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Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for
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DOI: 10.14723/tmrsj.35.473

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 Transactions of the Materials Research Society ofJapan 20th Anniversary Special Issue 47-57 (2012)
I'R_e_v-ie_w_p_a_p-er---,1

Ceramic Powders for Advanced Ceramics:

What are Ideal Ceramic Powders for Advanced Ceramics?*

Shigeyuki Somiyal), Sridhar Komarneni 2 ) and Rustum Roi)

1) 3-7-19 Seijo, Setagaya, Tokyo 157-0066, Japan
2) Materials Research Institute, Materials Research Laboratory, The Pennsylvania State University, University
Park, 16802, U. S. A.
Fax: 81-3-3417-2866
*This article was originally for the J. Korean Ceramic Society and current version is slightly modified.

One of the most important factors for advanced ceramics preparation is nature of the powders.
There are many methods to prepare powders for ceramics, namely, mechanical, thermal
decomposition, precipitation, hydrolysis, hydrothermal, melt and quenching, etc. This is a
review of powder preparation for advanced ceramics. Characteristics of these methods are
described. And also ideal powder for advanced ceramics is described.
Key words: Hydrothermal process, Powder characteristics, Fine ceramic powders

1. Introduction @Grain size distribution

Powders play a key role in many fields such @Shape of grain
as ceramics, catalyst, medicines, food, etc. @Size of grain.
Many books and papers have reported powder Concerning 0. A. Whittmore, Jr. 12 l, University of
preparation; for examples, C. R. Vealell, A. Kato Washington,
and T. Yamaguchi 2 l, P. Vincenzini 3 l, D. Segal4 l, S.
CDSize ofpore
Saito 5 l, S. Shirasaki and A. Makishima 6 l, G.
Jimbo7l, R. J. Brook 8 l, S. Somiya, T. Hayashi, and (2) Shape of pore
K. Asaga 9 - 13 l, D. Ganguli and D. Chatterjee 14 l, @Distribution of pore.
and TIC Editorial Office 15 l. As for J. A. Pask 13 ) of University of California,
There are many scholars who mentioned Berkeley, California,
about important characteristics for ceramic CD Coagulation of grain
powders. D. L. Segal 16l mentioned the ideal @Grain size
powder for Advanced Ceramics as follows: and so on. Each scholar had mentioned several
CDSub-micron size important things for powders.
@Absence of particle aggregates
®Narrow size of distribution 2. Characteristics of powders 7 • 14 • 15 )
Characteristics of powders from gas phase
@High chemical purity.
are:
In addition,
CD High purity, less impurity
®High compositional homogeneity
(2) Easy to control crystallinity and crystal
®Low cost.
structure for single and polycrystal
For instance, alkoxide is good but it is
® Easy to form polycomponent coating
expensive. Low cost is better than high cost.
According to H. Kent Bowen M. I. T., U. S. A. 9 l, particle
important powder characteristics are: @ Able to produce uniform particle
CDNarrow particle distribution chemically
@Not aggromerated ® Able to produce polyphase coating particle
@As spherical as possible ® Able to make porous or dense particle
@Uniformity of chemical composition. (f) Able to make non-aggregate or aggregate
Rustum Roy of the Pennsylvania State particles with different porosity
University 10 l developed the sol-gel process in the @ Particle size is from A to nm.
time period 1949-5 6, which has been cited
formally and informally over 30,000 times for Concerning powders from liquid phase,
making fine, pure, powders of virtually any characteristics are as follows:
composition in ceramics. He mentioned CD Easy to control of components even if it is
CD Control of chemical composition for a small amount
@Grain size (2) Rate of formation of particle through
®Simplicity. liquid is lower than through gas phase.
Related to A. I. Aksay, University of Therefore easy to control of particle size,
Washington 11 l, distribution of particles, crystallinity,
uniformity of composition, etc.
CDPore distribution

47
48 Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for Advanced Ceramics?

