To get better materials for hydrogen isotope separation and evalute the feasibility of Pd/Al2O3 for TCAP (Thermal Cycling Absorption Process, TCAP), the properities of Pd/Al2O3 were tested by inductively coupled plasma (ICP) atomic emission spectrometer,automation surface area and pore size analyzer, field emission SEM and XRD instrument. And the hydrogen absorb-desorb performance of Pd/Al2O3 were also tested on the Sieverts device.The test results indict that the materials have better hydrogen absorbing-desorbing quality and have good fine resist performance on the palladium loading amount of 45.3% (wt%),