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Preparation and characterization of LiFe_(1/2)Ni_(1/2)VO_4

机译:LiFe_(1/2)Ni_(1/2)VO_4的制备与表征

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A layered ceramic oxide, LiFe_(1/2)Ni_(1/2)VO_4 has been prepared using solid-state reaction technique. The preparation conditions have been optimized using thermogravimmetric analysis (TGA) studies. The formation of the material sample under the reported condition has been confirmed by X-ray diffraction (XRD) analysis. XRD analysis indicates the crystal structure to be orthorhombic with lattice parameter: a = 3.5637 A, b= 17.7486 A, c = 12.2884 A. The phase morphology and surface properties studied using scanning electron microscopy (SEM), suggest a polycrystalline texture with reasonable number of the voids. Complex impedance analysis of the sample has indicated: (ⅰ) conduction due to bulk contribution at T ≤ 200℃, (ⅱ) the presence of grain boundary effects at T ≥ 200℃, (ⅲ) negative temperature coefficient of resistance (NTCR) behaviour and (ⅳ) evidence of temperature dependent electrical relaxation phenomena in the sample. The DC conductivity (σ_(DC)) shows typical Arrhenius behaviour when observed as a function of the temperature. The activation energy value has been estimated to be 0.42 eV. σ_(DC), as evaluated from complex impedance spectrum, shows a jump of nearly ~4 orders of magnitude in the value at higher temperature when compared to that of the room temperature value. AC conductivity spectrum obeys Jonscher's universal power law. The results of σ_(AC) as a function of frequency are also discussed.
机译:使用固态反应技术已经制备了层状陶瓷氧化物LiFe_(1/2)Ni_(1/2)VO_4。使用热重分析(TGA)研究已经优化了制备条件。通过X射线衍射(XRD)分析已确认在报告的条件下材料样品的形成。 X射线衍射分析表明晶体结构为正交晶,晶格参数为:a = 3.5637 A,b = 17.7486 A,c = 12.2884A。使用扫描电子显微镜(SEM)研究的相形貌和表面性质表明具有合理数量的多晶织构的空隙。样品的复阻抗分析表明:(ⅰ)在T≤200℃时由于体积贡献而导通,(ⅱ)在T≥200℃时存在晶界效应,(ⅲ)负温度系数电阻(NTCR)行为(ⅳ)样品中取决于温度的电弛豫现象的证据。当观察到作为温度的函数时,直流电导率(σ_(DC))显示出典型的阿累尼乌斯行为。活化能值估计为0.42 eV。根据复阻抗谱评估,σ_(DC)与室温值相比,在较高温度下的值显示了近〜4个数量级的跃变。交流电导率频谱符合Jonscher的通用功率定律。还讨论了σ_(AC)作为频率的函数的结果。

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