Thermal behaviour of precursors for CuInS2 thin films deposited by spray pyrolysis

• Published in: Journal of thermal analysis and calorimetry Vol. 113; no. 3; pp. 1455 - 1465
• Main Authors: Oja Acik, I., Otto, K., Krunks, M., Tõnsuaadu, K., Mere, A.
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Dordrecht Springer Netherlands 01.09.2013; Springer
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; CHLORIDES; COPPER INDIUM SULFIDE; COPPER OXIDE; Cross-disciplinary physics: materials science; rheology; DECOMPOSITION; DIFFERENTIAL THERMAL ANALYSIS; Exact sciences and technology; Fourier transforms; Indium; Indium oxides; Inorganic Chemistry; Materials science; Measurement Science and Instrumentation; Other topics in materials science; OXIDES; Physical Chemistry; Physics; Polymer Sciences; Precursors; Spectroscopy; SPRAYING; Thermal decomposition; THIN FILMS; Thioureas; Copper indium disulphide; Simultaneous thermogravimetry (TG) and differential thermal analysis (DTA); ex situ FTIR and XRD; Thiourea; Chemical spray pyrolysis; Mass spectroscopy (MS); Evolved gas analysis (EGA); Infrared spectroscopy; Fourier transformation; Spray pyrolysis; Gas release; Gas analysis; XRD; Precursor; Characterization; Thin films; Indium Chlorides; Indium Sulfides; Chalcopyrite structure; Evolved gas analysis; Copper Chlorides; Ternary compounds; Thermogravimetry; Mass spectroscopy; Differential thermal analysis; Copper Indium Sulfides; Transition elements; Thermal analysis; Copper Sulfides
• ISSN: 1388-6150; 1588-2926; 1572-8943
• DOI: 10.1007/s10973-013-3155-7

The thermal decomposition of precursors for copper indium disulphide (CuInS 2 ) thin films obtained by drying aqueous solutions of copper chloride (CuCl 2 ), indium chloride (InCl 3 ) and thiourea (SC(NH 2 ) 2 ) at the Cu:In:S molar ratios of 1:1:3 ( 1 ) and 1:1:6 ( 2 ) was monitored by simultaneous thermogravimetry /differential thermal analysis/ evolved gas analysis-mass spectrometry (TG/DTA/EGA-MS) measurements in a dynamic 80 %Ar + 20 %O 2 atmosphere. X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy were used to characterise the dried precursors and products of the thermal decomposition. The precursors 1 and 2 are mixtures of copper and indium chloride thiourea complex compounds, whilst 1 can also contain unreacted InCl 3 . The thermal degradation of 1 and 2 in the temperature range of 30–800 °C consists of six steps with a total mass loss of 71.5 and 89.8 %, respectively. According to XRD, CuInS 2 is formed below 300 °C. Decomposition of 1 and 2 is completed at 620 and 600 °C, respectively. The final decomposition product of 1 at 800 °C consists of a mixture of In 2 O 3 and CuO phases, whilst 2 consists of In 2 O 3 , CuO and Cu 2 In 2 O 5 phases. EGA by MS revealed the release of CS 2 , NH 3 , H 2 NCN and HNCS, which upon their oxidation also yield COS, SO 2 , HCN and CO 2 .