and is used for experimental samples.
Applications
Table 2 shows three basic functions and applications of
PTC. PTC thermistors are used in a lot of electric products, such
as color televisions, refrigerators, hot-wind heaters, and personal
computers.
b- NTC Thermistors
The negative temperature coefficient (NTC) thermistors are
semiconductive materials whose resistance decreases with
increasing temperature as shown in Figure 4 with other
thermistors.
R = A exp(B/T), B = E/k, where A is a constant, B a thermistor
constant, E the activation energy, and k Boltzmanns constant.
Conduction Mechanism
NTC thermistor usually consists of transition metals (Cu,
Fe, Co, Ni, etc.) spinel manganites. The conductivity is due to
the transfer of electrons between Mn3+ and Mn4+ ions. The
resistance and thermistor constant is dependent on the
composition, purity, cation distribution, and crystal structures.
Mn3O4, NiO, Co2O3, and Fe2O3 are used as starting
materials. NTC thermistors are produced by the general method
of the manufacturing of electroceramics. Precious metals such as Figure 4 Temperature dependence of different types
of thermistors in contrast to a platinum
Ag, Pd, and Pt are used for electrodes of NTC thermistor, which
is mainly p-type semiconductor ceramics.
Applications
NTC thermistors are used as temperature compensation, temperature sensing, and surge current suppression
devices. All of these applications are based on the resistancetemperature characteristics of NTC thermistors.
Although various thermistor constant B and resistivity are required for many applications, these values are
obtained within certain limits, because the thermistor constant B is dependent on the resistivity.
Ceramic Varistors
Metal oxide varistors are ceramic semiconductive devices having highly nonlinear currentvoltage
characteristics, as shown in Figure 5, expressed as I = (V/C).
4
is the nonlinear exponent, C the constant corresponding to the

