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Synthesis, structural and spectroscopic characterizations of maghemite gamma-Fe2O3 prepared by one-step coprecipitation route

机译:一步共沉淀法制备磁赤铁矿γ-Fe2O3的合成,结构和光谱表征

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摘要

Maghemite (gamma-Fe2O3) is synthesized by one step coprecipitation method from mixed salt solutions containing Fe(II) and Fe(III) salts. This material was characterized using Rietveld refinement of the X-ray powder diffraction, heating stage Raman microscopy and Mossbauer spectroscopies. The Rietveld refinement of XRD pattern has indicated that the gamma-Fe2O3 shows a cubic cell structure. The superstructure reflection related to the long-range ordering of cation lattice vacancies was not detected in the diffraction pattern. The extra peaks corresponding to the Lepidocrocite phase gamma FeOOH in a small amount were observed in the XRD pattern. The crystallite size of maghemite compound is 18 nm calculated using Williamson-Hall method. Using Mossbauer spectroscopy, the result of Rietveld refinement was confirmed by the presence of magnetic sextet arising from the metallic iron of gamma-Fe2O3, and a paramagnetic doublet inferring the presence of paramagnetic iron of gamma FeOOH. Heating stage Raman microscopy reveals that the temperature of transition to maghemite phase up to hematite is 550 degrees C. The heating of our maghemite (gamma-Fe2O3) powder up to 550 degrees C yields a single phase of Hematite hexagonal-corundum structure with R (3) over barc space group. (C) 2015 Elsevier B.V. All rights reserved.
机译:磁赤铁矿(γ-Fe2O3)是通过一步共沉淀法从含有Fe(II)和Fe(III)盐的混合盐溶液中合成的。使用Rietveld精制的X射线粉末衍射,加热台拉曼显微镜和Mossbauer光谱对这种材料进行表征。 XRD图的Rietveld精炼表明,γ-Fe2O3显示出立方晶胞结构。在衍射图中未检测到与阳离子晶格空位的远距离有序相关的上部结构反射。在XRD图谱中观察到少量对应于纤铁矿相γFeOOH的额外峰。磁赤铁矿化合物的微晶尺寸为18纳米,采用Williamson-Hall方法计算。使用Mossbauer光谱,通过γ-Fe2O3的金属铁和顺磁性双线态推断出γFeOOH的顺磁性铁的存在,确定了六联体的存在,从而证实了Rietveld精制的结果。加热阶段拉曼显微镜显示,到赤铁矿转变成磁赤铁矿相的温度为550摄氏度。我们的磁赤铁矿(γ-Fe2O3)粉末加热到550摄氏度,产生的单相赤铁矿六方刚玉结构具有R( 3)超过巴克空间组。 (C)2015 Elsevier B.V.保留所有权利。

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