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Alternative etching methods to expand nanocasting, and use in the synthesis of hierarchically porous nickel oxide, zinc oxide, and copper monoliths

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Abstract

Nanocasting into silica templates for preparation of mesoporous materials has up to now been limited to those metal oxides and metals that can withstand the harsh silica etching processes currently used. Two new methods of removing the silica template are reported, either by dissolving the silica in methanolic base or by dissolution in aqueous base under an external potential. The utility of these methods is demonstrated in the synthesis of hierarchically porous zinc oxide, nickel oxide, and copper monoliths that would dissolve or react using other template removal methods. The successful etching of monolithic zinc oxide using methanolic base etching can be explained by the reduced solubility of zinc oxide in methanol compared with an aqueous base, while it also reduces the formation of hydroxides when etching the nickel oxide and copper monoliths. Alternatively, the formation of highly soluble copper oxide/hydroxide can be avoided by holding the copper monolith at a sufficiently negative potential while etching with an aqueous base.

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Acknowledgments

The use of Central Analytical Facility instruments (SEM, XRD) is greatly acknowledged. This work was partially supported by NSF under Grant No. CHE-0719398 (MGB) and by the Academy of Finland through Grant No. 259310 (JHS). The technical assistance of Ms. Kate Price in the development of the voltage stabilized etch, Mr. Jake Mims for sample preparation, and Mr. Clifton Watkins for running Raman spectroscopy are also much appreciated.

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Author notes

  1. Franchessa D. Sayler

    Present address: ThruPore Technologies LLC, Box 870204, Tuscaloosa, AL, 35487-0204, USA

Authors and Affiliations

  1. Department of Chemistry, The University of Alabama, Tuscaloosa, Alabama, 35487-0336, USA

    Amy J. Grano, Franchessa D. Sayler & Martin G. Bakker

  2. Center for Functional Materials and Laboratory of Physical Chemistry, Åbo Akademi University, Porthansgatan 3-5, FIN-20500, Turku, Finland

    Jan-Henrik Smått

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  1. Amy J. Grano
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Correspondence to Martin G. Bakker.

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Supplementary materials can be viewed in this issue of the Journal of Materials Research by visiting http://journals.cambridge.org/jmr.

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Grano, A.J., Sayler, F.D., Smått, JH. et al. Alternative etching methods to expand nanocasting, and use in the synthesis of hierarchically porous nickel oxide, zinc oxide, and copper monoliths. Journal of Materials Research 28, 2483–2489 (2013). https://doi.org/10.1557/jmr.2013.153

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