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Supercritical hydrothermal synthesis of polycrystalline gadolinium aluminum perovskite materials (GdAlO3, GAP)

机译:超临界水热法合成多晶g钙钛矿材料(GdAlO3,GAP)

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摘要

The orthorhombic perovskite, Gadolinium aluminum oxide (GdAlO3, GAP) material was successfully prepared by hydrothermal supercritical fluid method using co-precipitated gel of GAP. All experiments were carried out in the pressure and temperature ranges of 100–150 MPa and 180–650 °C respectively. The as-prepared GAP samples were systematically characterized by X-ray diffractionud(XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), X-ray spectroscopy (EDS), thermo gravimetry (TGA) and differential thermo gravimetry analysis (DTA). The XRD profile confirms fully crystalline and orthorhombic nature of as-prepared materials, which is well correlated to the reported results. The SEM studies reveal that the GAP materials synthesized at 650 °C/150 MPa for 92 hrs possesses polycrystalline nature with average particle size in the range of 5–20 μm. The DTA shows a crystallization peak at 361 °C at this temperature the agglomerated GAP gel starts to crystallize into polycrystalline GAP materials. When compared with other methods, like sol-gel and solid-state reactions our crystallization temperature is very much lower and feasible. This work not only demonstrates a simple way to fabricate GAP polycrystalline materials from co-precipitated gels but also shows a possible utilization of same technique for synthesis of other high temperature materials.
机译:采用共沉淀GAP水热超临界流体法成功制备了正交晶钙钛矿,氧化铝(GdAlO3,GAP)材料。所有实验分别在100-150 MPa和180-650°C的压力和温度范围内进行。通过X射线衍射 ud(XRD),扫描电子显微镜(SEM),傅立叶变换红外光谱(FT-IR),X射线光谱(EDS),热重量分析(TGA)对制得的GAP样品进行了系统表征和差示热重分析(DTA)。 XRD图谱证实了所制备材料的完全结晶和正交晶的性质,这与报道的结果很好相关。 SEM研究表明,在650°C / 150 MPa下合成92个小时的GAP材料具有多晶性质,平均粒径在5–20μm范围内。 DTA在此温度下在361°C处显示结晶峰,凝聚的GAP凝胶开始结晶为多晶GAP材料。与其他方法(例如溶胶-凝胶和固态反应)相比,我们的结晶温度要低得多并且可行。这项工作不仅证明了从共沉淀凝胶制备GAP多晶材料的简单方法,而且还表明了利用相同技术合成其他高温材料的可能方法。

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