Hindawi Publishing Corporation
Bioinorganic Chemistry and Applications
Volume 2011, Article ID 453759, 10 pages
doi:10.1155/2011/453759
Research Article
Sintering Behavior of Magnesium-Substituted Fluorapatite
Powders Prepared by Hydrothermal Method
S. Nasr and K. Bouzouita
U.R. Mat´ eriaux Inorganiques, Institut Pr´ eparatoire aux Etudes d’Ing´ enieur, University of Monastir, Rue Eben El Jazar 5019,
Monastir 5000, Tunisia
Correspondence should be addressed to S. Nasr, nasrsamia@yahoo.fr
Received 13 December 2010; Accepted 19 January 2011
Academic Editor: Lorenzo Pellerito
Copyright © 2011 S. Nasr and K. Bouzouita. This is an open access article distributed under the Creative Commons Attribution
License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly
cited.
Magnesium-substituted fluorapatite powders were synthesized by hydrothermal method, and their sintering behavior was
investigated by dilatometry in the temperature range 25–1100
◦
C. Analysis of the obtained powders by X-ray diffraction and
31
P NMR spectroscopy showed that the powders consisted of a single apatite phase and no amorphous phase has been formed.
Compared to pure fluorapatite, the shrinkage of the substituted samples occurred in two steps and the temperature at which
the sintering rate was maximum is lower. In addition, the shrinkage was interrupted by an expansion of the samples due to the
formation of a liquid phase. The latter phase led to the crystallization of needle-crystals by a dissolution-diffusion-reprecipitation
process.
1. Introduction
Owing to their physicochemical and biological properties,
the hydroxyapatite (Ca
10
(PO
4
)
6
(OH)
2
, HA) and to a lesser
extent the fluorapatite (Ca
10
(PO
4
)
6
F
2
, FA) have been exten-
sively investigated over the last three decades. They offer
important opportunities for applications in a diversity of
areas particularly in medicine and dentistry [1–7]. Moreover,
many applications have become possible thanks to their
notable stability and their ability to accommodate a great
number of substitutions; both cationic and anionic substi-
tutions are possible [8–10]. For example, Ca
2+
ion can be
substituted by various divalent cations such as Mg
2+
, Sr
2+
,
Pb
2+
, Cd
2+
, and so forth. Among these ions, some of them
(Sr
2+
, Cd
2+
or Pb
2+
) lead to a solid solution in the whole
range of composition [11–13], while the incorporation of
other ions such as Mg
2+
or Mn
2+
, into the apatite structure
remains limited [14–19].
Magnesium, whose concentration varies from 0.44 to
1.23 wt% [20], is one of the most abundant elements that
are present in hard tissues. It has a prominent effect on the
osteoporosis [21] and mineralization process [22, 23]. Thus,
the synthesis of hydroxyapatite and fluorapatite powders in
controlled Magnesium content is of a practical importance
to develop biomaterials whose chemical composition is
as close as possible to that of bone. Despite numerous
studies that have been devoted to the incorporation of Mg
into the hydroxyapatite structure [14–16], its substitution
limit is a subject of controversy and the process of its
incorporation remains unclear. Indeed, according to the used
synthesis method, the substitution limit of this element in
the hydroxyapatite varies from ∼0.3 to 28.4 wt% [16, 24].
Furthermore, it is reported that all of the Mg used was
not really incorporated into the apatite structure, but a sig-
nificant proportion is adsorbed on the surface of the particles
in an amorphous phase and/or in another form [14, 25].
Different methods can be used for synthesis the apatite
such as solid-state reaction [26], coprecipitation [15, 17],
sol-gel [27] and hydrothermal synthesis [18]. Hydrothermal
synthesis offers a relatively simple and effective way to