Synthesis of Cu2Mo6S8 powders and thin films from intermediate oxides prepared by polymeric precursor method

• Published in: Solid state sciences Vol. 14; no. 6; pp. 719 - 724
• Main Authors: Boursicot, S., Bouquet, V., Péron, I., Guizouarn, T., Potel, M., Guilloux-Viry, M.
• Format: Journal Article
• Language: English
• Published: Issy-les-Moulineaux Elsevier Masson SAS 01.06.2012; Elsevier Masson; Elsevier
• Subjects: CALCINATION; Chemical Sciences; Chevrel phases; Cross-disciplinary physics: materials science; rheology; CuxMo6S8; Exact sciences and technology; FABRICATION; Gas flow; Insertion material; Liquid phase epitaxy; deposition from liquid phases (melts, solutions, and surface layers on liquids); Material chemistry; Materials science; Methods of deposition of films and coatings; film growth and epitaxy; OXIDES; Physics; Polymeric precursors; POLYMERS; POWDERS; REDUCTION; SINGLE CRYSTALS; Sulfides; Sulfurization; Synthesis; THIN FILMS; Thin films; Sulfides; Chevrel phases; CuxMo6S8; Insertion material; Polymeric precursors; Liquid phase deposition; Calcium selenides; Mo; Multilayer; Molybdenum sulfide; Calcination; Hydrogen sulfides; Precursor; Heat treatments; Multilayers; Monocrystals; Cu; Sulfidation; S; Temperature effects; Sapphire; Copper sulfide; Spin-on coating; Sol-gel process
• ISSN: 1293-2558; 1873-3085
• DOI: 10.1016/j.solidstatesciences.2012.03.013

Powders and thin films of the copper molybdenum sulfide Cu2Mo6S8 were synthesized from intermediate oxides prepared by polymeric precursor method based on Pechini process. In the case of the thin films, deposition was performed onto R-plane sapphire single crystal by spin coating. The influence of temperature and duration of the 3 step heat treatment cycle (calcination, sulfurization and reduction) were investigated to optimize the synthesis conditions. The first step of calcination under air atmosphere performed for 3 h at 450 °C and 400 °C is suitable to obtain the intermediate oxides powders and thin films, respectively. The sulfurization treatment at 600 °C for 2 h under H2S/H2 gas flow followed by reduction at 650 °C for 4 h under H2 gas flow allowed to obtain Cu2Mo6S8 in powder or thin film form. In the last case, a multilayer process led to dense and homogeneous films. Moreover, the insertion and superconducting behaviour of the final powders allowed to validate the Cu2Mo6S8 synthesis by this moderate temperature process. [Display omitted]