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A series of NiP x B y nanomaterials were prepared by a chemical reduction method under various preparation parameters. Experiment results show that the different preparation parameters affected the morphology, particle size, surface area and the composition of the sample. However, they did not influence the electronic state of nickel. The type of solution showed significant influence on the properties of the sample, whereas, the type of nickel salt did not. The particle size of NiPB, NiB, and NiP were 10–30 nm. The NiP sample prepared in the aqueous solution had the largest particle size 50–150 nm. If the solvent was 50% ethanol in water, the surface area of the sample significantly increased nine fold for NiP and four fold for NiPB powders. In contrast, the surface area of NiB did not increase. The NiPB, NiB, and NiP powders had a spherical morphology if they were prepared with aqueous solution. The NiPB prepared in 50% ethanol solution showed floss morphology and had a very high surface area.  相似文献   
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