resistance, and V1 and V2 are the voltages at the currents of I1 and I2,
respectively. C is convenient1y given by Vc called varistor voltage,
that is, a voltage per unit length (V/mm) when 1 mA/cm2 of current
flows through the body. Thus, the ceramic varistor is characterized by
the non-linear exponent and varistor voltage Vc.
Two types of ceramic varistors are manufactured. Zinc oxide
based ceramic varistors were developed in 1970. They exhibit a high
non-linearity on voltagecurrent characteristics. Their value is in the
range of 4050, and the Vc adjustable to values in the range from 50
to 250 V/mm. Strontium titanate based varistors were developed in
1980. The feature of these varistors is their larger electrostatic
capacitance compared with ZnO varistors. The SrTiO3 ceramics are
essentially dielectrics with a die1ectric constant of 320, which is much
Figure 5 Typical VI characteristic of ceramic
higher than that of ZnO.
varistor
The effect of additives on varistor properties of
ZnO varistors are listed in Table 3. The varistor
voltage Vc is dependent on the number of grain
boundaries between a couple of electrodes, because
the varistor voltage across a single grain boundary is
constant value (3V) at each boundary. To obtain
the varistors with the various voltages Vc, the grain
size are controlled by firing temperature or
additives, such as B and Sb.
Strontium titanate based varistors are manufactured by firing in a reducing atmosphere and re-oxidized on only
grain boundary, like a boundary-layered ceramic capacitor.
Applications
Metal oxide varistors are mainly used in circuits for protection
against inductive surges, very short spike noise, or power surges. They
result to protect circuit simply by inserting between surge entrance
line and ground lines shown in Figure 6. A varistor should be chosen
that have a varistor voltage Vc slightly higher than the signal voltage
applied to the load to be protected. The varistor is insulator in normal Figure 6 Typical application of ZnO varistor
operation where the applied voltage is lower than Vc.
as a transient protective device.
If a transient pulse, whose voltage is higher than Vc, is incident, the current through varistor rapidly increases,
resulting in a conducting shunt path for the incident pulse.
ZnO-based varistor have become popular because of the high non-linearity on voltagecurrent characteristics.
3. Piezoelectric Ceramics
Certain materials produce electric charges on their surfaces as a consequence of applying mechanical stress. The
induced charges are proportional to the mechanical stress. This is called the direct piezoelectric effect and was
discovered in quartz by Piere and Jacques Curie in 1880. Materials showing this phenomenon also conversely have a
geometric strain proportional to an applied electric field. This is the converse piezoelectric effect. The root of the
word piezo means pressure; hence the original meaning of the word piezoelectricity implied pressure
electricity.
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Piezoelectricity is extensively utilized in the fabrication of various devices such as transducers, actuators, surface
acoustic wave devices, frequency control and so on. In this chapter we describe the piezoelectric materials that are
used, and various potential applications of piezoelectric materials.
Piezoelectric Materials
This section summarizes the current status of piezoelectric materials: single-crystal materials, piezoceramics,
piezopolymers, piezocomposites and piezofilms.
i- Single Crystals
Although piezoelectric ceramics are widely used for a large number of applications, single-crystal materials
retain their utility, being essential for applications such as frequency stabilized oscillators and surface acoustic
devices. The most popular single-crystal piezoelectric materials are quartz, lithium niobate (LiNbO3), and lithium
tantalate (LiTaO3). The single crystals are anisotropic, exhibiting different material properties depending on the cut of
the materials and the direction of bulk or surface wave propagation. Quartz has a cut with a zero temperature
coefficient.
ii- Polycrystalline Materials
Barium titanate (BaTiO3) is one of the most thoroughly studied and most widely used piezoelectric materials.
Just below the Curie temperature (120C), the vector of the spontaneous polarization points in the [001] direction
(tetragonal phase), below 5C it reorients in the [011] (orthrhombic phase) and below 90C in the [111] direction
(rhombohedral phase). The dielectric and piezoelectric properties of ferroelectric ceramic BaTiO3 can be affected by
its own stoichiometry, microstructure, and by dopants entering onto the A or B site in solid solution. Modified
ceramic BaTiO3 with dopants such as Pb or Ca ions have been developed to stabilize the tetragonal phase over a
wider temperature range and are used as commercial piezoelectric materials. The initial application was for
Langevin-type piezoelectric vibrators. Piezoelectric Pb(Ti,Zr)O3 solid solutions (PZT) ceramics have been widely
used because of their superior piezoelectric properties.
iii- Polymers
Polyvinylidene difluoride, PVDF or PVF2, is piezoelectric when stretched during fabrication. Thin sheets of the
cast polymer are then drawn and stretched in the plane of the sheet, in at least one direction, and frequently also in the
perpendicular direction, to transform the material to its microscopically polar phase. Crystallization from the melt
forms the non-polar -phase, which can be converted into the polar -phase by a uniaxial or biaxial drawing
operation; the resulting dipoles are then reoriented through electric poling.
iv- Composites
Piezo-composites, comprised of a piezoelectric ceramic and a polymer phase, are promising materials because of
their excellent and readily tailored properties. A piezo-composite, such as the PZTrod/polymer composite is a most
promising candidate. The advantages of this composite are high coupling factors, low acoustic impedance, good
matching to water or human tissue, mechanical flexibility, broad bandwidth, and low mechanical quality factor.
Piezoelectric composite materials are made by forming a composite structure, that is, by replacing some of the heavy,
stiff ceramic with a light, soft polymer. Piezoelectric composite materials are especially useful for underwater sonar
and medical diagnostic ultrasonic transducer applications.
v- Thin Films
Both zinc oxide (ZnO) and aluminum nitride (AlN) are simple binary compounds with a Wurtzite-type
structure(hexagonal crystal system), which can be sputter-deposited as a c-axis oriented thin film on a variety of
substrates. ZnO has large piezoelectric coupling and thin films of this material are widely used in bulk acoustic and
surface acoustic wave devices. The fabrication of highly oriented (along the c-axis) ZnO films have been studied and
developed extensively. The performance of ZnO devices is limited, however, due to their low piezoelectric coupling
(2030%). PZT thin films are expected to exhibit higher piezoelectric properties. At present the growth of PZT thin
films is being carried out for use in microtransducers and microactuators.
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Application:
a- Pressure Sensors/Accelerometers/Gyroscopes
One of the very basic applications of piezoelectric ceramics is a gas igniter. The very high voltage generated in a
piezoelectric ceramic under applied mechanical stress can cause sparking and ignite the gas. There are two means to
apply the mechanical force, either by a rapid, pulsed application or by a more gradual, continuous increase.
increase
Piezoelectric ceramics can be employed as stress sensors and acceleration sensors, because of the direct
piezoelectric effect. A three-dimensional
dimensional (3D) stress sensor can be designed by combining an appropriate number of
quartz crystal plates (extensional and shear types), the multilayer device can detect 3D stresses.
b- Piezoelectric Vibrators/Ultrasonic Transducers
Piezoelectric Resonance
When an electric field is applied to a piezoelectric material, deformation ((L)
L) or strain (L/L)
(
arises. When the
field
ield is alternating, mechanical vibration is caused, and if the drive frequency is adjusted to a mechanical resonance
frequency of the device, large resonating strain is generated. This phenomenon can be understood as a strain
magnification due to accumulating
ting input energy, and is called piezoelectric resonance. Piezoelectric resonance is very
useful for realizing energy trap devices, actuators, etc.
Electromechanical Coupling Factor
Factor,, k: corresponds to the rate of electromechanical transduction.
k2 = (stored
ed mechanical energy/input electrical energy)
k2 = (stored electrical energy/input mechanical energy) = d2/0 s
The general processes for calculating the electromechanical parameters (k31, d31, sE11, and X33) are:
1. The sound velocity in the specimen is obtained from the resonance frequency fR
2. Knowing the density , the elastic compliance sE11 can be calculated.
3. The electromechanical coupling factor k31 is calculated from the value and the antiresonance frequency fA
4. Knowing the permittivity X33, the d31 is calculated
Piezoelectric Vibrators
In the use of mechanical vibration devices such as filters or oscillators,
the size and shape of a device are very important, and both the vibrational
mode and the ceramic
ic material must be considered.
Figure 7 Piezoelectric buzzer.
The resonance frequency of the bending mode in a centimeter

