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Crystallization of amorphous Al2O3-SiO2 precursors doped with nickel

机译:掺杂镍的非晶态Al2O3-SiO2前驱体的结晶

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The crystallization of amorphous diphasic Al2O3-SiO2 precursors doped with nickel has been studied by differential scanning calorimetry (DSC), XRD diffraction (XRD) and scanning and transmission electron microscopy (SEM, TEM) equipped with energy dispersive X-ray spectroscopy (EDS). Diphasic gels with constant atomic ratio (Al + Ni)/Si = 3: 1, where 0, 1, 2 and 3 at.% of aluminum were replaced by nickel, have been prepared by hydrolyzing of TEOS in aqueous solution of aluminum nitrate. Crystallization of Ni-containing gamma-Al2O3 preceded the crystallization of Al-Si spinel. Activation energy of 603 +/- 16 kJ mol(-1) for crystallization of Ni-containing gamma-Al2O3 was obtained in non-isothermal conditions. Ni-incorporated gamma-Al2O3 transforms gradually with the temperature increase into Ni aluminate spinel, while Al-Si spiriel reacts with amorphous silica forming mullite at about 1200 degrees C. Rietveld structure refinement of phases present in the samples annealed at 1600 degrees C and SEM-EDS and TEM-EDS analyses of related phases have shown that nickel predominantly crystallizes as NiAl2O4, but small amount of nickel is incorporated in mullite structure, as well as, dissolved in the glassy phase of the system. (c) 2007 Elsevier B.V. All rights reserved.
机译:已通过差示扫描量热法(DSC),XRD衍射(XRD)以及配备能量色散X射线光谱仪(EDS)的扫描和透射电子显微镜(SEM,TEM)研究了掺杂镍的非晶相Al2O3-SiO2前驱体的结晶。 。通过在硝酸铝水溶液中水解TEOS,制得了具有恒定原子比(Al + Ni)/ Si = 3:1的两相凝胶,其中0、1、2和3 at。%的铝被镍代替。含镍的γ-Al2O3的结晶先于铝硅尖晶石的结晶。在非等温条件下获得了603 +/- 16 kJ mol(-1)的活化含镍的γ-Al2O3结晶的活化能。掺镍的γ-Al2O3随着温度的升高逐渐转变为铝酸镍尖晶石,而铝硅螺线管与非晶硅在大约1200摄氏度下反应形成莫来石。在1600摄氏度和SEM下退火的样品中存在的相的Rietveld结构细化-EDS和TEM-EDS相关相的分析表明,镍主要以NiAl2O4的形式结晶,但是少量的镍以莫来石结构结合,并溶解在系统的玻璃相中。 (c)2007 Elsevier B.V.保留所有权利。

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