Investigations of solvents and various sulfur sources influence on the shape-controlled synthesis of CuInS2 nanocrystals
Investigations of solvents and various sulfur sources influence on the shape-controlled synthesis of CuInS2 nanocrystals
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DOI：
10.1007/s11051-011-0381-4
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发表时间：
2011-05
影响因子：
2.5
通讯作者：
M. Kruszyńska;H. Borchert;J. Parisi;J. Kolny-Olesiak
中科院分区：
文献类型：
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作者：
M. Kruszyńska;H. Borchert;J. Parisi;J. Kolny-Olesiak
采用热注入法，以叔十二烷基硫醇为硫源，三辛基氧化膦和正十二烷基硫醇为配体，以乙酸铜（I）和乙酸铟（III）为原料，成功合成了CuInS 2（CIS）纳米晶.反应介质是两种溶剂的混合物：油胺和1-十八烯。改变这两种溶剂之间的比例导致纤锌矿CuInS 2颗粒的形成，其形状从三角形到棒状，长度可达50 nm。油胺以两种相反的方式影响反应条件：在注入硫前体之前导致单体耗尽，同时增加溶液中剩余单体的活性。通过将硫源由叔十二烷基硫醇改为油胺硫，合成了具有锌共混结构的三角形颗粒，粒径较小（约5 nm）。采用X射线粉末衍射（XRD）、透射电子显微镜（TEM）、X射线能量色散分析（EDX）和紫外-可见吸收光谱（UV-Vis）对材料进行了表征。
CuInS2(CIS) nanocrystals were successfully synthesized through a hot-injection technique employing a reaction of copper (I) acetate and indium (III) acetate withtert-dodecanethiol as a source of sulfur, and trioctylphosphine oxide and 1-dodecanethiol were used as ligands. The reaction medium was a mixture of two solvents: oleylamine and 1-octadecene. Varying the ratio between both solvents leads to the formation of wurtzite CuInS2particles with shapes ranging from triangular to rod-shaped with length up to 50 nm. Oleylamine turned out to influence the reaction condition in two opposite ways: by leading to monomer depletion before the injection of the sulfur precursor, and at the same time increasing the activity of the monomers remaining in solution. By changing the sulfur source fromtert-dodecanethiol to sulfur dissolved in oleylamine, triangular particles with zinc blend structure and a smaller size (~5 nm) were synthesized. The final materials were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDX), and absorption spectroscopy (UV–Vis).