Using Mo-Ni-NH3 as impregnation solution,the penetrating mesoporous Mo-Ni-NH3/γ-Al2O3 catalyst was prepared by nano self-assembly technique.The influence of dosage of different surfactants such as CTAB, OP-20, TW-80, OP-10, assistantagentia TEA and NS on dispersity and pore structure of catalyst in the process of self-assembly was investigated by BET,in-situ FTIR of adsorbed CO,XRD and TEM.The results showed that the modified catalyst TOP-3 was better than the others,which has a specific surface area of 183m2?g-1,a pore volume of 0.46m3?g-1 and an average pore size of 10.11nm,and its pore distribution of 10nm-30nm was greatly concentrated, and reached up to 35.63%.The adsorption of active site of Mo2+,Mo4+ and Ni2+ was at the presence of linear adsorption state which could be proved by the in-situ FTIR of adsorbed CO.There were four characteristic crystal plane diffraction peaks of(111),(102),(021) and (312) for Al2(MoO4)3 at 15.9°,20.8°,22.2° and 30.8° by the XRD analysis for NOP-3 and NOP-4.While the fact that the characteristic peaks of TOP catalysts were dispersive showed that the composites of TEA and OP-20 improved the dispersity obviously.The penetrating mesoporous structures in uniform dispersion between 15nm and 20nm could be obtained by TEM images.The structure features were beneficial to residue hydrotreating.