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A new concept of crystalline phase embedded in amorphous matrix is proposed as solid permeable material for the separation and purification of hydrogen. A β-(Ti,Zr,Nb) crystalline phase forms in the liquid during the cooling of Nb-containing Ti-based bulk metallic glasses (BMGs). The β-(Ti,Zr,Nb) body centered cubic phase composed of group 4 and 5 elements of the periodic table provides remarkable hydrogen permeation properties, which are superior to those of palladium alloys. The hydrogen permeability of those in-situ Ti-based BMG matrix composites has been investigated as a function of the volume fraction of crystalline phase at 623K and for the inner pressure of 1.75bar.