Ni65B35 and Ni80P11 ultrafine amorphous alloy particles (UFAAP) have been prepared by the reduction of Ni^2^+ in aqueous solution with KBH4 and NaH2PO2, respectively, at room temperature. Ni73P13B14 UFAAP has been prepared by the reduction of Ni^2^+ with KBH4 and NaH2PO2 at the same time. The Ni-P sample has relatively large particle size (c.a. 110nm) while Ni-B sample exhibits much smaller particle size (c.a. 20nm). The particle size of Ni-P-B (c.a. 40nm) is close to that of Ni-B. XPS showed that the interaction between Ni and P is stronger than that between Ni and B, since the electronic charge of P is similar in the Ni-P-B and Ni-P samples. However, the Ni-P-B sample is of higher surface area than Ni-P. In an addition, the Ni-P-B sample exhibits higher stability in amorphous state than Ni-P and Ni-B. The amorphous state of the Ni-P-B sample remained after heat treatment in N2 at 573K. The transformation of Ni3B to Ni3P during crystallization of the Ni-P-B sample also indicated that the interaction between Ni and P is stronger than that between Ni and B.

Key words: CATALYST, NICKEL ALLOYS, X-RAY DIFFRACTION ANALYSIS, ICP, PHOSPHORUS ALLOYS, BORON ALLOY, AMORPHOUS ALLOY