Available online at www.sciencedirect.com
Journal of the European Ceramic Society 30 (2010) 3377–3387
Follow-up of zirconia crystallization on a surface modified alumina powder
V. Naglieri
a,b
, L. Joly-Pottuz
b
, J. Chevalier
b,∗
, M. Lombardi
a
, L. Montanaro
a
a
Dept. Mater. Sci. and Chem. Eng., INSTM LINCE Lab., Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino, Italy
b
Université de Lyon, INSA de Lyon, MATEIS UMR CNRS 5510, Bât. Blaise Pascal, 7 Av. Jean Capelle, 69621 Villeurbanne, France
Received 18 February 2010; received in revised form 4 July 2010; accepted 16 July 2010
Available online 19 August 2010
Abstract
Here we report how thermal treatments of a surface modified -alumina powder on which a zirconium oxide precursor was grafted can be tailored
so as to obtain an alumina–zirconia composite powder with well-controlled phase distribution and size. The transformation of the zirconia precursor
from a starting amorphous phase to zirconia nano-grains bonded to the alumina particles surface was followed by X-ray diffraction (performed
at room temperature on different thermally treated powders, as well as in situ at high-temperature) and by both conventional and high resolution
transmission electron microscopy (TEM and HRTEM). Phase and nanostructure evolutions were followed on a large temperature span. The
crystallization kinetics were analysed in terms of nucleation-growth mechanisms by exploiting Avrami–Johnson–Mehl–Kolmogorov formalism.
Based on the above investigations, a tentative description of nucleation and growth features is proposed. This knowledge-based step represents a
first approach towards nanopowders engineering.
© 2010 Elsevier Ltd. All rights reserved.
Keywords: Calcination; Sintering; Grain growth; Nanocomposites; Microstructure-final; Microstructure-prefiring
1. Introduction
Alumina–zirconia composites are used as grinding media and
cutting-tools, wear parts
1
and biomedical implants,
2,3
since they
exhibit high hardness, strength and high fracture toughness due
to transformation toughening mechanisms.
4–7
Especially, they
are raising interest in orthopaedics, since they exhibit a larger
crack resistance than alumina and a lower sensitivity to aging
than zirconia. However, the content and the distribution of zir-
conia grains inside the alumina matrix have a strong impact
on their performances.
2
In particular, micro-nano-composites in
which nano-zirconia particles are embedded in micron sized alu-
mina matrix are expected to exhibit improved slow crack growth
resistance and stability.
8
To achieve the control of microstruc-
tural features at different scales, each step of the process, from
powder synthesis to sintering, must be carefully set up.
Alumina–zirconia powders can be prepared by various strate-
gies, from the simple powder-mixing
2
to chemically based
routes, like sol–gel,
4,9,10
co-precipitation,
11
and mixed-salts
thermal decomposition.
12,13
Torrecillas and co-workers recently
∗
Corresponding author.
E-mail address: jerome.chevalier@insa-lyon.fr (J. Chevalier).
proposed a sophisticated and effective approach based on the
powder–alkoxide mixture,
14
in which a zirconium alkoxide is
grafted to the surface of alumina grains. After thermal treat-
ments, zirconia nanocrystals, strongly bonded to the alumina
surface, are developed. Such promising route has been applied
and simplified by working in aqueous medium with inor-
ganic zirconium salts.
15
These powders offer the opportunity to
develop dense composite materials with very fine and homo-
geneous microstructures, which represent a robust approach
towards real nanostructured ceramic materials with promising
properties. However, to our knowledge, there is still a lack
of investigation concerning the intermediate steps between the
starting amorphous phase on the alumina surface and the final
developed microstructure, whereas a strict control of the nucle-
ation and growth of zirconia crystals is needed to really achieve
fully tailored microstructures.
Here, this aim was pursued, by a precise follow-up of zirco-
nia crystallization at the surface of alpha alumina grains during
thermal treatments via X-ray diffraction (XRD) analysis and
TEM observations. The final goal of the present work was to
propose a possible nucleation-growth scenario able to support
the choice of a suitable powder treatment to tailor phase distri-
bution and size in the alumina–zirconia composite powder and
consequently on sintered bodies.
0955-2219/$ – see front matter © 2010 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jeurceramsoc.2010.07.029