® In some cases, able to make uniform size 3. Methods for producing fine ceramic powders
particle There are two big ways, so called break
@ Washing, filtration, removal of some down 14 • IS) and building up processes. 14J As for
chemicals, dry process, etc. are necessary m building up process, it is divided into 4 groups,
some cases. namely thermal decomposition, precipitation or
@ Many cases, dehydrated powder is hydrolysis, hydrothermal, melting and quenching,
aggregated etc.
(a) Break down process
@ Many cases, powder is spherical and
This is shown in Table 1.
flowing is good.
(b) Building up process
This section is divided into 4 sub-divisions and is
In the case of alkoxides
shown in Table 2. In ordinary case, raw
CD Purification is easy materials of advanced ceramics are produced by
@ Obtain high purity particles these methods.
® Characteristics of powder depend on mole
ratio of alkoxide: water, temperature of
reaction, time for ageing , } ~ '!',~~, ~e~?,~POOO~,~tion
; a Heating(evaporation)
@ Particle size and distribution are 0

b.'SP~Y'drYin~g,
dependent on temperature and time for ageing c. Flame spraying
, d. p~~ spray·illg
® In ordinary case, products are amorphous.
In the case of spray drying,
CD Easy to control of chemical composition
by concentration of solution.

Characteristics of ideal powder 18 l from our stand

point are shown below
CD Fine powder less than 1 flm
@ Soft or no agglomeration
® Narrow particle size distribution
@ Spherical morphology as much as possible
® Chemical compositions are controllable
@ Microstructure is controllable
(/) Uniformity is good
® Free flowing i.Microwave

® Fewer defects, dense particle ;k.

j. Ultrasonic
MiC~~~~~e+Uit;;;~nic
® Less stress 4jMeltingand rapid quenching

@ Reactivity and sinterability are good

@ Crystallinity is good
@ Process is easy to control
and so on.
tiX.cirothermal treat111ent
;'T'.lb,i~ 1'. 'Meth,?,~ fo~'Pr~dticing Fill'~ c~~c P'O~~~~ ~eCh'~~~~ Mitii~~ Hydrothermal alteration
:Origfial Data by M.Naito, N.Shinohara, K.Uematsu: Modified by s:sorniya .... liydl-oih~~al d~hydr~iio~- ·
HydJ:~t~~IIDai extract·i~~---
Hydrothermal reaction sintering
High-pressure roller mill
Hidrothermal s~terin,g
..... Ang;;rili···
'A.;;)'C)[~limill
.... Tumbling ball nril[ ..

~i&ot~~~~+ ~iii~o~ic ~·-

Hydrothermal+ microwave
Hydiothe~+ uitrasonic·..;. IDicrowave

4. What is Hydrothermal? 14 • 16 - 34 l
The term hydrothermal or
"hydrothermal synthesis" came from the earth
S. Somiya et al. Transactions of the Materials Research Society ofJapan 20th Anniversary Special Issue 47-57 (201 0) 49

sciences where it implies a region of high

temperature and water pressures, above 100 oC
(Table 3). Cement researchers, however, want
the temperature to be above 60°C rather than
100°C.
Processings of hydrothermal synthesis are
shown in Table 3 and major differences of
powders and processing between hydrothermal
and technologies for powder preparation are
shown in Table 4.
,:Table 4. Major Differences of Powders and Processing Between Hydrothermal
and Other Technologies for Powder Preparation 181

l. Powders are formed directly from solution.

2:-po:...;;der_s_ are ~Yd;~~s-, CrY~t~lli.n~, 0~ ~~rph~us .dependin~ ?n fhe"hY4r~th~rmal temperattire.
i Particle s~e-COOtrOited by hydrot'h~nna(te~erature. . ... ~ ~ ...
4. Particle shape controlled by starting materials.

