The origin of native Si-Fe alloy mineral is thought to be related with mantle and aerolite. The native Si-Fe alloy minerals from podiform chromites of the Luobusha ophiolite in the Yarlong Zangbo suture zone were examined by a new method for powder-like diffractograms of small single crystals, using an SMART APEX-CCD area-detector X-ray diffractometer. The powder diffraction pattern shows that the minerals are composed of FeSi, FeSi2, β-FeSi21) and native silicon. The association of these minerals suggests that the crystallization order of the mineral may be from early to late FeSi→mFeSi2→mnative silicon, accompanied by gradually increasing deoxidization.