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Quaternary amorphous Fe-Mo-W-B alloy have been deposited by electroless plating. The structure and crystallization processes of the alloys have been studied by X-ray diffraction. It is found that for boron contents of 9.8 to 27.3 at.%, the structure is amorphous, which is wider than the range for the binary Fe-B, but is more narrow than that of ternary Fe-Mo-B amorphous films. A two-step process of crystallization is observed for the deposits. At first, the crystallization phases are alpha-Fe, Fe3B and (Mo, W),B-2, then Fe2B, (Mo, W)B and Fe-2(Mo, W) for high temperatures in the amorphous films.