アルコキシドの水熱処理によるAl2O3-SiO2系粉末の調製

概要

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Aluminosilicate powders were obtained by hydrothermal treatment of mixed alkoxide solution containing Al2O3:Si02=3:2 (mol ratio) with distilled water at 300-600°C under 10-100 MPa for 2 hr. Very fine crystalline pseudoboehmite (γ-AlOOH)-like phase was formed at 300-500°C under 10-100 MPa. Above 600°C, instead of the pseudoboehmite-like phase, amorphous product was formed under 10 MPa, Al-Si spinel under 50 MPa, and hydralsite (2Al2O3⋅2SiO2⋅H2O), AS(H)-II (close to Al2SiO5), Al-Si spinel and a small amount of mullite (3Al3O3⋅2SiO2-2Al2O3SiO2) under 100 MPa, respectively. Transmission electron microscope (TEM) revealed that the pseudoboehmite-like phase obtained at 300°C under 50 MPa was thin plate of about 10 nm thick and 100 nm long, and contained homogeneously both Al and Si in the narrow area as a few hundreds nm2, by energy dispersive spectrometric (EDS) analysis. The organic solvent such as benzene and alcohol might stabilize the fine crystals of pseudoboehmite-like phase and prevent the crystalization of hydralsite or As(H)-II.
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