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TEM characterization of iron-oxide-coated ceramic membranes

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Abstract

Commercially available porous alumina–zirconia–titania ceramic (AZTC) membranes having a titania surface coating were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), and the Brunauer–Emmett–Teller (BET) method. TEM photomicrographs showed the as-received AZTC membrane to be a multi-layered structure consisting of a porous alumina–zirconia–titania core having ultrafine pore sizes, coated by an additional layer of nanoporous titania. Electron diffraction studies revealed an amorphous surface titania layer while the underlying AZTC membrane was crystalline. The AZTC membranes were coated 20, 30, 40, 45, or 60 times with iron oxide (Fe2O3) nanoparticles, after which the membranes were sintered in air at 900 °C for 30 min. TEM revealed a relatively uniform nanoporous Fe2O3 coating on the sintered, coated membranes, where the Fe2O3 coating thickness increased with increasing number of layers. Electron diffraction patterns showed the Fe2O3 coating to be crystalline in nature. This was confirmed by the XRD results showing the structure to be α-Fe2O3, while the AZTC membrane was a mixture of the anatase and rutile phase of TiO2 as well as ZrO2 and corundum, Al2O3. The average pore size of the underlying AZTC membrane increased after the Fe2O3-coated membrane was sintered. The nanoporosity in the sintered Fe2O3 coating increased until 40 layers, beyond which no significant increases in the average pore size were observed. The iron-oxide-coated membrane improved catalytic properties when used in combination with ozone to treat water. The optimal benefit, in terms of water treatment efficacy, was found at 40 layers of Fe2O3.

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Acknowledgements

The authors would like to acknowledge the US Environmental Protection Agency (US EPA) Science to Achieve Results (STAR) Program (Grant No. RD830090801) and the National Science Foundation Nanoscale Interdisciplinary Research Teams (NSF-NIRT) Program (Grant No. BES0506828) for financial support of this work. Our thanks also go to Ms. Alicia Pastor, from the Center for Advanced Microscopy and Mr. Robert Pcionek for there assistance during TEM sample analysis. Mr. Rui Huang is also acknowledged for XRD analysis of the samples. Thanks are due to Yang Chen for performing the BET measurements. We would also like to thank Mr. David Jackson for his assistance with the membrane coating process. Finally, we gratefully acknowledge the helpful suggestions and comments from Prof. G.M. Janowski of the University of Alabama at Birmingham.

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Authors and Affiliations

  1. Malcolm Pirnie, Inc., 1700 West Loop South, Suite #1450, Houston, TX, 77027, USA

    B. S. Karnik

  2. Department of Chemical Engineering & Materials Science, Michigan State University, East Lansing, MI, 48824, USA

    M. J. Baumann & L. M. Corneal

  3. Department of Civil & Environmental Engineering, Michigan State University, East Lansing, MI, 48824, USA

    S. J. Masten & S. H. Davies

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  1. B. S. Karnik
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  2. M. J. Baumann
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  3. L. M. Corneal
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  4. S. J. Masten
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  5. S. H. Davies
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Correspondence to L. M. Corneal.

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Karnik, B.S., Baumann, M.J., Corneal, L.M. et al. TEM characterization of iron-oxide-coated ceramic membranes. J Mater Sci 44, 4148–4154 (2009). https://doi.org/10.1007/s10853-009-3608-3

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  • DOI: https://doi.org/10.1007/s10853-009-3608-3

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