centimeter-size
size sample ranges from 100 to 1000 Hz, which is
much lower than that of the thickness mode (1
(100 kHz). For these vibrator applications, the piezoceramic should have
a high mechanical quality factor (QM) rather than a large piezoelectric coefficient d; that is, hard piezoelectric
ceramics are preferable. For speakers or buzzers, audible by humans, ddevices
evices with a rather low resonance frequency
are used (kilohertz range).
c- Ultrasonic Transducers
Ultrasonic waves are now used in various fields. The sound source is made from piezoelectric ceramics as well as
magnetostrictive materials. Piezoceramics aare
re generally superior in efficiency and in size to magnetostrictive
materials. In particular, hard piezoelectric materials with a high QM are preferable. A liquid medium is usually used
for sound energy transfer. Typical applications are uultrasonic washers,, ultrasonic microphones for short-distance
short
remote control and underwater detection, such as sonar and fish finding, and non
non-destructive
destructive testing. Ultrasonic
scanning detectors are useful in medical electronics for clinical applications ranging from diagnosis
diagnos to therapy and
surgery.
One of the most important applications is based on ultrasonic echo field. Ultrasonic transducers convert electrical
energy into mechanical form when generating an acoustic pulse and convert mechanical energy into an electrical
signal
gnal when detecting its echo. The transmitted waves propagate into a body and echoes are generated which travel
back to be received by the same transducer. These echoes vary in intensity according to the type of tissue or body
7

