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Controlled-Atmosphere Flame Fusion Growth of Nickel Poly-oriented Spherical Single Crystals—Unraveling Decades of Impossibility

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Abstract

Experimental research using monocrystalline electrodes has been a hallmark of interfacial electrochemistry and electrocatalysis since 1980. However, it has been limited to mainly noble metals because of the challenges encountered when using non-noble metals. We report on the development of controlled-atmosphere flame fusion that enables the growth of spherical single crystals of non-noble metals in controlled gaseous atmosphere and without the formation of surface or bulk oxides. The set-up is used to grow nickel single crystals the structure of which is verified using Laue X-ray back-scattering and scanning electron microscopy (SEM). The equilibrium shape of the nickel single crystals calculated using Wulff construction agrees with the actual shape determined using SEM. Electrochemical measurements in aqueous NaOH solution using the monocrystalline Ni electrodes reveal cyclic voltammetry features unique to their surface structure. The methodology, transferrable to other metals, creates enormous research opportunities in interfacial electrochemistry, electrocatalysis, surface science, gas-phase catalysis, and corrosion science.

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Acknowledgments

We gratefully acknowledge the technical support of Charles Hearns and Patrick Given in designing and manufacturing the stainless-steel chamber bottom. We thank Drs. Gabriele Schatte and Kevin McEleney for their assistance in acquiring scanning electron microscope images. We thank Profs. Christophe Coutanceau and Stève Baranton for their assistance in manufacturing the quartz chamber.

Funding

This research was conducted as part of the Engineered Nickel Catalysts for Electrochemical Clean Energy project administered from Queen’s University and supported by grant number RGPNM 477963-2015 under the Natural Sciences and Engineering Research Council of Canada (NSERC) Discovery Frontiers Program. This work was supported by MITACS through the Globalink Research Award and the DAAD which made the collaboration between Queen’s University and Ulm University possible. This work was funded by the German Research Foundation (DFG) under project ID 390874152 (POLiS Cluster of Excellence) as well as the Sonderforschungsbereich (collaborative research centre) SFB-1316.

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Author notes

  1. Derek Esau and Fabian M. Schuett contributed equally to this work.

Authors and Affiliations

  1. Department of Chemistry, Queen’s University, 90 Bader Lane, Kingston, Ontario, K7L 3N6, Canada

    Derek Esau, K. Liam Varvaris & Gregory Jerkiewicz

  2. Institute of Electrochemistry, Ulm University, Albert-Einstein-Allee 47, 89081, Ulm, Germany

    Fabian M. Schuett & Timo Jacob

  3. Department of Physics, Chemistry and Biology, IFM, Linköping University, 58183, Linköping, Sweden

    Jonas Björk

  4. Helmholtz-Institute-Ulm (HIU) Electrochemical Energy Storage, Helmholtzstr. 11, 89081, Ulm, Germany

    Timo Jacob

  5. Karlsruhe Institute of Technology (KIT), P.O. Box 3640, 76021, Karlsruhe, Germany

    Timo Jacob

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  1. Derek Esau
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Contributions

D.E. and F.M.S. carried out all the experiments, developed the CAFF set-up and method, analyzed the data, and wrote the first version of the manuscript with equal contributions. K.L.V contributed to materials synthesis and to the electrochemical measurements. J.B. carried out the DFT calculations of the Wulff construction under the guidance of T.J. G.J. and T.J. conceived the experiments, supervised the project, analyzed the results, and contributed to the manuscript writing. All authors contributed to the discussion section and the finalization of the text and figures of the manuscript.

Corresponding authors

Correspondence to Timo Jacob or Gregory Jerkiewicz.

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The authors declare no competing interests.

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The research presented in this manuscript was initially submitted to Science on June 18, 2019 and subsequently to Nature Materials on September 12, 2019. The research was presented at the 70th Annual Meeting of the International Society of Electrochemistry in Durban, South Africa, on August 8, 2019 (the respective abstract was published on the ISE website on June 25, 2019).

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Esau, D., Schuett, F.M., Varvaris, K.L. et al. Controlled-Atmosphere Flame Fusion Growth of Nickel Poly-oriented Spherical Single Crystals—Unraveling Decades of Impossibility. Electrocatalysis 11, 1–13 (2020). https://doi.org/10.1007/s12678-019-00575-w

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