溶胶-凝胶法制备amoo4 (A= Co 2+和Mn 2+)纳米粉体的Rietveld细化、形貌分析、电子、磁性、光学和光催化性能

H. Lakhlifi, Y. El Jabbar, A. Natik, M. Benchikhi, H. Lassri, L. Er-Rakho, R. El Ouatib
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摘要

采用溶胶-凝胶法制备了钼基二元氧化物AMoO4 (A= Co2+和Mn2+)。采用热分析(TGA/DTA)、x射线衍射(XRD)和Rietveld细化数据对制备的纳米粉体进行了表征。硝酸钴(G1凝胶)粉末的扫描电镜(SEM)显示多孔团聚体形成笼状结构,这些笼状结构是分阶段脱气形成的。同时,用氯化钴(G2凝胶)制备的粉末进行了预烧结。钼酸CoMoO4的透射电镜(TEM)显示为准球形颗粒,纳米尺寸范围为10 ~ 60 nm。拉曼光谱显示了O-Metal、Metal-O-Metal和O-Metal- o三种振动模式的存在,证实了所需相的形成。基于光学带隙能量(Eg=1.98 eV),单斜斜b-MnMoO4是一种半导体材料。b-MnMoO4样品的理论磁矩近似为μ理论= 5.00049 μB。以钼酸钴(CoMoO4)为光催化剂,研究了靛蓝染料的光催化降解过程,并对该过程进行了紫外-可见吸收光谱分析。紫外光照射下的光催化活性测试表明,125 min后变色效率为45%,H2O2的加入使这一率提高到74%。
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Rietveld Refinement, Morphology Analysis, Electronic, Magnetic, Optical and Photocatalytic Performance of AMoO 4 (A= Co 2+ and Mn 2+) Nanopowders Synthesized by Sol-Gel Method
Molybdenum-based binary oxides AMoO4 (A= Co2+ and Mn2+) have been successfully synthesized using the sol-gel method. The prepared nanopowders were characterized by means of thermal analysis (TGA/DTA), X-ray diffraction (XRD) and Rietveld refinement data. Scanning electron microscope (SEM) of the powders obtained from cobalt nitrate (G1 gel) showed porous agglomerate that formed cages, which came from the degassing in several stages. Meanwhile, pre-sintering was observed in the powders obtained from cobalt chloride (G2 gel). The transmission electron microscopy (TEM) of CoMoO4 molybdate showed quasi-spherical particles with nanometric size range of 10-60 nm. Raman spectroscopy revealed the presence of the vibrational modes O-Metal, Metal-O-Metal, and O-Metal-O, which confirm the formation of the desired phase. Based on the optical band-gap energy (Eg=1.98 eV), the monoclinic b-MnMoO4 is a semiconductor material. The theoretical magnetic moment of the b-MnMoO4 sample is approximately μtheorical = 5.00049 μB. The photocatalytic degradation process of Indigo dye was investigated using cobalt molybdate (CoMoO4) as a photocatalyst, this process was followed by UV–vis absorption spectroscopy analyzes. The photocatalytic activity tests under UV light irradiation show a 45% of discoloration efficiency after 125 min. The addition of H2O2 increases this rate to 74 %.
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