Electrochemical synthesis of nanocrystalline In2O3:Sn (ITO) in an aqueous system with ammonium acetate as conducting salt.
Nanoscaled so called indium tin oxide In2O3:Sn (ITO) with a specific BET surface area of 50 m2/g to 60 m2/g was prepared via an electrochemical method in an aqueous system containing ammonium acetate as conductive salt. As an intermediate product of the synthesis nanocrystalline In(OH)3 is obtained which serves as a precursor for the subsequent calcinations accompanied by tin doping resulting in ITO powders with various tin concentrations. Its phase transitions and the reduction behaviour of hydroxide to oxide during the calcination process in air flow and forming gas atmosphere of N2 to H2 ratio of 95 to 5 respectively, have been investigated by high temperature X-ray diffraction, TG/DSC/MS, HRTEM and SEM analysis. Depending on the atmosphere dehydration of tin doped In(OH)3 started at 150 degrees C, cubic ITO solid solution formed between 190 degrees C and 300 degrees C. The total weight loss of the hydroxide of approx. 21% occurred mainly below 360 degrees C and the burn-out of organic components mainly between 308 degrees C and 316 degrees C. The results of DSC and MS analyses were in good agreement with the results of the X-ray diffraction. In addition, the products have been characterized by EDX associated with TEM, XPS, ICP-AES, BET analysis and 119Sn Mössbauer spectroscopy. Completely reacted samples of ITO have been processed to pellets, calcined and sintered in the temperature range between 900 degrees C and 1100 degrees C and characterized by measurements of the electrical conductivities of bulk and surface in the reduced as well as in the oxidized state giving values up to 1400 Scm(-1).
INM-Leibniz Institute for New Materials, Campus D2 2, D-66123 Saarbrücken, Germany.
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Veith
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Rabung
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Grobelsek
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Klook
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Wagner
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