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Preparation and characterization of copper-containing alumina and silica aerogels for catalytic applications

  • Invited Paper: Nano- and macroporous materials (aerogels, xerogels, cryogels, etc.)
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Abstract

Catalytic, copper-impregnated alumina and silica aerogels were prepared. Alumina gels were prepared from a solution of aluminum chloride via an epoxide-assisted synthesis. Silica gels were fabricated from tetramethyl orthosilicate using a base-catalyzed approach to the hydrolysis and polycondensation reactions. Copper was introduced into the alumina and silica gels through exposure of the wet gel to a solution of copper(II) nitrate during a solvent-exchange step prior to aerogel formation via rapid supercritical extraction. Undoped silica and alumina aerogels were fabricated for comparison. A barrage of physical characterization methods were employed to analyze the aerogels as-prepared, following heat-treatment and following catalytic testing. These include bulk density, Brunauer-Emmett-Teller surface area, Barrett-Joyner-Halenda pore distribution, infrared spectroscopy, X-ray diffraction, and scanning electron microscopy with energy-dispersive X-ray spectroscopy. As-prepared copper-silica aerogels have density 0.11 g/cm3, surface area 780 m2/g, and 9-nm average pore diameter. As-prepared copper-alumina aerogels have density 0.09–0.11 g/cm3, surface area 430 m2/g, and 23-nm average pore diameter. Calcining to 800 °C results in 10% lower surface area and average pore size 22 nm for copper-silica aerogels, 70% lower surface area for copper–alumina aerogels and, in both types of materials, yields microcrystalline CuO. A catalytic testbed was employed to assess the suitability of the copper–alumina and copper–silica aerogels as three-way catalysts for eventual application in automotive pollution mitigation. Both copper–silica and copper–alumina aerogels performed as three-way catalysts.

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Acknowledgements

This material is based upon work supported by the National Science Foundation (NSF) under Grants No. DMR-1206631 and CBET-1228851. The authors thank Elizabeth Donlon, Samuel Kleinberg and Tyler Gurian for assistance with experimental work. ZMT, AMB, and RMB are grateful for funding from Union College through the Summer Research Fellowship and Student Research Grant programs. LFP acknowledges summer funding from the Union College Chemistry Department’s Kane Fund and the Union College Summer Research Fellowship Program.

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Authors and Affiliations

  1. Department of Chemistry, Union College, Schenectady, NY, USA

    Zachary M. Tobin, Luisa F. Posada, Aude M. Bechu & Mary K. Carroll

  2. Department of Mechanical Engineering, Union College, Schenectady, NY, USA

    Ryan M. Bouck, Ann M. Anderson & Bradford A. Bruno

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  1. Zachary M. Tobin
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  2. Luisa F. Posada
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  3. Aude M. Bechu
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  4. Mary K. Carroll
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Correspondence to Mary K. Carroll.

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Tobin, Z.M., Posada, L.F., Bechu, A.M. et al. Preparation and characterization of copper-containing alumina and silica aerogels for catalytic applications. J Sol-Gel Sci Technol 84, 432–445 (2017). https://doi.org/10.1007/s10971-017-4425-9

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  • DOI: https://doi.org/10.1007/s10971-017-4425-9

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