Many laboratories have researched membrane for gasification of coal technique, separating hydrogen from fossil fuel. In general, Pd membrane of separating hydrogen is very good a property of hydrogen selectivity on high temperature, but it has some problems, hydrogen embrittlement and costly material. So, we need some materials of good properties about hydrogen selectivity instead of Pd. In this research, we fabricate membrane for hydrogen permeation, that is great in resistance to acids and chemically steady TiN. Our laboratory investigated about hydrogen selectivity. TiN powder is milled 30, 60 and 240 minutes by vibration mill, respectively. After than the samples put in operate spark plasma sintering. We analyze XRD, SEM, BET and TG/DSC. Also, in this research take an inspect hydrogen selectivity by ourselves manufactured Sievert’s type hydrogen permeation membrane equipment.