Ni 8 wt.%-doped tin oxide (SnO2) thick films were fabricated into gas sensors by the method of screen printing onto alumina substrates. The particle size of SnO2 was controlled by changing the ball-mill time between 0~120 h. The structural and morphological properties of these thick films were investigated using X-ray diffraction and scanning electron microscopy. The structural properties of SnO2 powders showed a tetragonal phase with (110) dominant orientation. The particle size of the SnO2:Ni powders after ball-mill of 120 h was about 0.05 μm. The gas sensitivity (S = Rg/Ra) to 5 ppm CH4 gas and CH3CH2CH3 gas was measured at room temperature by comparing the resistance in air (Ra) with that of the target gases (Rg). The sensitivity of the SnO2 gas sensors was enhanced by increasing the ball-mill time. There was an association between the sensitivity of both the CH4 gas and the CH3CH2CH3 gas and the particle size of the SnO2. SnO2 gas sensors prepared by 72 h ball-mill showed a sensitivity of about 13 to 5 ppm CH4 gas and CH3CH2CH3 gas. The response time of the SnO2:Ni gas sensors to the CH4 gas was about 20 seconds.