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Novel Process for Solid State Reduction of Metal Oxides and Hydroxides

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Abstract

Recently the reductive expansion synthesis (RES) method was introduced as a means to create nano- and sub-micron metal particles and alloys by rapid heating of physical mixtures of urea with a metal nitrate. In the present work the generality of the RES method was demonstrated by creating metal micron and sub-micron particles from oxide and hydroxide precursors, and outlining the impact of temperature, precursor ratio, and gas flow rate on the product. For example, precursor selection impacted the temperature required for complete reduction, the amount of carbon present, and the size of the metal particles. For complete NiO reduction to micron scale particles, high urea content and a high temperature [ca. 1073 K (800 °C)] were required. In contrast, Ni(OH)2 was reduced to metal at far lower temperatures. Moreover, the Ni particles formed from NiOH were sub-micron (ca. 200 nm) in size and carbon encapsulated. Other parameter variations had a similarly significant impact. Indeed, the reciprocal relationship between inert gas flow rate and the extent of reduction supports the supposition that the primary mechanism of reduced metal particle formation is the reduction of metal oxide particles by gases produced by urea decomposition. Collectively these and other findings indicate the RES method can be manipulated to create a range of micron and sub-micron reduced metal particle architectures appropriate for different applications.

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Authors and Affiliations

  1. Department of Aerospace and Mechanical Engineering, Naval Postgraduate School, Monterey, CA, 93943, USA

    Claudia Luhrs (Associate Professor) & Margaret Kane (Student)

  2. Department of Mechanical Engineering, University of New Mexico, Albuquerque, NM, 87131, USA

    Zayd Leseman (Associate Professor)

  3. Physics Department, Naval Postgraduate School, Monterey, CA, 93943, USA

    Jonathan Phillips (Research Professor)

Authors
  1. Claudia Luhrs
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  2. Margaret Kane
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  3. Zayd Leseman
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  4. Jonathan Phillips
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Correspondence to Jonathan Phillips.

Additional information

Manuscript submitted April 12, 2012.

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Luhrs, C., Kane, M., Leseman, Z. et al. Novel Process for Solid State Reduction of Metal Oxides and Hydroxides. Metall Mater Trans B 44, 115–122 (2013). https://doi.org/10.1007/s11663-012-9756-x

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  • DOI: https://doi.org/10.1007/s11663-012-9756-x

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