Frank Anna, Grunwald Jan, Breitbach Benjamin, Scheu Christina
Max-Planck-Institut für Eisenforschung GmbH, Max-Planck-Straße 1, 40237 Düsseldorf, Germany.
Ludwig-Maximilians-Universität, Butenandtstraße 5-11, 81377 Munich, Germany.
Nanomaterials (Basel). 2018 Jun 5;8(6):405. doi: 10.3390/nano8060405.
This work demonstrates that the solvothermal synthesis of nanocrystalline CuInS₂ thin films using the amino acid l-cysteine as sulfur source is facile and robust against variation of reaction time and temperature. Synthesis was carried out in a reaction time range of 3⁻48 h (at 150 °C) and a reaction temperature range of 100⁻190 °C (for 18 h). It was found that at least a time of 6 h and a temperature of 140 °C is needed to produce pure nanocrystalline CuInS₂ thin films as proven by X-ray and electron diffraction, high-resolution transmission electron microscopy, and energy-dispersive X-ray spectroscopy. Using UV-vis spectroscopy, a good absorption behavior as well as direct band gaps between 1.46 and 1.55 eV have been determined for all grown films. Only for a reaction time of 3 h and temperatures below 140 °C CuInS₂ is not formed. This is attributed to the formation of metal ion complexes with l-cysteine and the overall slow assembly of CuInS₂. This study reveals that the reaction parameters can be chosen relatively free; the reaction is completely nontoxic and precursors and solvents are rather cheap, which makes this synthesis route interesting for industrial up scaling.
这项工作表明,以氨基酸L-半胱氨酸作为硫源,通过溶剂热法合成纳米晶CuInS₂薄膜简便易行,且对反应时间和温度的变化具有较强的耐受性。合成在3⁻48小时(150℃)的反应时间范围内以及100⁻190℃(18小时)的反应温度范围内进行。结果发现,通过X射线和电子衍射、高分辨率透射电子显微镜以及能量色散X射线光谱证实,至少需要6小时的时间和140℃的温度才能制备出纯的纳米晶CuInS₂薄膜。使用紫外-可见光谱法,已确定所有生长的薄膜都具有良好的吸收行为以及1.46至1.55 eV之间的直接带隙。仅在反应时间为3小时且温度低于140℃时,不会形成CuInS₂。这归因于金属离子与L-半胱氨酸形成络合物以及CuInS₂的整体缓慢组装。该研究表明,反应参数可以相对自由地选择;该反应完全无毒,且前驱体和溶剂相当便宜,这使得这种合成路线对于工业放大生产具有吸引力。