Cryst. Res. Technol. 44, No. 5, 463 – 468 (2009) / DOI 10.1002/crat.200800604
© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Flux growth and characterization of Ti- and Ni-doped forsterite
single crystals
A. Bloise*, E. Barrese, C. Apollaro, and D. Miriello
Dipartimento di Scienze della Terra, Università della Calabria - Via Pietro Bucci, 87036 Arcavacata di Rende
(CS), Italy
Received 13 December 2008, revised 23 January 2009, accepted 5 February 2009
Published online 20 February 2009
Key words flux crystal growth, Ti-doped forsterite crystals, Ni-doped forsterite crystals.
PACS 81.10.-h, 61.72.Ww
Forsterite monocrystals doped with Ti and Ni were grown by the flux growth technique. A suitable mixture of
flux (MoO
3
, V
2
O
5
, Li
2
CO
3
) and nutrient was slowly cooled down to 750 °C from 1250 °C or 1350 °C. The
crystals were then characterized by powder and single-crystal X-ray diffraction, scanning electron microscopy
and differential scanning calorimetry (DSC). Variations observed in crystal size were attributed by both the
varying experimental conditions in which they had been obtained, and to the amount of Ni substituted for Mg
in the structure. High abundances of doped forsterite required a cooling rate of 1.8 K h
-1
. These synthetic,
well-characterized Ti and Ni doped forsterite crystals may have potential for exploitation in industrial fields.
© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
1 Introduction
Forsterite (Mg
2
SiO
4
) is the magnesium-rich end-member of the olivine solid-solution family and the major
component of the earth’s upper mantle [1]. The crystalline structure of forsterite is based on a nearly hexagonal
close-packed array of oxygens with Si in the tetrahedral and Mg in the octahedral sites, and crystallizes in the
orthorhombic system with space group Pnmb. There are two kinds of Mg-octahedral sites, M1 (Ci symmetry)
and M2 (Cs symmetry), M1 being smaller than M2 [2].
Forsterite crystals, owing to their good properties, e. g. refractoriness (melting point 1890 °C), low
dielectric permittivity, low thermal expansion, and chemical stability, are ideal substrates in electronics and
optimal materials for thermal insulation in applications at high temperatures. The usual presence of foreign
ions (Fe, Ni, Mn, etc.) in natural forsterite and their inconstant amounts, may inhibit as high-performance
materials. For these reasons, pure and doped forsterite have been grown by several researchers [3-8] with
differing methods (e.g., Czochralski methods, sol-gel, co-precipitation, etc.). The synthesis and
characterization of forsterite doped with transition metal ions has also been an important subject in recent years
[9-11], since potential use have been found in laser optics [12]. It has been calculated that, in Ti-doped
forsterite crystals grown by Czochralski methods, the concentration of Ti
3+
ions on site M2 is ten times greater
than that on site M1[13]. Such crystals may have useful applications for lasers in the future.
Ni-doped forsterite, which may also be used in tunable lasers, grown by the floating zone technique, shows
that Ni
2+
ion preferentially substitutes for Mg in the centrosymmetric M1 site at low concentrations [14]
although, at higher concentrations, M2 site is also occupied [15]. So far, doped forsterite has been synthesized
in various experimental conditions, mainly to study its spectral and luminescent properties and not to define in
detail the kinetic process allowing their growth. The purpose of the present work was to optimize the
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* Corresponding author: e-mail: andrea.bloise@unical.it