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Understanding the Polymorphism of Cobalt Nanoparticles Formed in Electrodeposition─An In Situ XRD Study
ACS Materials Letters ( IF 9.6 ) Pub Date : 2023-03-06 , DOI: 10.1021/acsmaterialslett.2c00861 Xuetian Ma 1 , Yifan Ma 1 , Adelaide M Nolan 2 , Jianming Bai 3 , Wenqian Xu 4 , Yifei Mo 2 , Hailong Chen 1
ACS Materials Letters ( IF 9.6 ) Pub Date : 2023-03-06 , DOI: 10.1021/acsmaterialslett.2c00861 Xuetian Ma 1 , Yifan Ma 1 , Adelaide M Nolan 2 , Jianming Bai 3 , Wenqian Xu 4 , Yifei Mo 2 , Hailong Chen 1
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An advanced synchrotron-based in situ X-ray diffraction (XRD) technique is successfully developed and employed to track and monitor the formation and phase selection of cobalt (Co) in electrodeposition in real time and verify DFT computational results. The impacts of a number of controlling factors including the pH of the electrolyte and deposition overpotential are systematically studied. The results show that the yielded phase of the electrodeposited Co is controlled by both thermodynamics and kinetics. The low pH low overpotential condition favors the formation of the thermodynamically stable fcc phase. While the high pH high overpotential condition promotes the formation of the metastable hcp phase. The experimental results agree well with the nanometric phase diagram computed with DFT. Layer-by-layer alternative stacking of fcc-hcp polymorphic phases can be facilely fabricated by just varying the overpotential. This work not only offers an effective means to control the phase of electroplating of Co but also presents a new approach to reveal the fundamental insights of the formation of metals under electrochemical reduction driving force.
中文翻译：
了解电沉积中形成的钴纳米粒子的多晶型——一项原位 XRD 研究
成功开发了一种基于同步加速器的先进原位X 射线衍射 (XRD) 技术，并用于实时跟踪和监测电沉积中钴 (Co) 的形成和相选择，并验证 DFT 计算结果。系统地研究了包括电解质 pH 值和沉积过电位在内的许多控制因素的影响。结果表明，电沉积 Co 的屈服相受热力学和动力学的控制。低 pH 低过电势条件有利于热力学稳定的fcc相的形成。而高 pH 高过电位条件促进了亚稳态hcp的形成阶段。实验结果与用 DFT 计算的纳米相图非常吻合。只需改变过电势，就可以轻松地逐层交替堆叠fcc-hcp多晶相。这项工作不仅提供了一种控制 Co 电镀阶段的有效手段，而且还提供了一种新方法来揭示在电化学还原驱动力下金属形成的基本见解。
更新日期：2023-03-06
中文翻译：
了解电沉积中形成的钴纳米粒子的多晶型——一项原位 XRD 研究
成功开发了一种基于同步加速器的先进原位X 射线衍射 (XRD) 技术，并用于实时跟踪和监测电沉积中钴 (Co) 的形成和相选择，并验证 DFT 计算结果。系统地研究了包括电解质 pH 值和沉积过电位在内的许多控制因素的影响。结果表明，电沉积 Co 的屈服相受热力学和动力学的控制。低 pH 低过电势条件有利于热力学稳定的fcc相的形成。而高 pH 高过电位条件促进了亚稳态hcp的形成阶段。实验结果与用 DFT 计算的纳米相图非常吻合。只需改变过电势，就可以轻松地逐层交替堆叠fcc-hcp多晶相。这项工作不仅提供了一种控制 Co 电镀阶段的有效手段，而且还提供了一种新方法来揭示在电化学还原驱动力下金属形成的基本见解。
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