A ZnO nanostructure having a high surface area was developed for use as a desulfurization sorbent. The ZnO nanostructure was prepared by using zinc acetate and activated carbon by the matrix-assisted method. Activated carbon was the matrix in the matrix-assisted method and zinc acetate was the precursor. The desulfurization tests of the ZnO nanostructure were carried out in a packed bed desulfurization system in the temperature range of 300-500 ℃. The ZnO nanostructures before and after the sulfidation process were characterized by BET, XRD and SEM. The formulated ZnO nanostructure consisted of ZnO nanoparticles with a size of 10-20 nm and its surface area was very high. Therefore, the sulfur capture efficiency of the ZnO nanostructure was 3 times higher than that of commercial ZnO. However, a reduction of some of the ZnO occurred because of the reducibility of the coal-derived gas, and the surface area of the ZnO nanostructure was slightly reduced due to the sintering of ZnO. It was also confirmed that the silica and alumina containing activated carbon used as the matrix prevent the thermal sintering of ZnO in the sulfidation process at high temperature.