FTIR study of unsupported molybdenum sulfide -: in situ synthesis and surface properties characterization

Self-supporting molybdenum sulfide samples with high surface area were prepared by in situ thermal decomposition in vacuum of ammonium thiomolybdate. BET specific surface area of the resulting material has its highest values of about 120 m(2)/g for samples treated in situ at 473 K and decreases on further beating, while the composition of samples treated at 423-473 K is close to MoS3, and after heating up to 573 K corresponds to MoS2. FTIR spectra show that precursor decomposition is almost completed already after treatment at 423 K, although the sample still contains admixed ammonium ions. After 473 K most of contaminations are gone. Spectra of adsorbed NH3, ND3, CO, SO2, CO2, COS and CH3SH adsorbed on samples pretreated at 423-473 K are very close to those obtained for air-contacted MoS2 powder. However higher band intensities and the use of labeled compound enabled us to identify the bands of coordinately bonded NH3 molecules and to point to the existence of acidic sites capable to protonate ammonia. Molecularly adsorbed CH3SH could be distinguished from its dissociative form; this reveals the existence of acid-base pair sites on bulk molybdenum sulfide. (C) 2004 Elsevier B.V. All rights reserved.