6. Powders are highly reactive in sintering

7. In many cases, powders do not need calcination.
8. fu wy ;;ases, po~d~ d~ not•n~ a milling process.

Figure 2. Reaction vessel with a cold-cone seat

closure (Tem-Press). 35 l

• Tem-Press 35 l___ They are the best source for

research vessels of all kinds, including test
tube bombs and gas intensifiers for specialized
gases such as argon, hydrogen, oxygen,
ammonia, etc.
Autoclave Engineers 37 ) ---They make a
complete line of laboratory-scale valves,
tubing, collars, fittings for connections, etc.
and they also make very large autoclaves (1-3
m) for quartz and other chemical processes.
• Parr Instrument Co. 36 ) ___ They make simple,
low-pressure (1000 bars), low-temperature
(300°C) laboratory-scale autoclaves (50 m! to
1 L) for low-temperature reactions, including
vessels lined with Teflon.
Figure 1. Autoclave with flat plate closure.
(Morey, G. W., J. Am. Ceram. Soc., 36, 279, Each autoclave has limitation of pressure
1953.) and temperature. It is shown in Table 5 and
Figure 3. They are depended on materials of
For typical hydrothermal research we need autoclave, sealing methods, and duration of time
a high-temperature, high-pressure apparatus (Table 6, Figure 4). Japan has regulation for
called an autoclave or bomb. A great deal of high pressure gas experiments. Therefore safety
early experimental work was done using the is one of important points for operation of
Morey bomb 21 l and Tuttle-Roy test tube bomb autoclaves.
(made by Tern-Press), which are shown in Figure
1 and Figure 2 35 ). Hydrothermal synthesis 4.1 Starting materials 29 l
involves water both as a catalyst and occasionally For the hydrothermal experiments, the
as a component of solid phases in synthesis at starting materials are very important.
elevated temperatures (greater than lOOoC) and Requirements for the starting materials are
pressure (more than a few atmospheres). At CD Accurate composition,
present, one can get many kinds of autoclaves to @ As homogenous as possible,
cover different pressure-temperature ranges and @ As pure as possible of purity,
volumes. In the U. S., there are three @) As fine as possible,
companies: etc.
50 Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for Advanced Ceramics?

,Table 5, Limits of pressure and Temperature of Autoclaves carbonate without water, (e) natural minerals
After R.A. Laudise and J.W. and S.Somiya20 • and/or rocks, (f) pure metal powders, and so on.

Pressure 'Temp. 4.2 Heating Methods 29 l

(atm) (°C) There are two methods. One is internal
Pyrex (5mm inside diameter, 9mm outside diameter) 0.6 250
and the other is external heating system.
Quartz ( 5mm inside diameter, 9mm outside diameter), 0.6 300
External system is very common around the world.
Morey Type (Flat Plate Seal) 400 400
Internal heating system is able to pressurize up to
Welded Walker-Buebler 2000 480
Delt~Ri~g 2300 400
10 kb or 1.5 kb.
Bridgeman Seal 370 500
Modified Bridgeman Seal 3700 500 4.3 A Batch System or A Continuous System29 l
Cold Seal Test Tube Concerning operation, there are two ways.
Stellite 25 4000 800 One is a batch system and the other is a
10000 740 continuous system. In the ordinary case, batch
1100 systems are common. Some researchers like the
continuous systems.

4.4 Some Results in Different Categories

A. Hydrothermal Decomposition 38 J
Ilmenite (FeTi0 3) is a very stable mineral.
Extraction of titanium dioxide (Ti0 2) from such
ores has potential. Using l 0 M KOH or 10 M
NaOH mixed with ilmenite in a ratio of 5:3
(ilmenite: water) under reaction conditions of
500°C and 300 kg/cm 2, ilmenite was decomposed
completely after 63 h. If the ratio of ilmenite to
water is 5:4, under the same conditions, 39 h is
needed to decompose the ilmenite. Reactions
were as follows, in the case of KOH solution:
3FeTi0 3 + H 2 0 ---'> Fe 3 04 + 3Ti02 + H 2
Figure 3. P-T limits for stellite vessel, Catalog nTi0 2 + 2KOH ---'> K 2 0(Ti0 2)n + HzO, n
Information, Tempress Inc., State College, ~ 4 or 6.
Pennsylvania.
B. Hydrothermal Metal Oxidation 39 l
Table 6. Sealing methods 20J Zirconium metal powder (10-50 g) was
reacted with water to form Zr0 2 :
Flat plate closure(Morey)
Zr + 2H 20 (at 300°C) ---'> Zr02 + ZrHx
Cold-cone seat closure(Tuttle)
(400°C) ---> Zr0 2 + 2H2.
Delta and "D"ring closure
Modified Bridgeman closure
Gray Loc closure