structure, thereby creating images.
mages. An ultrasonic image represents the mechanical properties of the tissue, such as
density and elasticity. We can recognize anatomical structures in an ultrasonic image since the organ boundaries and
fluid-to-tissue
tissue interfaces are easily distinguished.
The ultrasonic imaging process can also be done in real time.
This means we can follow rapidly moving structures such as the heart
without motion distortion. In addition, ultrasound is one of the safest
diagnostic imaging techniques. It does not use ion
ionizing radiation like
X-rays,
rays, thus, it is routinely used for fetal and obstetrical imaging.
Useful areas for ultrasonic imaging include cardiac structures, the
vascular systems, the fetus, and abdominal organs such as liver and
kidney. In brief, it is possible
ble to see inside the human body without
breaking the skin by using a beam of ultrasound.
Figure 8 Basic transducer geometry for
d- Resonators/Filters
acoustic imaging applications.
When a piezoelectric body vibrates at its resonant frequency, it absorbs considerably more energy than at other
frequencies resulting in a dramatic decrease in the impedance. This phenomenon enables piezoelectric materials to be
used as a wave filter. A filter
lter is required to pass a certain selected frequency band or to block a given band. The band
width of a filter fabricated from a piezoelectric material is determined by the square of the coupling coefficient k, that
is, it is nearly proportional to k2. Quartz
artz crystals with a very low k value of about 0.1 can pass very narrow frequency
bands of approximately 1% of the center resonance frequency. On the other hand, PZT ceramics with a planar
coupling coefficient of about 0.5 can easily pass a band of 10% of the center resonance frequency. The sharpness of
the passband is dependent on the mechanical quality factor QM of the materials. Quartz also has a very high QM of
about 106, which results in a sharp cut-off
off to the passband and a well
well-defined
defined oscillation frequency.
fr
e- Surface Acoustic Wave Devices
A surface acoustic wave (SAW), also called a Rayleigh wave, is essentially a coupling between longitudinal and
shear waves. The energy carried by the SAW is confined near the surface. An associated electrostatic wave exists for
a SAW on a piezoelectric substrate, which allows electro
electro-acoustic coupling via a transducer.
There is a very broad range of commercial system applications which include front-end
front
and intermediate
frequency (IF) filters, community antenna television (CATV) and video cassette recorder (VCR) components,
synthesizers, analyzers and navigators.
f- Piezoelectric Transformers
When input and output terminals are fabricated on a piezo device and input/output voltage is changed through the
vibration energy transfer, the device is called a piezoelectric transformer. Piezoelectric transformers were used in
color
lor TVs because of their compact size in comparison with the conventional electromagnetic coil-type
coil
transformers.
Recent lap-top
top computers with a liquid crystal display require a very thin, no electromagnetic-noise
electromagnetic
transformer to
start the glow of a fluorescent back-lamp.
g- Piezoelectric Actuators
Piezoelectric and electrostrictive devices have become key components in smart actuator systems such as
precision positioners, miniature ultrasonic motors and adaptive mechanical dampers.
Piezoelectric actuators are forming a new field between electronic and structural ceramics. Application fields are
classified into three categories: positioners, motors and vibration suppressors.
The manufacturing precision of optical instruments such as lasers and cameras, and the positioning accuracy for
fabricating semiconductor chips, which must be adjusted using solid
solid-state
state actuators, are generally on the order of
0.1m. Regarding conventional electromagnetic motors, tiny motors smaller than 1 cm3 are often required in office
offic
or factory automation equipment and are rather difficult to produce with sufficient energy efficiency. Ultrasonic
motors whose efficiency is insensitive to size are considered superior in the mini
mini-motor
motor area. Vibration suppression in
space structures and military vehicles using piezoelectric actuators is another promising field of application.
8

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Advanced Ceramics

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Advanced Ceramics 4th year Lecture notes

Dr. Saad B. H. Farid 2014

Course 1: Functional and Engineering Ceramics

Insulating// Thermal Conductive Ceramics

1. Insulating Ceramics/High Thermal Conductive Ceramics