用 M2+（M = Co、Ni）和类似古巴比伦的 Ni4O4 单元装饰

用 M2+（M = Co、Ni）和类似古巴比伦的 Ni4O4 单元装饰的还原型 Preyssler 聚氧化金属酸盐的电化学辅助单晶生长。

Kirkland Sheriff, Dino Sulejmanovic, Jiheon Jun, William Cannon, Lauren Petta, Johnathan Phillips, Colin McMillen, Shiou Jyh Hwu

摘要

聚氧化金属酸盐（POMs）是科学界非常感兴趣的物质，其还原和成核已通过多步骤技术得到证实。本研究开发了一种电化学方法，用于同时还原含多氧金属酸盐的固体并使其成核。在此，我们报告了还原型 Preyssler 聚氧化钨酸盐基（阴离子式 [NaP5W30O110]14-）新晶体固体的晶体生长情况，该固体由 Co2+ 和 Ni2+ 离子相互连接的 Preyssler 阴离子构成。在室温条件下，使用双银丝电极装置，在恒定外加电位下的各种水溶液中实现了晶体成核和原位还原。POM 材料沉积在阴极上，并通过 X 射线衍射技术对其结构进行了表征。观察到的主要结构类型包括由无序 Co2+/Ni2+ 八面体装饰的 POM，以及由附加 Co2+/Ni2+ 八面体融合成的 1-D 柱。在基于 Ni 的反应中观察到了一个次生相，还原的 Preyssler 阴离子被 Ni4O4 立方体状单元装饰。为了解电化学过程，介绍了电解质溶液的极化曲线，提出了最适合晶体生长的应用电位。这项研究强调了电化学途径的有效性，在这种途径中，POM 的成核和同时还原可以生成新型还原 POM 固体。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

Electrochemically Assisted Single Crystal Growth of Reduced Preyssler Polyoxometalates Decorated with M2+ (M = Co, Ni) and Cubane-Like Ni4O4 Units.

Polyoxometalates (POMs) are of great interest to the scientific community, and their reduction and nucleation have been well-established by multi-step techniques. The present study develops an electrochemical approach for simultaneous reduction and nucleation of polyoxometalate-containing solids. Herein we report crystal growth of reduced Preyssler polyoxotungstate-based (anionic formula [NaP5W30O110]14-) new crystalline solids made of Preyssler anions interlinked by Co2+ and Ni2+ ions. Crystal nucleation and in situ reduction were achieved at room temperature using a two silver wire electrode setup in various aqueous solutions under constant applied potentials. The POM material was deposited on the cathode, and its structure was characterized by X-ray diffraction techniques. The primary structure type observed involves POMs decorated by disordered Co2+/Ni2+ octahedra and fused into 1-D pillars by additional Co2+/Ni2+ octahedra. A secondary phase was observed in the Ni-based reactions, where reduced Preyssler anions are decorated by Ni4O4 cubane-like units. To understand the electrochemical process, polarization curves of the electrolyte solutions are presented, suggesting an applied potential best suited for crystal growth. The work highlights the effectiveness of an electrochemical pathway where nucleation and simultaneous reduction of POMs can make novel reduced POM solids.

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