A conventional
hydrothermal reaction process was selected for the synthesis of WS2 nanostructures. The hydrothermal preparation of WS2 was noted to be highly sensitive to the reaction temperature. It
was reported that reaction temperatures below 240 °C cannot induce
the chemical reactions favorable for the formation of WS2.44 (link) So, a higher reaction temperature
of 265 °C was selected for the fabrication of WS2 nanostructures
in the present study. The hydrothermal process was carried out by
taking tungsten(VI) chloride (WCl6) and thioacetamide (TAA)
as primary precursors. A 1.1898 g portion of WCl6 and 1.1269
g of TAA were added to 40 mL of D-D water, and the solution was continuously
stirred for 30 min. The obtained solution was moved to a 50 mL PTFE-lined
autoclave and was subjected to heating at a temperature of 265 °C
for 24 h. After the hydrothermal reaction, a black precipitate was
collected. The precipitate was further filtered, washed, and dried
in a vacuum oven at 80 °C. The hydrothermal reaction process
for the formation of WS2 is represented by eqs 9 and 10.45 (link)
When TAA reacts with H2O,
H2S is released. The released H2S is a strong
reducing agent, and it acts as a source of sulfur. This H2S reduces WCl6 to form WS2 through sulfurization.