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脉动直流复合电沉积(Pulsed co-elec-trode position-PCD)是制备纳米晶合金材料的新方法.本文用位置敏感原子探针(Posi-tion Sensitive Atom Probe-PoSAP),透射电子显微镜(TEM)和X-ray能量分散谱(EDS)研究了PCD法制备的纳米晶Co-Ni磁性合金的微观结构和Co含量与电解液化学成分的关系.根据Co-Ni合金相图,室温下Ni含量小于 27 ％为 hcp结构的εCo固溶体, Ni含量大于 36 ％为 fcc结构的 αCo, Ni含量在 27％～36％之间时为εCo+αCo两相结构.TEMSEM和 X-ray对不同沉积参数样品的观测表明,在电流密度为200A/m~2,电解液温度为30℃,脉动直流参数 t_(on)= t_(off)= 0.5 S的条件下可获得平均晶粒尺寸为 70 nm的沉积层(t_(on)为导通时间,t_(off)为截止时间).制备εCo,εCo+ αCo和αCo 3种典型 Co-Ni合金的电解液的化学成分见表 1.纯度 99. 9％,厚 0. 2mm的铜板为阴极,纯度 99. 9％的钴板和纯度
Pulsed co-elec trodeposition (PCD) is a new method for the preparation of nanocrystalline alloys.In this paper, we use Posi-Sensitive Atom Probe-PoSAP, TEM, And X-ray energy dispersive spectroscopy (EDS) were used to study the relationship between the microstructure and the content of Co in the nanocrystalline Co-Ni magnetic alloy prepared by PCD method and the chemical composition of the electrolyte.According to the phase diagram of Co-Ni alloy, the Ni content at room temperature is less than 27% of εCo solid solution with hcp structure, αCo with fcc structure with 36% of Ni content, and εCo + αCo phase with 27% -36% Ni content.EMSEM and X-ray diffraction patterns of samples with different deposition parameters The observation shows that under the conditions of a current density of 200 A / m 2, an electrolyte temperature of 30 ° C and pulsating DC parameter t on (on) = t off (off) = 0.5 S, a deposit with an average grain size of 70 nm (t_ (on) for the on-time, t_ (off) for the cut-off time.) Preparation of the chemical composition of the three kinds of typical Co-Ni alloy εCo, εCo + αCo and αCo electrolyte purity of 99.9% 0. 2mm copper cathode, purity 99.9% of the cobalt plate and purity