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Phase-Pure Copper Vanadate (α-CuV2O6): Solution Combustion Synthesis and Characterization
Chemistry of Materials ( IF 7.2 ) Pub Date : 2020-06-26 , DOI: 10.1021/acs.chemmater.0c02227
Mohammad Kabir Hossain 1 , Hori Pada Sarker 2 , Paola Sotelo 1 , Uyen Dang 1 , Ingrid Rodríguez-Gutiérrez 3 , Joanna Blawat 4 , Abbas Vali 1 , Weiwei Xie 4 , Gerko Oskam 3, 5 , Muhammad N. Huda 2 , Robin T. Macaluso 1 , Krishnan Rajeshwar 1
Affiliation  

This study addresses a perennial problem in the synthesis of copper vanadates, namely, that of phase purity. A time-efficient solution combustion synthesis (SCS) was employed for obtaining α-CuV2O6 in a polycrystalline powder form in a matter of minutes. Admixture of the final product with α-Cu2V2O7 or V2O5 was avoided by a combination of careful pH control of the SCS precursor mixture and by a postsynthesis NaOH wash. The phase purity of the resultant product was demonstrated by Rietveld refinement of the X-ray diffraction data, energy-dispersive X-ray analyses, and laser Raman spectroscopy. Photoelectrochemical (PEC) measurements showed the material to be an n-type semiconductor. Possible applicability of α-CuV2O6 in PEC devices designed for solar water splitting hinges on a comprehensive study of its structural, optical, magnetic, and optoelectronic attributes; this was done by a combination of theory and experiment. Intensity-modulated photocurrent spectroscopy on thin film samples permitted an assessment of the balance between charge transfer and surface recombination, underlining that the charge separation efficiency determined the photocurrent magnitude. Finally, experiments on the PEC stability of this material on prolonged (∼4 h) irradiation revealed self-healing behavior induced by incipient photocorrosion product layer formation on the oxide semiconductor surface.

中文翻译:

相纯钒酸铜(α-CUV 2 ö 6):溶液燃烧合成和表征

这项研究解决了钒酸铜合成中的一个常年问题,即相纯度问题。甲时间高效的解决方案的燃烧合成(SCS)被用于获得α-CUV 2 ö 6在几分钟之内就在多晶粉末形式。最终产物的混合物与α-Cu系2 V 2 ö 7或V 2 ø 5通过小心控制SCS前体混合物的pH值和通过合成后的NaOH洗涤可以避免这种情况。通过X射线衍射数据的Rietveld精炼,能量色散X射线分析和激光拉曼光谱证明了所得产物的相纯度。光电化学(PEC)测量表明该材料是n型半导体。的可能的应用性α-CUV 2 ö 6在设计用于太阳能分水铰链的PEC设备中,对它的结构,光学,磁性和光电属性进行了全面研究;这是通过理论和实验相结合来完成的。通过对薄膜样品进行强度调制的光电流光谱学,可以评估电荷转移和表面复合之间的平衡,从而强调电荷分离效率决定了光电流的大小。最后,对这种材料在长时间(〜4 h)辐照下的PEC稳定性进行的实验表明,氧化物半导体表面上形成的初始光腐蚀产物层会引起自修复行为。
更新日期:2020-07-28
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