分别将粒径5 μm镍粉与45~75 μm铝粉（1^#）、0.2 μm镍粉与45~75 μm铝粉（2^#）、0.2 μm镍粉与0.5 μm铝粉（3^#）按物质的量比为1：1混合，通过真空热压制备Ni/Al含能结构材料试样，研究了粉末粒径对试样压缩性能和能量释放特性的影响。结果表明：3种试样在镍/铝界面处均生成了一层Al₃Ni扩散层；1^#试样中镍颗粒均匀分布在连续的铝基体中，压缩性能较好；2^#试样中镍颗粒发生团聚，相对密度最小，抗压强度最低；3^#试样中镍相为连续基体，致密性最好，抗压强度最高，但生成的Al₃Ni最多；随着粉末粒径减小，3种试样放热反应能量密度均提高，最高达1 147.8 J·g^-1，反应活化能降低，能量释放效率提高，3^#试样的能量释放特性最佳。

Ni and Al powders with particle size of 5 μm and 45—75 μm (1^#), 0.2 μm and 45—75 μm (2^#), 0.2 μm and 0.5 μm (3^#), respectively, and with molar ratio of 1:1 were mixed, and then Ni/Al energetic structural material samples were prepared by vacuum hot-pressing. The effect of powder particle size on the compression performance and energy release characteristics of the samples was studied. The results show that the three samples all had a Al₃Ni diffusion layer formed at the Ni/Al interface. In 1^# sample, the Ni particles uniformly distributed in the continuous Al matrix, and the compression performance was relatively good. In 2^# sample, the Ni particles agglomerated, and the relative density and compressive strength were the lowest. In 3^# sample, the Ni phase was continuous matrix, and the densification and compressive strength were the highest, but the most Al₃Ni was formed. As the particle size of the powders decreased, the exothermic reaction energy density of the three samples increased, up to 1 147.8 J·g^-1, the reaction activation energy was reduced, and the energy release efficiency was improved. The energy release characteristics of 3^# sample were the best.