用电子探针、透射电镜、旋转阳极Ｘ射线衍射仪和原子力显微镜分析观察了化学镀ＣｏＮｉＰ合金镀层的成分、结构和表面形貌。化学镀ＣｏＮｉＰ合金开始以晶态沉积， 表面由“圆锥峰”组成。随施镀时间的延长、镀层厚度的增加， 在原子尺寸、添加剂和镀层成分等影响下， 向微晶和非晶态转化， 镀层表面趋于平整。镀层厚度是按叠层生长方式增加的。 The composition, structure and surface morphology of electroless CoNiP alloy coatings were observed by electron probe, transmission electron microscopy, rotary anode X-ray diffraction and atomic force microscopy. Electroless plating Co  Ni  P alloy began to crystallize, the surface consists of “cone peak.” With the extension of plating time, the increase of coating thickness changes into microcrystalline and amorphous under the influence of atomic size, additive and coating composition, and the surface of the coating tends to be flat. The thickness of the coating is increased by the growth of the stack.