A novel method to low temperature synthesis of nanocrystalline forsterite

doi:10.1016/j.materresbull.2006.07.020

Materials Research Bulletin

Volume 42, Issue 4, 12 April 2007, Pages 666-673

https://doi.org/10.1016/j.materresbull.2006.07.020 Get rights and content

Abstract

Nanocrystalline forsterite (Mg₂SiO₄) powder was synthesized using sucrose as a chelating agent and template material from an aqueous solution of magnesium nitrate and colloidal silica. The synthesized powders were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), simultaneous thermal analysis (STA), and scanning electron microscopy (SEM). The synthesized nano-powder had particle size smaller than 200 nm and average crystallite size of powders calcined at 800 °C for 3 h was in the range of 10–30 nm. Also the effect of addition 2 and 4 wt.% forsterite seed on nucleation temperature and crystallite size of forsterite was investigated. The presence of small amounts of Mg₂SiO₄ as seed obviously accelerated the crystallization of forsterite. According to DTA results the inceptive formation temperature of Mg₂SiO₄ without any seed was 760 °C, while this temperature for the specimen containing 4 wt.% seed was 700 °C.

Introduction

Forsterite is a crystalline magnesium silicate with chemical formula Mg₂SiO₄, which has extremely low electrical conductivity that makes it an ideal substrate material for electronics. On the other hand it shows good refractoriness due to high melting point (≈1890 °C), low thermal expansion, good chemical stability and excellent insulation properties even at high temperatures [1], [2], [3].

Forsterite has been synthesized by different methods such as solid-state reaction, self-propagation high-temperature synthesis, and sol–gel. The production of forsterite via solid-state reactions usually requires high temperature and long reaction time while the sol–gel process can provide molecular-level of mixing and high degree of homogeneity, which leads to reduce crystallization temperature and prevent from phase segregation during heating. However, in multi-component silicate systems, the hydrolysis and condensation rates are different with in silica and the other alkoxides which may cause non-uniform precipitation and chemical inhomogeneity of the gels, and also result in higher crystallization temperature and undesired phases [4], [5], [6], [7].

One of the effective methods that recently have been developed is sucrose process, which is established for the preparation of fine oxide ceramic powders [8]. In this technique, a uniform particle size powder is produced due to a homogeneous metal ion distribution in the solution. As mean while, other elements such as C, H, and N are easily removed during calcination. Therefore, the purity of the final powder does not get affected when sucrose is used as a chelating agent and template material [9]. The object of the present research is the synthesis of nanocrystalline forsterite powder from magnesium nitrate, colloidal silica, and sucrose at low temperatures. Also the effect of seed addition on nucleation and inceptive formation temperature of forsterite has been investigated.

Section snippets

Powder preparation

Magnesium nitrate (Mg(NO₃)₂·6H₂O), sucrose as a template material, PVA (polyvinyl alcohol, M_W = 145,000), nitric acid (all purchased from Merck Co., Germany) and colloidal silica with particle size smaller than 14 nm (26 wt.% solid fraction-from Monatso Co., Belgium) were used as starting materials.

To prepare a transparent sol, 0.0142 mol magnesium nitrate (3.639 g) was dissolved in 50 ml of deionized water. Then 0.0071 mol of silica (1.642 g of colloidal silica) was introduced into the solution to set

STA results

The STA curves of the precursor are shown in Fig. 2. The small endothermic peak about 110 °C in DTA accounted for 6% of the initial weight loss in TG, is assigned to exit of free water. As it can be seen 50% weight loss between 200 and 420 °C is due to decomposition of precursor and burning of carbon. Simultaneously the exothermic peak between 200 and 420 °C proves the burning of polymeric matrix. Also the second exothermic peak (520 °C) may be caused by the formation of periclase (MgO). The third

Conclusions

Nanocrystalline Forsterite (Mg₂SiO₄) has been synthesized by a polymer matrix method at low temperatures. The crystallite size is in the range of 10–30 nm, and its particle size is smaller than 200 nm in the calcined sample at 800 °C. This chemical synthesis through polymer matrix comprising sucrose and PVA, is applicable and cost effective compared to those of other processes, for the preparation of nano-sized forsterite. The initial crystallization temperature of forsterite powder is about 760

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A novel method to low temperature synthesis of nanocrystalline forsterite

Abstract

Introduction

Section snippets

Powder preparation

STA results

Conclusions

J. Alloys Compd.

J. Eur. Ceram. Soc.

Mater. Lett.

Mater. Lett.

J. Non-Cryst. Solids

Phil. Mag. Lett.

Refractories Production and Properties