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[求助]
求助各位大哥大姐和大佬，关于合金XRD计算问题
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我电镀制备NiCo涂层，先用拟合对主峰进行拟合分析，然后通过谢勒公式计算对分别对ni和co的主要相进行晶粒尺寸计算，但审稿人认为Co 应溶解在Ni 中，以生成具有纯 Ni（即 fcc）相同晶格结构的 Ni-Co 固体溶液。但是，由于Co 的原子半径大于 Ni，因此预期Ni 峰位置（相对于 jcpds 卡）的位置会向左移动。这并不意味着存在具有 fcc 晶格结构的 Co 相！Co的晶格结构仍然是hcp，其浓度可能高于饱和度。同时co 具有 hcp 晶格，因此，其平面应呈现为 （10.0） 和 （10.1），而不是 （100） 和 （101）。 我到底该怎么去计算合金涂层的晶粒尺寸，还有晶面表达是（10.0）和 （10.1）的这种加点的方式么？ 以下是审稿人的意见： 1- in phase analysis of ni-co alloy using xrd technique, the authors believe that ni and co phases are present together with an fcc lattice structure. this idea is also presented in fig. 9. according to the ni-co phase diagram, co should dissolve in ni to produce a ni-co solid solution with the same lattice structure of pure ni (i.e., fcc). however, since the atomic radius of co is larger than ni, a left shift in positions of ni peaks (relative to jcpds cards) is expected. this does not mean that a co phase with fcc lattice structure is present! the lattice structure of co remains hcp, and it could present at concentrations higher than the saturation one. 2- co has an hcp lattice, and thus, its planes should be presented as (10.0) and (10.1), not as (100) and (101). 3- for determining the crystallite size using scherrer formula, beta is the peak broadening and not the fwhm of the diffraction peaks. this parameter should be calculated by subtracting the instrumental widening from that of the fwhm. for this reason, strange values of crystallite size (15-50 nm) are reported by the authors. indeed, if any peaks relating to ni (fcc) are considered for the crystallite size calculation, this cannot be correct (see comment # 1).  微信截图_20200719211003.png@comma@wacky1980 |
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