Preparat ion o f no ble met al (NM) (Rh, Pd, Ru, Pt) phosphide species and t heir cat alyt ic act ivit ies for hydrodesulfur izat ion (HDS) of t hiophene w er e invest igat ed. Noble met al phosphides (NM X P Y) cat alyst s were prepared by reduct ion o f Padded NM (NM-P) support ed on silica (S iO 2) wit h hydrogen. Hydrogen co nsumpt io n peaks at around 350−700 °C, which wer e at t ribut ed t o t he for mat io n o f NM X P Y , were obser ved in t emper at ure-programmed reduct io n (TPR) spect ra of al l NM-P/S iO 2. Furt her more, X-ray diffr act ion (XRD) pat t erns o f NM-P/S iO 2 indicat e t hat NM X P Y (Rh 2 P, Pd 4. 8 P, Ru 2 P, Pt P 2) were for med by hydrogen reduct ion at high t emperat ure. The reduct ion t emperat ure st rongly affect ed HDS act ivit ies o f NM-P/S iO 2 cat alyst s. The NM-P/S iO 2 cat alyst s, ot her t han Pt , showed higher HDS act ivit ies t han NM/S iO 2 cat alyst s. The HDS act ivit y o f t he Rh-P/S iO 2 cat alyst was t he highest amo ng t hose o f NM-P/S iO 2 cat alyst s. This act ivit y was higher than that of the NiP catalyst and was t he same as t hat of pre-sulfided CoMoP/Al 2 O 3 cat alyst. Furt her more, t he Rh-P/S iO 2 cat alyst showed st able act ivit y even aft er react ion for 30 h. The XRD, t ransmiss io n elect ron microscopy (TEM), and energy disper sive X-ray spect roscopy (EDS) result s revealed t hat t he for mat io n o f sma ll Rh 2 P part icles and suit able P addit io n t o for m Rh 2 P caused t he high HDS act ivit y o f t he Rh-P cat alyst .