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Systematic Investigation on Synthesis of CuInS 2 Powder and its Influencing Factors
Author(s) -
Liu Kegao,
Li Jing,
Xu Yong,
Shi Lei,
Gao Wencheng
Publication year - 2018
Publication title -
crystal research and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.377
H-Index - 64
eISSN - 1521-4079
pISSN - 0232-1300
DOI - 10.1002/crat.201700203
Subject(s) - hydrate , wurtzite crystal structure , hydrazine (antidepressant) , crystallinity , powder diffraction , materials science , scanning electron microscope , chemical engineering , solvent , crystal structure , nuclear chemistry , chemistry , inorganic chemistry , crystallography , zinc , organic chemistry , metallurgy , chromatography , composite material , engineering
CuInS 2 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 CuInS 2 powders. With CuC1 2 ·2H 2 O, InCl 3 and SC(NH 2 ) 2 as raw materials, the wurtzite CuInS 2 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 CuInS 2 . The wurtzite CuInS 2 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 CuInS 2 powder are at 160 °C for 20 h using CuC1 2 ·2H 2 O, InCl 3 and SC(NH 2 ) 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 CuInS 2 are more obvious, but the new impurity phase Cu 2 S appears at 220 °C. With holding time prolonging, it is helpful to eliminate the XRD peaks of impurity and promote chalcopyrite CuInS 2 formation. The optimum conditions for chalcopyrite CuInS 2 are reacting at 220 °C for 30 h with ethanol without hydrazine hydrate as solvent and CuC1 2 ·2H 2 O, InCl 3 and SC(NH 2 ) 2 as raw materials.