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Controlled hydrolysis experiments of the heterobimetallic alkoxide {Cu[Al(OPri)4]2}, were investigated. The progress of hydrolysis was monitored by the FT-IR and NMR spectroscopy. A blue colored gel appeared after four days of hydrolysis and the hydrolysis experiments were continued up to ten days. The elemental analysis and FT-IR spectrum revealed the presence of isopropoxy group in the gel obtained even after ten days of hydrolysis. The presence of carbon was further confirmed from the presence of a weak signal at 3.351 ppm in the 13C CP-NMR spectrum. The thermal analysis of the hydrolyzed gels in air also suggested that they were not simple hydroxides of copper and aluminum. The gels on one time heat treatment at 900 °C in air yielded inverse spinel CuAl2O4 as shown by the PXRD patterns. CuO was observed along with CuAl2O4 in the case of the fired product of the gel obtained after five or six days of hydrolysis which was absent in the fired product of ten days hydrolyzed gel. The phase pure spinel was nanocrystalline in nature as revealed by the analysis of PXRD pattern. TEM images revealed porous structured nanocrystallites. The optical property of the spinel was evaluated by the diffuse reflectance spectroscopy. Raman spectrum showed five bands at 767, 698, 595, 450 and 356 cm?1 conforming to the spinel structure. 相似文献
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Epsita?Ghanti Nobel?Tomar Prikshit?Gautam R.?NagarajanEmail author 《Journal of Sol-Gel Science and Technology》2011,57(1):12-15
Al(OPh)3 involving sterically hindered phenyl groups on ultrasonic assisted micro hydrolysis yielded a mixture of boehmite and bayerite
as deduced from the FTIR and powder X-ray diffraction pattern. In the thermogravimetric trace, the complete removal of decomposable
moieties of the hydrolyzed gel occurred around 530 °C. Calcining the gel at temperatures 600, 700, 800 and 900 °C showed crystalline
tetragonal δ-Al2O3 to be the product at 900 °C as deduced from FTIR, 27Al NMR and PXRD techniques. δ-Al2O3 showed a surface area of 135 m2/g with rectangular bar like morphology with the sizes below 50 nm in the TEM images. 相似文献
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