Pd/Si-MFI membranes are fabricated by depositing palladium nanoparticles onto Si-MFI membranes via opposing reactants chemical fluid deposition in supercritical carbon dioxide. Palladium hexafluoroacetylacetonate [Pd(hfac)(2)] and ethanol are used as the Pd precursor and the reducing agent, respectively, in the deposition process. The resulting Pd/Si-MFI membrane is characterized using SEM, XRD, EPMA, TEM, and EDX techniques. It is demonstrated that a continuous layer of Pd particles with size of 10 nm is covered on the matrix surface while 30-nm Pd particles are plugged into the defects within the matrix. The H-2/N-2 permselectivity has been significantly increased due to the deposition of Pd nanoparticles in the Si-MFI membrane, which could keep stable below the critical temperature. This bifunctional membrane and similar membranes possess the application potential to achieve various one-step syntheses.