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Effect of synthesis parameters on structural and morphological properties of nanocrystalline bismuth phosphorus oxide materials

机译:合成参数对纳米晶氧化铋铋材料结构和形貌特性的影响

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摘要

Bismuth phosphorus oxide (BPO) has attracted much attention due to its various applications such as catalysts, photocatalysts, ionic conductors, and metal ion sensors. This material is usually produced via solid state reaction, hydrothermal synthesis, and ball milling which are associated with long reaction time, high synthesis temperature, and microsized products. Thus, an attempt was carried out in this research to synthesize nanocrystalline BPO using a relatively simple hot injection method at low reaction temperature. Bismuth acetate and calcium phosphide were used as precursors of bismuth and phosphorus, respectively. Phosphorus precursor reacted with 4 M hydrochloric acid (HCl) to generate phosphine (PH3) gas which later reacted with bismuth precursor in a mixture of 1-octadecene (ODE) and myristic acid (MA). Several parameters in synthesis condition including reaction temperature, type of reaction solvent, ratio of stabilizer (MA) to reaction solvent (ODE), amount of reaction solvent, reaction time, and ageing time were investigated. X-ray diffraction (XRD) results suggested that single phase BPO material with high crystallinity was obtained at reaction temperature 180°C with reaction time of 30 minutes and ratio of MA:ODE of 1:90. The XRD pattern of this material was best fitted with that of reported Bi3.69P0.31O6.31 (PDF 2010:43-0455), implying formation of face centered cubic (FCC) phase with lattice parameter a = 0.5416 nm. This FCC phase was in good agreement with transmission electron microscopy (TEM) analysis with average lattice fringes spacing of 0.337 nm. As evidenced, TEM and XRD results showed that particle size of the materials were in range of 10 to 20 nm. These materials are interesting as they have an ordered lamellar structure with both large meso and macro pores, indicating the formation of porous structure between the layers of BPO materials. In conclusion, nanocrystalline BPO was successfully synthesized via hot injection method for the first time.
机译:氧化铋磷(BPO)由于其在催化剂,光催化剂,离子导体和金属离子传感器等领域的各种应用而备受关注。这种材料通常是通过固态反应,水热合成和球磨生产的,这些反应需要较长的反应时间,较高的合成温度和微小的产物。因此,在本研究中尝试了使用相对简单的热注射方法在低反应温度下合成纳米晶BPO。乙酸铋和磷化钙分别用作铋和磷的前体。磷前驱物与4 M盐酸(HCl)反应生成膦(PH3)气体,然后在1-十八碳烯(ODE)和肉豆蔻酸(MA)的混合物中与铋前驱物反应。研究了合成条件中的几个参数,包括反应温度,反应溶剂类型,稳定剂(MA)与反应溶剂(ODE)的比例,反应溶剂的量,反应时间和老化时间。 X射线衍射(XRD)结果表明,在180℃的反应温度,30分钟的反应时间和1∶90的MA∶ODE比下,获得了具有高结晶度的单相BPO材料。该材料的XRD图谱与所报道的Bi3.69P0.31O6.31(PDF 2010:43-0455)的图谱最匹配,这意味着形成晶格参数a = 0.5416 nm的面心立方(FCC)相。此FCC相与透射电子显微镜(TEM)分析非常吻合,平均晶格条纹间距为0.337 nm。如所证明的,TEM和XRD结果表明材料的粒径在10至20nm的范围内。这些材料很有趣,因为它们具有带大的介孔和大孔的有序层状结构,表明在BPO材料层之间形成了多孔结构。总之,首次通过热注射法成功合成了纳米晶BPO。

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    Khairi Osman Hartini;

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  • 年度 2013
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