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Reaction Tailoring for Synthesis of Phase‐Pure Nanocrystals of AgInSe2, Cu3SbSe3 and CuSbSe2
ChemistrySelect ( IF 2.1 ) Pub Date : 2018-03-13 , DOI: 10.1002/slct.201702986
Anuraj S. Kshirsagar 1 , Pawan. K. Khanna 1
Affiliation  

Present article highlights synthesis of phase pure I, III, VI2 and I, V, VI2 ternary selenides nanocrystals (NCs) using oleic acid and oleyl amine capping agents. The synthesis of AgInSe2 (AISe), Cu3SbSe3 and CuSbSe2 (CSSe) NCs was executed by employing cyclohexeno‐1,2,3‐selenadiazole (SDZ) as Se precursor. The current study is the first report describing use of thermally labile organoselenium compound for the synthesis of such technologically important ternary selenide NCs. Systematic study of the formation of AISe and CSSe NCs at different reaction time is carried out in order to confirm phase purity and stoichiometry. The spherical, stoichiometric and NIR active semiconductors showed formation of orthorhombic crystal structure as confirmed from XRD analysis. It was observed that formation of phase pure AISe NCs requires 5 hours (h) of constant heating at about 220οC irrespective of the capping agents however, CuSbSe2 was obtained within an hour in presence of oleyl amine at same reaction temperature. Nanocrystals were characterized by different analytical tools such as UV‐Visible spectroscopy, FTIR, XRD, SEM/EDS, TEM, particle size and XPS analysis. Based on the results, possible chemical reaction pathway for ternary chalcogenide is presented.

中文翻译:

AgInSe2,Cu3SbSe3和CuSbSe2相纯纳米晶体的反应定制

本文重点介绍了使用油酸和油胺封端剂合成相纯的I,III,VI 2和I,V,VI 2三价硒纳米晶体(NC)。AgInSe 2(AISe),Cu 3 SbSe 3和CuSbSe 2的合成(CSSe)NCs是通过使用环己烯-1,2,3-硒代二唑(SDZ)作为Se前体来执行的。当前的研究是描述使用热不稳定的有机硒化合物合成这种技术上重要的三价硒化NC的第一份报告。为了确定相纯度和化学计量,对系统在不同反应时间形成AISe和CSSe NCs进行了系统研究。球形,化学计量和NIR活性半导体显示出正交晶体结构的形成,这已通过XRD分析得到了证实。据观察,形成纯相AISE NC的需要不断加热5小时(h)在约220 ο Ç不论封端剂的然而,CuSbSe 2在相同的反应温度下,在油胺存在下,在一小时内获得 纳米晶体通过不同的分析工具进行表征,例如紫外可见光谱,FTIR,XRD,SEM / EDS,TEM,粒度和XPS分析。根据结果​​,提出了三元硫属元素化物可能的化学反应途径。
更新日期:2018-03-13
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