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Elucidation of the chemical state of phosphorus and boron in crystallographically amorphous nickel electroplates

机译:阐明非晶态镍电镀中磷和硼的化学态

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Using the valence-to-core version of X-ray emission spectroscopy (valence-to-core XES) together with X-ray diffraction analysis, the structure and the composition of nickel coatings deposited from solutions containing hypophosphite ions or dimethylaminoborane (DMAB) are studied. The diffraction patterns of prepared deposits are characterized by the presence of a wide "halo". Annealing of crystallographically amorphous deposits at temperatures of 500°C and higher transforms these haloes into the spectra corresponding to metal nickel and its phosphides or borides present in the crystallized deposits. A result of fundamental importance obtained in the simultaneously conducted examination of the same deposits by the valence-to-core XES method is that both the binding energy and the intensities of Kβ satellite spectral lines of annealed samples remain unchanged as compared with original samples. Based on this comparison, it is concluded that phosphide and boride nickel compounds were already formed in the course of electrodeposition, whereas the thermal treatment of deposits (crystallization) leads only to aggregation of the metal and metal-metalloid nanoparticles.
机译:结合使用X射线发射光谱的价核形式(XES价核)和X射线衍射分析,可以确定从含次磷酸盐离子或二甲基氨基硼烷(DMAB)的溶液中沉积的镍涂层的结构和组成。研究。制备的沉积物的衍射图的特征在于存在宽的“晕”。在500°C或更高温度下对结晶无定形沉积物进行退火,将这些光晕转变为对应于结晶沉积物中存在的金属镍及其磷化物或硼化物的光谱。通过价-心XES方法同时进行的相同沉积物检查获得的根本重要性是,退火样品的结合能和Kβ卫星光谱线的强度与原始样品相比均保持不变。基于该比较,可以得出结论,在电沉积过程中已经形成了磷化物和硼化物镍化合物,而沉积物的热处理(结晶)仅导致金属和金属准金属纳米粒子的聚集。

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