The thermal decomposition of ammonium tetrathiotungstate (ATT), (NH 4 ) 2 WS 4 was studied by SEM, FTIR, XRD, EDX and TG/DTA-MS. The decomposition of ATT involved three steps in inert atmosphere: (i) release of free water between 30-140 °C; (ii) formation of an amorphous WS 3 phase between 170-280 °C, from which (iii) a slightly crystalline WS 2 formed between 330-470 °C. As a difference compared to inert atmosphere, in air in the second step the ATT decomposed into directly WS 2 instead of WS 3 . This WS 2 phase was amorphous, and still contained traces of ATT. Between 260-2 500 °C from the WS 2 monoclinic tungsten oxide crystallized in two steps: at 302 °C a slightly crystalline m-WO 3 formed, which became more crystalline at 471 °C. During the investigation of the effect of the particle size, it was found that the thermal behaviour of ATT crystals was similar to ATT powder, with some shift in the decomposition temperature. The XRD results showed that the WS 2 formed from the ATT powder in N 2 had a higher level of crystallization, compared to the WS 2 obtained from ATT crystals.

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