I am trying to synthesize MoS₂ nanomaterials via hydrothermal process following some of the previously reported procedures.
In detail, I dissolved 0.62 g of Sodium molybdate dihydrate and 1.14 g of thiourea in 60 mL of deionized water. Then, I transferred the chemical mixture to Teflon-lined stainless steel autoclave for 24 h at 180 ℃.
However, the weight yield of MoS₂ is very low (
perhaps some of sulfide hydrolyzed to oxide? You might check the supernatent solution. If ammonium molybdate is present in high amount, then indeed ammonium has also taken up a good amount of molybdenum species.
And also have a check on the fact that, since molybdenum form cations in aquous species, the Na-molybdate solution is likelt to be quite alkaline. Is it possible that this alkaline Molybdenum reacted with F of Teflon liner, since you heated it for too long? If not much gaseous product is not evolved, both ammonium ions from thiourea and Na from molybdate must have a counterion, be it hydroxide from water or floride from teflon. Teflon m.p. is around 270 degrees C, still, such cannot be ruled out- or may be nanoparticles themselved got embedded into liner!
All these are mre speculations. Test the solution yourself, find the ions (say by AAS/ Flame photometry) and then you can do causation.
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