Understanding the Polymorphism of Cobalt Nanoparticles Formed in Electrodeposition–An In Situ XRD Study

Ma, Xuetian; Ma, Yifan; Nolan, Adelaide M.; Bai, Jianming; Xu, Wenqian; Mo, Yifei; Chen, Hailong

doi:10.1021/acsmaterialslett.2c00861

Understanding the Polymorphism of Cobalt Nanoparticles Formed in Electrodeposition–An In Situ XRD Study

Journal Article · Mon Mar 06 00:00:00 EST 2023 · ACS Materials Letters

DOI:https://doi.org/10.1021/acsmaterialslett.2c00861· OSTI ID:1973510

Ma, Xuetian ^[1]; Ma, Yifan ^[1]; ^[2]; ^[3]; Xu, Wenqian ^[4]; ^[2]; ^[1]

Georgia Institute of Technology, Atlanta, GA (United States)
Univ. of Maryland, College Park, MD (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
Argonne National Lab. (ANL), Lemont, IL (United States). Advanced Photon Source (APS)

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.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States); Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS); Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)

Sponsoring Organization:: Georgia Institute of Technology; National Science Foundation (NSF); National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC02-06CH11357; SC0012704

OSTI ID:: 1973510

Alternate ID(s):: OSTI ID: 2404495

Report Number(s):: BNL-224384-2023-JAAM

Journal Information:: ACS Materials Letters, Journal Name: ACS Materials Letters Journal Issue: 4 Vol. 5; ISSN 2639-4979

Publisher:: ACS PublicationsCopyright Statement

Country of Publication:: United States

Language:: English

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