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PART

I
I N T R OD UC TION:
HISTORY, RAW MATERIALS,
CERAMIC POWDER
CHARACTERIZATION

Many options are to be considered in organizing a book


on the fundamentals of ceramic powder processing. One
could organize a book along phenomenological lines (e.g.,
similar thermodynamics and reaction or diffusion kinet-
ics) or along material classifications lines (e.g., oxides,
carbides, and nitrides) or along material properties lines
(e.g., structural ceramics and electronic ceramics). After
considering the many possibilities, this book has been or-
ganized as if the reader were following a ceramic process
in a factory from powder to final finished piece. Ceramic
powder processing can take two traditional routes: one is
a wet powder processing route, where the powder is mixed
in the liquid and cast into the green body before firing;
the second is a dry ceramic powder processing route, which
consists of pressing the dry powder (with binder) into the
green body and then firing. Both of these processing routes
are shown in the Figure 1.1. This is the flow sheet for
the computer controlled tile making facility for the ' INAX
Corporation in Japan. Here they use these two routes, a
wet paste-extrusion route and a dry-pressing route, to
make ceramic tiles. These processing routes are also used
for modern ceramics such as tiles for the space shuttle's
surface and electronic BaTiO3 capacitors.
In this figure one sees all the steps that go into making
ceramics, starting with grinding the ceramic powders to
develop a very fine particle-size distribution (the grinding
circuits contain classification and recycle loops). This is
2 Part I Introduction

followed by putting the ceramic powder into liquid form, adding differ-
ent additives to adsorb to the particle surface and prevent coagulation
of the particles, as well as to adjust the rheology of the paste and
provide a binder of the particles after consolidation. The paste is then
dewatered to the best consistency for extrusion into the desired shape.
The resulting green bodies are dried very slowly, then subject to binder
burn-out treatment at higher temperatures followed by sintering. Dur-
ing sintering, pores are removed from the ceramic body, leaving behind
a fully dense piece which must then be finished in some way (e.g.,
applying a glaze or grinding to size). This constitutes the wet route as
shown in Figure 1.1. The outline of this book follows that sequence of
events very closely. As a result we have the following parts of this book:

F I G U R E 1.1 Ceramictile manufacturingprocess. Photo courtesyof Inax Corp., Japan.


Part I Introduction 3

Part I. Introduction: History, Raw Materials, Ceramic Powder


Characterization
Part II. Ceramic Powder Synthesis
Part III. Ceramic Paste Formation: Mise-en Pdte
Part IV. Green Body Formation: Mise-en Forme
Part V. Presintering Heat Treatments of Drying and Binder
Burnout
Part VI. Sintering and Finishing

The parts are further broken down into chapters discussing the
chemical, physical, and engineering fundamentals of each step of
the process.
The other route for ceramic manufacturing, starting with dry
powders and pressing them with a polymer or binder, is discussed
in this book in the different sections. This route will have in common
with the wet processing methods the steps of powder synthesis and
ceramic green body formation, binder burn-out, sintering, and fin-
ishing; thus, the reader interested in the dry powder processing
route can follow this processing sequence by stepping over various
materials which are not of interest. For the students particularly
interested in ceramic part manufacture, Part II of this book, discuss-
ing ceramic powder synthesis, would be of less interest. As a result
the student can start with the part three after reading the introduc-
tory chapters in Part I on raw materials and ceramic powder charac-
terization.
Each chapter is broken into sections with the first section always
stating the objectives of the chapter, and the last section always
providing a summary of the chapter. In the text, problems are worked
to elucidate the points discussed. Finally at the end of each chapter
there are unworked problems that the students can do for homework.
The book attempts to provide a large list of references for specific
concepts and ideas presented elsewhere, and we hope that the reader
will refer to these references for the derivation of specific equations
not presented. This book is highly mathematical in comparison with
other texts in the field, because this field should be much more
quantitative than heretofore presented. With these mathematics,
the field of ceramic powder processing can become more quantitative
in the future.
4 Part I Introduction

1.1 G E N E R A L C O N C E P T S OF C E R A M I C
POWDER PROCESSING

Several general ideas are associated with ceramic powder processing.


These general ideas have been generated after many years of research
and have resulted in a philosophy of ceramic powder processing.
The first idea is that uniformity in the microstructure of a single
phase ceramic is better for electrical and mechanical properties. This
idea is based on the Griffith fracture theory for ceramics, where the
strength of the ceramic is related to the largest flaw size. With a bigger
flaw size, weaker single phase ceramics result. Uniformity is also im-
portant for electrical ceramics. For example, the final grain size distri-
bution of BaTiO3 should be uniform to have the highest dielectric con-
stant for ceramic capacitors or the highest piezoelectric coupling
constants for actuators. In the case of the capacitor, the grains should
be uniformly small; and in the case of the actuator, they should be
uniformly large to achieve the orthorhombic crystal structure necessary
for piezoelectricity, which is prevented for grains less than 1 micron
in size for pure BaTiQ. The idea of uniformity remains for both large
and small grains in the case of electrical properties. This is sometimes
difficult when cannibalistic grain growth occurs during sintering, lead-
ing to a bimodal grain size distribution. For this reason, dopants are
used to prevent cannibalistic grain growth.
Another idea is that the microstructural inhomogeneities that occur
in casting a green body remain (or even get larger) during drying, binder
burn-out, and sintering. Therefore, to obtain the best uniformity the
casting process must be performed very carefully with suspensions
that contain no bubbles or large pieces of polymers. In addition, the
uniformity produced in the green body should not be destroyed by rough
handling. In the case of drying and binder burn-out, huge volumes of
gas, many thousands of times that of the green body itself, must leave
the green body. This process puts tensile stress on the green body which
can cause cracks. To prevent these cracks, drying and binder burn-
out conditions which are very slow are desirable. Uniformity is also
extended from the green body casting down to the ceramic suspension
utilized for casting. In this case uniformity of the particles used is
important because larger and smaller particles segregate into different
parts of the mold during casting of monophase ceramics, leading to
1.1 General Concepts of Ceramic Powder Processing 5

nonuniformity. This is the same reason why stable colloidal suspensions


are used for casting to prevent packing inhomogeneities caused by
aggregates. With composite ceramics which consist of two or more
different phases, uniform mixing in the suspension is also important.
This may be impossible if the two powders utilized have either different
densities or different particle-size distributions or both. For this reason,
the suspension is often flocculated with polymers so that the well-mixed
nature of a suspension is preserved in the flocs..These flocs, with their
inhomogeneous packing of particles, are then broken into homogeneous
green bodies by pressing at high pressure.
The last general concept of ceramic powder processing is that smaller
powders sinter to give smaller grains that give a stronger ceramic piece.
This idea is again based on the Griffith fracture theory for ceramics,
where the strength of the ceramic is related to the largest flaw size.
Assuming homogeneity, a smaller grain size will result in a smaller
flaw size, leading to a stronger ceramic. The sintering times tl and t2
for two powders with the same chemistry but different particles sizes
rl and r2 is given by Herring's scaling law [1]:

t2 = [r2/rl]ntl
where n is a constant depending on the sintering mechanism. In the
case of volume diffusion, n = 3. From the Herring scaling law, we see
that, as the mean particle size is decreased, the time needed to sinter
a ceramic piece is decreased.
These general concepts will play an important role in the selection
of a process for the manufacture of a particular ceramic part and as a
result these general concepts will be encountered again and again
throughout this book.

Reference
1. Herring, C., J. Appl. Phys. 21, 301 (1950).

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