利用TEM、XRD、X射线能量散射谱(EDS)、位置敏感原子探针场离子显微镜(PoSAP)等方法研究了脉冲电沉积法制备的块体纳米晶Co-Ni合金的微观组织结果表明:沉积层中Co含量随电解液中Co2+离子浓度增加而显著增加;沉积层合金点阵参数随Co含量的增加按Vegard定律增加,同时晶粒尺寸减小;当晶粒尺寸减小到十几纳米时,出现附加的晶格膨胀效应;脉冲沉积与直流沉积相比,晶粒明显细化;PoSAP操作的在线观测和大量数据的计算机三维重构图表明,Co原子在沉积层中呈均匀分布;FIM观察分析表明纳米晶Co-Ni合金中存在三类晶间结构:正常晶界、非长程有序也非短程有序.的"类气态结构"和少量暗区.
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