Synthesis of self-passivated, and carbide-stabilized zirconium nanopowder
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RESEARCH PAPER
Synthesis of self-passivated, and carbide-stabilized zirconium nanopowder Amr M. Abdelkader • Derek J. Fray
Received: 21 May 2013 / Accepted: 5 November 2013 / Published online: 17 November 2013 Ó Springer Science+Business Media Dordrecht 2013
Abstract An electrochemical technique was used to synthesis air-stable zirconium nanoparticles by cathodically reducing a precursor of ZrO2 and carbon. It was possible by controlling the carbon content and the heat treatment procedure prior to the electrodeoxidation to produce different structures. At low carbon content and low initial sintering temperature, the nanoparticles are about 100 nm and tend to agglomerate to form micron-sized clusters passivated by a layer rich in oxygen. The passivation protocol has changed and was achieved through the strong Zr–C bond on the dispersed particles when ZrC was present in the cathode before electrolysis. It was also possible to control the size of the particles as small as 25 nm or less. Keywords Reactive metal Electrodeoxidation Self-passivated Nanoparticles
Electronic supplementary material The online version of this article (doi:10.1007/s11051-013-2112-5) contains supplementary material, which is available to authorized users. A. M. Abdelkader (&) School of Materials, University of Manchester, Grosvenor Street, Manchester M1 7HS, UK e-mail: [email protected] D. J. Fray Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ, UK
Introduction Synthesis of reactive metal nanoparticles has been attracting a great deal of attention due to the unusual electronic, magnetic, and catalytic properties in nanophase metals (Fu¨rstner 1993; Leslie-Pelecky and Rieke 1996; Dlott 2006). Of particular interest, zirconium nanoparticles have strong potential for applications such as energy conversion, catalysis, powder metallurgy, nanocomposites, and biomedical engineering (Thomsen et al. 1997; Golightly and Castleman 2007; Vasquez et al. 2008; Tokushige et al. 2010). Zirconium based materials have a good thermal conductivity, a low neutron absorption cross sections, and a weak damage sensitivity under irradiation (Abdelkader and El-Kashif 2007; Gusev 1997). These properties coupling with the significant improvement in the mechanical properties of the nano-sized grains, make nanocrystalline zirconium alloys, or composites based thereon, suitable construction materials for the new generation of nuclear reactors (Gen-IV project) (Goddard 2006; Murty and Charit 2008). So far, synthesis of nanophase reactive metal as powders has followed two general protocols: physical route, such as laser ablation (Dolgaev et al. 2002) and ball milling (Yen 1998; Barraud et al. 2008); chemical approaches, such as vapor deposition, plasma phase reduction (Murphy 2004), and wet chemical procedures (Bo¨nnemann et al. 1994; Berry et al. 2003; Ghosh et al. 2008; Epshteyn et al. 2009). However, there is a challenge on using these methods in the
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