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X-ray diffraction and micro-Raman spectroscopy analysis of new nickel hydroxide obtained by electrodialysis

机译:电渗析得到的新型氢氧化镍的X射线衍射和显微拉曼光谱分析

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摘要

Industrial nickel hydroxide samples produced by electrodialysis have been characterized both by X-ray diffraction (XRD) and by wicro-Raman spectroscopy. A comparison with some commercial products of p-type Ni(OH)_2 is made. Aged in KOH solution, these nickel hydroxides are transformed to the β-Ni(OH)_2 phase and undergo Ostwald ripening, leading to crystallite sizes ranging between 260 and 380 A with a reduction in defects. The anisotropic broadening of the XRD peaks in the β-Ni(OH)_2 pattern is interpreted in terms of crystalline lattice micro-strains and crystallite size. For the first time, Rietveld refinement has been performed on industrial Ni(OH)_2. The results indicate that the micro-strain effects increase the peak width according to the sequence of families (hk0) → (00l) → (h0l). This 8tudy shows that the presence of proton vacancies leads to a lower degree of distortion in the crystalline lattice than does the presence of stacking faults or the adsorption of inorganic species at the border of the crystallites. A very high concentration of point defects inducing 8trong distortions in the crystal lattice is correlated with the presence of high energy Ni--O bond vibrations in the Raman spectra, with a frequency shift towards unusually high values.
机译:通过电渗析生产的工业氢氧化镍样品已通过X射线衍射(XRD)和wicro-Raman光谱进行了表征。与p型Ni(OH)_2的一些商品进行了比较。这些氢氧化镍在KOH溶液中老化后,转变成β-Ni(OH)_2相并经历Ostwald成熟,从而导致晶粒尺寸在260至380 A之间,并减少了缺陷。 β-Ni(OH)_2图案中XRD峰的各向异性展宽是根据晶格微应变和微晶尺寸来解释的。首次对工业Ni(OH)_2进行Rietveld精炼。结果表明,微应变效应根据族(hk0)→(00l)→(h0l)的序列增加了峰宽。该8研究表明,质子空位的存在导致晶体晶格中的变形程度低于堆积缺陷或无机物在晶体边界处的吸附。极高浓度的点缺陷在晶格中引起8trong畸变,与拉曼光谱中高能Ni-O键振动的存在相关,频率向异常高的值移动。

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