Figure 4. Comparison for self- and pressure-

energized sealing systems applied to larger
autoclaves. (Modified Bridgman seal and
Gray-Loc seal) After J. Asahara, K. Nagai, and S.
Figure 5. TEM of zirconia powder by
Harada. 62 J
hydrothermal oxidation (1 00 MP a at 500oC for 3
There are 6 types of starting materials h).
which commonly used in experiments: (a) glasses,
(b) gels, (c) dry mixtures of oxides, (d) chemical At 300°C under 98 MPa, Zr0 2 and ZrHx appeared.
salts such as nitrates, sulphate, hydroxides, and At temperatures above 400 oC under 98 MP a,
S. Somiya et al. Transactions of the Materials Research Society ofJapan 20th Anniversary Special Issue47-57 (2010) 51

ZrHx disappeared and only Zr0 2 was formed. is one of the best ways to produce zirconia
Figure 5 and Figure 6 show Zr0 2 powders formed powders. The process, properties of the
by hydrothermal oxidation. powders, and microstructure of the sintered body
are shown in Table 8 and Figure 9, Figure 10, and
Figure 11.

Numinum
Figure 6. Schematic illustration of hydrothermal h;ydcoxi de seeds
oxidation of zirconia powder.

C. Hydrothermal Reactions 40 - 44 l
Hydrated zirconia was formed when ZrC14
solution was reacted with NH 4 0H. Then it was
washed with distilled water and dried for 48 h at
120oC. This starting material was placed into a
platinum or gold tube with various solutions
under lOO MPa at 300°C for 24 h (Figure 7).
The results are shown in Table 7.

D. Hydrothermal Precipitation or Hydrothermal

Hydrolysis
(1) Alumina 45 l
One of the industrial applications of
hydrothermal precipitation is ordinary alumina
production. The Bayer process is shown in
Figure 8.

Figure 8. Bayer process (Riman). 45 )

Table 8. Typical Characteristics of Zr02 Powders by Hydcothermal

Chemical composition (wt%)

Zr0 2 94.7 86.0 >99.9
Y 20 3 13.9
Al,03
Si0 2
Fe203
Na2 0
er
Figure 7. TEM of monoclinic zirconia powder
using hydrothermal reaction (100 MPa at 400°C
for 24 h) using 8 wt % KF solution.

Table 7. Pbases Present and Crystallite Size ofProdncts by

Hydcothennal Reaction at 100 MPa for 24 h

Temperature
Mineralizer (oC)

KF(8wt%) 200 Not detected

KF(8wt%) 300 Not detected
'Three-point bending method.
NaOH (30 wt%) 300 Not detected
:,M! method.
H 20 300 15 17
LiCl(J5wt%) 300 15 19
KBr (10 wt%) 300 13 15
E. Hydrothermal Electrochemical Method 48 • 49 )
Figure 12 shows an apparatus used in the
(2) Zirconia 46 • 47 ) hydrothermal electrochemical method. For
preparing BaTi0 3 , titanium and platinum plates
Hydrothermal homogeneous precipitation
52 Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for Advanced Ceramics?

are used as anodes and cathodes, respectively.

A solution of barium nitrate 0.1 N or 0.5 N and
temperatures up to 250 oC were used for the
experiment. The current density was 100
mA/cm 2 . Under these conditions we were able
to produce BaTi0 3 powder. The BaTi0 3 powder
produced by this process is shown in Figure 13.
Zr0 2 was also produced by this method. In the
case of Zr0 2 , Zr plates were used.

Figure 11. SEM of zirconia sintered at 1400°C

for 2 h.

Figure 9. Zr0 2 produced by the hydrothermal

homogeneous precipitation process.

