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X-ray spectroscopic analysis of stochastic, periodic precipitation in Co–Fe-Based Prussian blue analogues
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-04-26 00:00:00 , DOI: 10.1039/c8ja00068a Hisashi Hayashi 1, 2, 3, 4, 5 , Yui Sato 1, 2, 3, 4, 5 , Hitoshi Abe 5, 6, 7, 8, 9
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-04-26 00:00:00 , DOI: 10.1039/c8ja00068a Hisashi Hayashi 1, 2, 3, 4, 5 , Yui Sato 1, 2, 3, 4, 5 , Hitoshi Abe 5, 6, 7, 8, 9
Affiliation
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Inorganic precipitates sometimes spontaneously create complex, interesting banding structures in gels, which are potentially applicable in materials engineering. A new member of such self-organizing bandings, i.e., stochastic, periodic banding of the precipitates of Co–Fe-based Prussian blue analogues (Co–Fe PBAs), denoted as “pattern-A”, was observed in water-glass gels. The pattern-A periodic bands did not obey empirical scaling laws that many Liesegang bands follow, illustrating the importance of ripening effects. Time-resolved X-ray fluorescence (XRF) and position-dependent X-ray absorption near-edge structure (XANES) measurements were conducted for a pattern-A sample, which was prepared from 0.30 M CoCl2 and 0.05 M K3[Fe(CN)6] solutions. XRF results demonstrated that the Co–Fe PBA distributions fluctuated highly over the sample tube, including the turbid zone, and suggested that significant Ostwald ripening of the Co–Fe PBAs takes place in the periodic bands. XANES results indicated that the local structures and symmetries of the Co–Fe PBAs in the periodic bands were highly uniform. Furthermore these results are consistent with a model where the periodic bands contain a relatively high concentration of Co–Fe PBAs, with the most dominant local structure being Co(OC)4(NCFe)2, co-existing with [Co(H2O)6]2+ ions. These findings not only provide an interesting piece of information for future self-organization processes of Co–Fe PBAs, but also confirm the potential of the combined X-ray spectroscopic techniques for in-depth analysis of the periodic precipitation phenomenon in gels.
中文翻译：
X射线光谱分析基于钴铁的普鲁士蓝类似物的随机，周期性降水
无机沉淀物有时会自发地在凝胶中形成复杂的，有趣的带状结构，这可能适用于材料工程。在水玻璃中观察到了这种自组织带的新成员，即Co-Fe基普鲁士蓝类似物（Co-Fe PBAs）的沉淀物的随机，周期性带状出现。凝胶。模式A的周期性谱带没有遵循许多Liesegang谱带遵循的经验标度定律，这说明了成熟效应的重要性。对A型样品进行了时间分辨X射线荧光（XRF）和位置依赖性X射线吸收近边缘结构（XANES）测量，该样品由0.30 M CoCl 2和0.05 MK 3 [Fe（ CN）6]解决方案。XRF结果表明，Co-Fe PBA的分布在整个样品管中（包括混浊区）波动很大，并且表明Co-Fe PBA的明显奥斯特瓦尔德熟化发生在周期带中。XANES结果表明，Co-Fe PBA在周期带中的局部结构和对称性非常均匀。此外，这些结果与周期带包含相对较高浓度的Co-Fe PBA的模型相一致，其中最主要的局部结构为Co（OC）4（NCFe）2，与[Co（H 2 O ）6 ] 2+离子。这些发现不仅为Co-Fe PBA的未来自组织过程提供了有趣的信息，而且证实了结合X射线光谱技术对凝胶中周期性沉淀现象进行深入分析的潜力。
更新日期：2018-04-26
中文翻译：
X射线光谱分析基于钴铁的普鲁士蓝类似物的随机，周期性降水
无机沉淀物有时会自发地在凝胶中形成复杂的，有趣的带状结构，这可能适用于材料工程。在水玻璃中观察到了这种自组织带的新成员，即Co-Fe基普鲁士蓝类似物（Co-Fe PBAs）的沉淀物的随机，周期性带状出现。凝胶。模式A的周期性谱带没有遵循许多Liesegang谱带遵循的经验标度定律，这说明了成熟效应的重要性。对A型样品进行了时间分辨X射线荧光（XRF）和位置依赖性X射线吸收近边缘结构（XANES）测量，该样品由0.30 M CoCl 2和0.05 MK 3 [Fe（ CN）6]解决方案。XRF结果表明，Co-Fe PBA的分布在整个样品管中（包括混浊区）波动很大，并且表明Co-Fe PBA的明显奥斯特瓦尔德熟化发生在周期带中。XANES结果表明，Co-Fe PBA在周期带中的局部结构和对称性非常均匀。此外，这些结果与周期带包含相对较高浓度的Co-Fe PBA的模型相一致，其中最主要的局部结构为Co（OC）4（NCFe）2，与[Co（H 2 O ）6 ] 2+离子。这些发现不仅为Co-Fe PBA的未来自组织过程提供了有趣的信息，而且证实了结合X射线光谱技术对凝胶中周期性沉淀现象进行深入分析的潜力。
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