The in situ decomposition of ammonium thiometallates during the hydrod
esulfurization (HDS) of dibenzothiophene (DBT), to obtain molybdenum d
isulfide and tungsten disulfide catalysts, was investigated. It was fo
und that very efficient catalysts for the HDS of DBT were obtained by
in situ decomposition. Mechanical uniaxial pressing of the precursors
(ammonium thiometallates) affected both textural and catalytic propert
ies of the catalysts. Surface areas of molybdenum and tungsten disulfi
des increased as a function of uniaxial pressing, while catalytic acti
vities went through a maximum. For MoS2, the hydrogenation selectivity
was much higher for in situ catalysts than for ex situ ones. For WS2
catalysts, the hydrogenation selectivity was less sensitive to the con
dition of decomposition (ex situ/in situ). The surface S/M (M = Mo, W)
atomic ratio from the Auger signal decreased as a function of uniaxia
l pressing, while the CIM ratio remained almost constant at 1.6. The b
est catalyst showed an experimental S/Mo ratio that is slightly higher
than the stoichiometric value. The effect of ill situ decomposition a
nd mechanical deformation of thiometallate precursors is discussed.