F. Reactive Electrode Submerged Arc 50 • Sl)

Reactive electrode submerged arc (RESA) is a
totally new process for making powders. RESA
produces extremely high temperatures Figure 12. Schematic of the electrochemical cell
(approximately 10,000 K) with a pressure of 1 and circuit arrangements for anodic oxidation of a
atm H 2 0. It allows one to change liquids very titanium metal plate under hydrothermal
easily. Figure 14 shows the apparatus to conditions. (A) Counter electrode (platinum
produce powders. plate), cathode; (B) thermocouple; (C) stirrer; (D)
reference electrode (platinum plate); (E) working
electrode (titanium plate), anode.

Figure 10. TEM pictures of hydrothermal

homogeneous precipitation Zr0 2 .
S. Somiya et al. Transactions of the Materials Research Society ofJapan 20th Anniversary Special Issue47-57 (2010) 53

Figure 13. TEM of BaTi0 3 powders prepared by

the hydrothermal electrochemical method (250°C,
0.5 N Ba(N0 3h, titanium plate). (a) Apparatus of Spark Discharge Process

(b) Aluminum metal (c) Alumina powder

Figure 15. Spark Discharge Process.

G. Spark Discharge Process 52 • 53 l

This method is the similar to the reactive
electrode submerged arc (RESA) by Iwatani
Chemical Industry Co. Ltd., so called "Spark
Figure 14. Schematic of microprocessor- Discharge Process." The process is shown in
controlled RESA apparatus for fine powder Figure 15. The company produced only Ah0 3 ,
preparation (A. Kumar and R. Roy). 50 · 5 1l MgO, Al(OH) 3 , Mg(OH)2, spinel, spinel hydrate,
etc. by this method. Properties of the products
are shown in Table 9.

Table ~9. PaWdes bf'Spark Discharlie ProceSs

IWATANIAU!MJNA s 3
Aluminum hydroxide Activated alumina Activated alumina u-Alumina
RH-30 RH-40 RK-30 RK-40 RG-30 RG-40 RA-30 RA-40 R-2
d AI,O,(%) >99.90 >99.99% >99.9 >99.99 >99.9 >99.99 >99.9 >99.99 >99.99
:~ Fe 0.0150 0.0005 0.0210 0.0007 0.0210 0.0007 0.0210 0.0007 0.0010
~
Si 0.0150 0.0013 0.0210 0.0018 0.0210 0.0018 0.0210 0.0018 0.0026
E'
8 Cu 0.0004 0.0001 0.0005 0.0001 0.0005 0.0001 0.0005 0.0001 0.0001

]
u
Mg
Ni
0.0002
0.0002
0.0001
0.0001
0.0003
0.0003
0.0001
0.0001
0.0003
0.0003
0.0001
0.0001
0.0003
0.0003
0.0001
0.0001
0.0007
0.0001
Na 0.0004 0.0002 0.0005 0.0003 0.0005 0.0003 0.0005 0.0003 0.0011
Specific surface area (m 2/g) 37.0 282.0 48.0 5.3 6.5
Mean particle size (Jl) 1.35 0.71 0.51 0.98 0.50
Green density (gfcm3) - I I I. - _I 2.17
Fired density (glcm3) I 3.92
(I)! _1000kgcm'_

IWATANI MAGNESIA AND SPINEL

~esium hydro Magnesium oxide Spinel by drat Spine!
MH-30 MTK-30 MJ-30 SP-H SP-12
A1 0.0070 0.0100 0.0100 50.19 71.7
Fe 0.0020 0.0028 0.0028 0.0125 0.0180
Si 0.0075 0.0110 0.0110 0.0160 0.0230
Mg >99.9 *" 1
>99.9 *-2 >99.9 *" 2 19.74 28.2
Ca 0.0006 0.0009 0.0009 0.0005 0.0007
Specific surface area (m2/g) 58.0 160.0 28.0 45.0 17.0
Mean particle size (Jl) 0.40 0.23 0.32 0.23 0.30
54 Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for Advanced Ceramics?

