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Synthesis andcharacterisation of nanocrystalline MgAl2O4 ceramic powders by use of molten salts

机译:熔融盐法合成纳米晶MgAl 2 O 4 陶瓷粉及其表征

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Nanocrystalline MgAl2O4 powders were prepared by a thermal decomposition method, i.e. by use of molten salts. This method involves co-melting stoichiometric amounts of magnesium nitrate hydrate Mg(NO3)2.6H 2O and aluminium nitrate hydrate Al(N O3) 3.9H2O at 500°C. The spinel content of the co-melted and calcined powders at different firing temperatures up to 1000°C was determined by chemical analysis and the powders were characterised with respect to spinel formation, crystallite and particle sizes by X RD, T EM , and IR spectroscopy. The results obtained revealed that the co-melted materials were amorphous. After heat treatment of the amorphous materials at up to 1000°C, pure spinel powder was obtained, reaching over 98% spinel content. During calcination at different firing temperatures up to 1000°C the amorphous material progressively crystallised, forming nanocrystalline spinel with a maximum crystallite size of about 10 nm and particle size of around 300 nm. Bands in IR spectra were observed corresponding to the ex istence of AlO6 groups prior to magnesium spinel formation, which was the only crystalline phase at 1000°C.
机译:通过热分解方法,即使用熔融盐,制备纳米晶态的MgAl 2 O 4 粉末。该方法涉及将化学计量的硝酸镁水合物Mg(NO 3 2 .6H 2 O与硝酸铝水合物Al(NO 3 3 .9H 2 O在500°C下。通过化学分析确定在不同的烧成温度下直至1000°C的共熔融和煅烧粉末的尖晶石含量,并通过X射线衍射,TEM和IR光谱对粉末的尖晶石形成,微晶和粒度进行表征。 。所得结果表明,共熔材料是非晶态的。在高达1000°C的温度下对无定形材料进行热处理后,可获得纯尖晶石粉末,其尖晶石含量超过98%。在至多1000℃的不同烧成温度下煅烧期间,无定形材料逐渐结晶,形成具有最大微晶尺寸为约10nm且粒径为约300nm的纳米晶尖晶石。观察到红外光谱带对应于镁尖晶石形成之前AlO 6 基团的存在,这是1000°C时唯一的结晶相。

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