Hydrothermal Synthesis of Advanced Ceramic Powders
Wojciech L. Suchanek
1, a
and Richard E. Riman
2, b
1
Sawyer Technical Materials, LLC, 35400 Lakeland Boulevard, Eastlake, OH 44095, USA
2
Rutgers University, Department of Materials Science and Engineering, 607 Taylor Road,
Piscataway, NJ 08855, USA
a
wls@SawyerLLC.com,
b
riman@email.rci.rutgers.edu
Keywords: Hydrothermal synthesis, review powder synthesis, morphology control,
hydroxyapatite, PZT, alumina, zinc oxide, carbon nanotubes.
Abstract. This paper briefly reviews hydrothermal synthesis of ceramic powders and shows how
understanding the underlying physico-chemical processes occurring in the aqueous solution can be
used for engineering hydrothermal crystallization processes. Our overview covers the current status
of hydrothermal technology for inorganic powders with respect to types of materials prepared, ability
to control the process, and use in commercial manufacturing. General discussion is supported with
specific examples derived from our own research (hydroxyapatite, PZT, Į-Al
2
O
3
, ZnO, carbon
nanotubes). Hydrothermal crystallization processes afford excellent control of morphology (e.g.,
spherical, cubic, fibrous, and plate-like) size (from a couple of nanometers to tens of microns), and
degree of agglomeration. These characteristics can be controlled in wide ranges using
thermodynamic variables, such as reaction temperature, types and concentrations of the reactants, in
addition to non-thermodynamic (kinetic) variables, such as stirring speed. Moreover, the chemical
composition of the powders can be easily controlled from the perspective of stoichiometry and
formation of solid solutions. Finally, hydrothermal technology affords the ability to achieve cost
effective scale-up and commercial production.
Introduction
Hydrothermal research was initiated in the middle of the 19
th
century by geologists and was aimed at
laboratory simulations of natural hydrothermal phenomena. In the 20
th
century, hydrothermal
synthesis was clearly identified as an important technology for materials synthesis, predominantly in
the fields of hydrometallurgy and single crystal growth [1]. However, the severe (supercritical)
reaction conditions required particularly for growing single crystals have discouraged extensive
research and commercialization for many materials. In recent years, commercial interest in
hydrothermal synthesis has been revived in part because a steadily increasing large family of
materials, primarily ceramic powders, has emerged that can be prepared under mild conditions
(T<350ºC, P<100 MPa). The growing number of scientific papers on hydrothermal synthesis of
ceramic powders, which almost quadrupled between 2000 and 2004 (Fig. 1a), illustrates the rising
interest in this area, with China, Japan, and USA publishing most extensively (Fig. 1b).
Hydrothermal Synthesis as a Materials Synthesis Technology
Process Definition. Hydrothermal synthesis is a process that utilizes single or heterogeneous phase
reactions in aqueous media at elevated temperature (T>25ºC) and pressure (P>100 kPa) to
crystallize ceramic materials directly from solution. However, researchers also use this term to
describe processes conducted at ambient conditions. Syntheses are usually conducted at autogeneous
pressure, which corresponds to the saturated vapor pressure of the solution at the specified
temperature and composition of the hydrothermal solution. Upper limits of hydrothermal synthesis
extend to over 1000ºC and 500 MPa pressure [2]. However, mild conditions are preferred for
commercial processes where temperatures are less than 350ºC and pressures less than
Advances in Science and Technology Vol. 45 (2006) pp. 184-193
online at http://www.scientific.net
© (2006) Trans Tech Publications, Switzerland
All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the
written permission of the publisher: Trans Tech Publications Ltd, Switzerland, www.ttp.net . (ID: 12.45.174.100-24/10/06,17:51:02)