H. Hydrothermal Mechanochemical Process 54 ) magnitude compared to conventional

Ba(OH)z and FeC1 3 were used as starting hydrothermal processing. The use of
materials. The precipitate was crystallized microwaves in both solid and liquid states is
hydrothermally in an apparatus (Figure 16) gaining in popularity for many reasons, but
combined with an attritor and ambient water especially because of the potential energy savings.
pressure. The starting solutions with the The use of microwaves under hydrothermal
precipitate and stainless steel balls (5 mm conditions can accelerate the synthesis of
diameter) were placed in Teflon beakers. A anhydrous ceramic oxides such as titania,
Teflon propeller was rotated in the beaker under hematite, barium titanate, lead zirconate titanate,
200°C and 2 MPa. The speed of the propeller lead titanate, potassium niobate, and metal
was from 0 to 107 rpm. The number of stainless powders such as nickel, cobalt, platinum,
steel balls was 200, 500, and 700. X-ray palladium, gold, silver, etc., and this is expected
diffraction profiles are shown in Figure 17. to lead to energy savings. The term
"microwave-hydrothermal" processing was first
coined by us for reactions taking place in
Teflon propeller solutions that are heated to temperatures greater
than 100°C in the presence of microwaves. The
value of this technique has been demonstrated in
rapid heating to the temperature of treatment,
which can save energy; increasing the reaction
' kinetics by one to two orders of magnitude;
forming novel phases; and eliminating metastable
. phases. Figure 19 shows a nanophase powder of
•
• .·as '-
(1)
hematite .

o BaO · 6Fe20 3
• (1)
0
:I: A BaO · Fe203
0
• • 0
•

Starting materials
Teflon beaker
Figure 16. Experimental apparatus for
hydrothermal mechanochemical reactions.

I. Microwave Hydrothermal Process 55 . 58 l (a)

Microwave-assisted hydrothermal
synthesis is a novel powder processing
technology for the production of a variety of
ceramic oxides and metal powders under
closed-system conditions. Komarneni et al.
25 30 35 40 45 50
developed this hydrothermal process into which
microwave are introduced. This closed-system
20 Cuka
technology not only prevents pollution during the Figure 17. X-ray diffraction profiles of (a)
synthesis of lead-based materials, but also saves starting materials, (b) material fabricated at
energy, and thus could substantially reduce the 200oC under 2 MPa for 4 h without rotation, and
cost of producing many ceramic powders. (c) material fabricated at 200°C for 4 h using 200
Hydrothermal microwave treatment of 0.5 M balls at 37 rpm.
TiCl4 was done in 1 M HCl to form rutile. The
system operated at a 2.45 GHz. The vessel is J. Hydrothermal Sonochemical Method or
lined with Teflon (Figure 18) and the system is Hydrothermal Ultrasonic Method 59 . 61 l
able to operate up to 250°C. The parameters Ultrasonic waves are often used in
used are temperature, pressure, time, analytical chemistry for dissolving powder into
concentration of the metal solution, pH, etc. solution. The hydrothermal sonochemical
The key result is crystallization reactions, which method is a new method for synthesizing
lead to faster kinetics by one or two orders of materials.
S. Somiya et al. Transactions of the Materials Research Society ofJapan 20th Anniversary Special Issue 47-57 (201 0) 55

Acknowledgement
5. Summary One of the authors of this paper, S. S. was
This paper describes a review of powders, nominated Honorary Member of the Korean
especially characteristics of powders from gas Ceramic Society on November 8, 2007. He
phase, liquid phase and ideal powders for presented this paper at the meeting of the 50th
ceramics. Powders from hydrothermal process Anniversary Ceremonies of the Korean Ceramic
are close to the ideal powders. Hydrothermal Society. He wishes to express his appreciation
powders are explained in detail. to the Korean Ceramic Society and his friends.

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method. 61 ) 17. H. Yamamoto, Preparation Powders, 22-38 (1991) in
Ref.7
56 Ceramic Powders for Advanced Ceramics: What are Ideal Ceramic Powders for Advanced Ceramics?

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(Received December 15, 2009; Accepted August 25, 2010)

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