Synthesis of finely divided molybdenum sulfide nanoparticles in propylene carbonate solution

Journal Article · Thu May 01 00:00:00 EDT 2014 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2014.02.030· OSTI ID:22334215

Afanasiev, Pavel

Molybdenum sulfide nanoparticles have been prepared from the reflux solution reaction involving ammonium heptamolybdate and elemental sulfur in propylene carbonate. Addition to the reaction mixture of starch as a natural capping agent leads to lesser agglomeration and smaller size of the particles. Nanoparticles of MoS{sub x} (x≈4) of 10–30 nm size are highly divided and form stable colloidal suspensions in organic solvents. Mo K edge EXAFS of the amorphous materials shows rapid exchange of oxygen to sulfur in the molybdenum coordination sphere during the solution reaction. Thermal treatment of the amorphous sulfides MoS{sub x} under nitrogen or hydrogen flow at 400 °C allows obtaining mesoporous MoS{sub 2} materials with very high pore volume and specific surface area, up to 0.45 cm{sup 3}/g and 190 m{sup 2}/g, respectively. The new materials show good potential for the application as unsupported hydrotreating catalysts. - Graphical abstract: Solution reaction in propylene carbonate allows preparing weakly agglomerated molybdenum sulfide with particle size 20 nm and advantageous catalytic properties. - Highlights: • Solution reaction in propylene carbonate yields MoS{sub x} particles near 20 nm size. • Addition of starch as capping agent reduces particles size and hinder agglomeration. • EXAFS at Mo K edge shows rapid oxygen to sulfur exchange in the solution. • Thermal treatment leads to MoS{sub 2} with very high porosity and surface area.

• OSTI ID: 22334215
• Journal Information: Journal of Solid State Chemistry, Vol. 213; Other Information: Copyright (c) 2014 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
77 NANOSCIENCE AND NANOTECHNOLOGY
ABSORPTION SPECTROSCOPY
AGGLOMERATION
CATALYSTS
FINE STRUCTURE
HEAT TREATMENTS
HYDROGEN
MOLYBDENUM
MOLYBDENUM SULFIDES
NANOPARTICLES
NANOSTRUCTURES
ORGANIC SOLVENTS
OXYGEN
PARTICLE SIZE
POROSITY
SILICON OXIDES
SOLUTIONS
SURFACE AREA
SYNTHESIS
X-RAY SPECTROSCOPY