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In situ high-temperature electron microscopy of 3DOM cobalt, iron oxide, and nickel

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Abstract

High-temperature electron microscopy was used to follow how the structure of two specimens of three-dimensionally ordered macroporous (3DOM) materials, also known as inverse opals, and one specimen of a precursor to a 3DOM material changed with temperature. The change in grain size with temperature of 3DOM cobalt and 3DOM iron oxide (as magnetite) was monitored in situ in the TEM by heating in stages to 900 and 1,000 °C, respectively. The two materials studied by TEM showed contrasting grain growth behavior. For 3DOM cobalt, carbon surrounding the nanometer-size grains led to slower grain growth in thinner sample areas than in areas in closer contact with other grains; a bimodal grain-size distribution was observed after heating above 700 °C for 90 min. The grains of the 3DOM iron oxide had no carbon coating and coarsened more evenly to give a unimodal size distribution. Line scans from selected-area diffraction (SAD) patterns were used for phase analysis and showed that traces of cobalt oxide present in the 3DOM cobalt sample at room temperature disappeared when the sample was heated above 500 °C. The transformation of a 3DOM precursor material, nickel(II) oxalate–polystyrene (PS) latex composites, was followed in situ by variable-temperature environmental scanning electron microscopy (ESEM) from room temperature to ca. 700 °C in 0.5–0.7 kPa O2. The ESEM examination of the 3DOM precursors permitted real-time observation of the polymer template decomposition and the shrinkage that occurs upon calcination of these precursor materials.

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Acknowledgements

The authors thank Dr. Hongwei Yan for providing the samples of 3DOM materials, Dr. Stuart McKernan for assistance with the ESEM and TEM, and the David and Lucile Packard Foundation and the 3M Heltzer Endowed Chair of the University of Minnesota for research funding.

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Authors and Affiliations

  1. Department of Chemistry, University of Minnesota, 207 Pleasant Street SE, Minneapolis, MN, 55455-0431, USA

    Christopher F. Blanford & Andreas Stein

  2. University of Oxford, Inorganic Chemistry Laboratory, South Parks Road, Oxford, OX1 3QR, UK

    Christopher F. Blanford

  3. Department of Chemical, Materials & Biomolecular Engineering, University of Connecticut, 191 Auditorium Road Unit 3222, Storrs, CT, 06269-3222, USA

    C. Barry Carter

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  1. Christopher F. Blanford
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Correspondence to Christopher F. Blanford.

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Blanford, C.F., Carter, C.B. & Stein, A. In situ high-temperature electron microscopy of 3DOM cobalt, iron oxide, and nickel. J Mater Sci 43, 3539–3552 (2008). https://doi.org/10.1007/s10853-008-2550-0

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