Hydrogen separation membranes are important for the purification of hydrogen for use in the production of chemicals the refining of petroleum and in energy conversion devices such as fuel cells. Among the best membranes are palladium membranes but these are susceptible to poisoning by sulfur. Sulfur is a common contaminant in feedstocks for hydrogen production such as natural gas and petroleum products coal and some biomass sources. This invention provides materials and methods of preparation of sulfur-tolerant membranes based on palladium or palladium alloys. The compositions consist of the palladium or palladium alloys combined with phosphorus to form phosphides. The method consists of treatment of the metal precursor with a phosphorous source such as phosphine. Applications: 1) Fuel cells 2) Petroleum refining
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