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Mechanical alloying(MA) technique and single-roller melt spinning technique were used to prepare Fe86Zr5.5Nb5.5B3 nanocrystalline and amorphous powders, bulk alloys were prepared by cryogenically high-pressure quick sintering. The results showed that: (1) after MA process for 15 hours, the grain size of α-Fe phase was ≤10nm; (2) melt spinning powders were fragmented by ball milling, but remained amorphous state. The crystallization temperature of this amorphous powder was about 500℃. Apparent activation energy of the amorphous crystallization was E=294.1KJ/mol; (3) under the quick sintering conditions of P=5.5GPa/t=3min/Pw≥1050W, single phaseα-Fe nanocrystalline(8～15nm) bulk alloys with relative density≥98.7% can be obtained.