Abstract
AbstractCuInS2 powders were prepared by solvothermal method. The effects of experimental conditions on crystal structure, composition phase and morphology were investigated systematically. The phases of product samples were analyzed by X‐ray diffraction (XRD) on the Bruker D8 Advance XRD system with Nifiltered Cu‐Kα (λ = 1.5059 Å). The morphology of the product powders were observed using scanning electron microscope (SEM) with a model of JSM‐6380LA made by Japan Electronics Co., Ltd. The elemental compositions of the product powders were analyzed by energy dispersive spectroscopy (EDS). The results show that, different solvents have important effects on the crystal structures of CuInS2 powders. With CuC12·2H2O, InCl3 and SC(NH2)2 as raw materials, the wurtzite CuInS2 obtained with the mixed solvent of ethanol and hydrazine hydrate has better crystallinity than that obtained by the mixed solvent of ethylene glycol and hydrazine hydrate. The product powder obtained with ethanol without hydrazine hydrate has major phase chalcopyrite CuInS2. The wurtzite CuInS2 powder consists of aggregated particles with diameters of 0.1 ∼ 0.5 μm. The sample with chalcopyrite has relatively more large particles with diameters of 3 ∼ 5 μm which consist of smaller flakes. The optimum conditions for preparing wurtzite CuInS2 powder are at 160 °C for 20 h using CuC12·2H2O, InCl3 and SC(NH2)2 as raw materials and the mixed solution of ethanol and hydrazine hydrate as solvent. With the increase of reaction temperature, the XRD peaks of chalcopyrite CuInS2 are more obvious, but the new impurity phase Cu2S appears at 220 °C. With holding time prolonging, it is helpful to eliminate the XRD peaks of impurity and promote chalcopyrite CuInS2 formation. The optimum conditions for chalcopyrite CuInS2 are reacting at 220 °C for 30 h with ethanol without hydrazine hydrate as solvent and CuC12·2H2O, InCl3 and SC(NH2)2 as raw materials.
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