Preparation and Characterization of Nano-Sized Magnesium Ferrite Powders By a Starch-Gel Process and Corresponding Ceramics

R. Köferstein, T. Walther, D. Hesse, S. Ebbinghaus
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Abstract

The synthesis and characterization of nano-sized MgFe2O4 by a starch-gel method is described herein. A phase-pure nano-sized MgFe2O4 powder (1a) was obtained after calcining a (MgFe) starch gel at 550 °C. The powder has a specific surface area of 60.6 m2/g and a crystallite size of 9 nm. TEM investigations reveal particles in the range of 7 to 15 nm. The activation energy of the crystallite growth process was calculated as 89 ± 14 kJ/mol. The shrinkage and sintering behaviour of resulting compacts were studied. UV−VIS investigations of the nano-sized powder 1a reveal an optical band gap of 2.38 eV, whereas calcination at 1100 °C (powder 1g) leads to a crystallite size of 129 nm and a band gap of 2.16 eV. Magnetization loops at 300 K and the temperature dependence of both the field-cooled (FC) and the zero-field-cooled (ZFC) agnetization indicate a superparamagnetic behaviour. The blocking temperature for powder 1a was determined as 140 K at a field of H = 500 Oe. We found different saturation magnetizations (Ms) depending on the calcination temperature. Calcination at 550 °C (1a) results in Ms = 20.0 emu/g which increases with calcination temperature to a maximum of 37.7 emu/g for powder 1e calcined at 900 °C. Ceramic bodies sintered between 1450 and 1600 °C exhibit Ms values of 25−28 emu/g. Magnetic investigations at 10 K on powders 1a−1g show hysteresis loops with coercivities up to 950 Oe, remanences to 10 emu/g and Ms values to 50.4 emu/g. Additionally, the nano-scaled powders show a shift of the hysteresis loops.
淀粉-凝胶法制备纳米铁氧体镁粉体及其陶瓷表征
本文介绍了淀粉-凝胶法制备纳米MgFe2O4并对其进行了表征。在550℃下煅烧(MgFe)淀粉凝胶,得到相纯纳米MgFe2O4粉末(1a)。该粉体的比表面积为60.6 m2/g,晶粒尺寸为9 nm。透射电镜研究显示颗粒在7至15纳米范围内。晶体生长过程的活化能为89±14 kJ/mol。研究了压坯的收缩率和烧结性能。对纳米级粉体1a的UV - VIS研究显示其光学带隙为2.38 eV,而在1100℃(粉末1g)下煅烧得到的晶体尺寸为129 nm,带隙为2.16 eV。300 K下的磁化回路以及场冷(FC)和零场冷(ZFC)磁化的温度依赖性表明了超顺磁行为。在H = 500 Oe的电场下,确定粉末1a的阻滞温度为140 K。我们发现不同的饱和磁化强度(Ms)取决于煅烧温度。在550°C (1a)下煅烧得到的Ms = 20.0 emu/g,随着煅烧温度的增加,在900°C下煅烧的粉末1e最高可达37.7 emu/g。在1450 ~ 1600℃之间烧结的陶瓷体的Ms值为25 ~ 28 emu/g。在10k条件下,对1a ~ 1g粉末进行磁性研究表明,磁滞回线矫顽力高达950 Oe,剩磁量为10 emu/g,磁阻值为50.4 emu/g。此外,纳米级粉末的磁滞回线也发生了位移。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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