CARBOTHERMAL REDUCTION SYNTHESIS OF ZrB2 NANOFIBRES VIA PRE-OXIDISED ELECTROSPUN ZIRCONIUM N-PROPOXIDE

Zirconium diboride (ZrB2) nanofibres, with an average diameter of 297 plus or minus 103 nm, were fabricated using a combination of electrospinning and carbothermal reaction. The solution for electrospinning was prepared by dissolving zirconium n-propoxide (Zr(OPr)4) and boric acid in glacial acetic...

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Bibliographic Details
Published in:Ceramics international 2015-01, Vol.41 (5), p.6905-6911
Main Authors: Ghelich, R, Aghdam, R M, Torknik, F S, Jahannama, M R, Keyanpour-Rad, M
Format: Article
Language:English
Subjects:
Argon
Atmospheres
Carbon
Electrospinning
Nanostructure
Reduction
Synthesis
Zirconium
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Summary:Zirconium diboride (ZrB2) nanofibres, with an average diameter of 297 plus or minus 103 nm, were fabricated using a combination of electrospinning and carbothermal reaction. The solution for electrospinning was prepared by dissolving zirconium n-propoxide (Zr(OPr)4) and boric acid in glacial acetic acid and 2,4-pentanedione followed by mixing in PVP/ethanol solution. The effects of the supplemental source of carbon, pre-heat treatment of the electrospun nanofibres in air and materials used for the fabrication of the crucible in the carbonisation treatment in an argon atmosphere were studied to optimise the experimental conditions for the synthesis of ZrB2 nanofibres. The synthesised nanofibres were then characterised using FESEM, EDS, DSC-TGA, XRD and BET method. Results showed that an increased C/Zr ratio caused an increase in the diameter of the as-spun fibres and a reduction of ZrO2 impurities in the final product. The PVP/Zr(OPr)4 hybrid nanofibres maintained their fibrous morphology after stabilisation at 150 C in air for 24 h, pre-oxidation at 350 C in an ambient environment for 4 h followed by carbonisation at 1350 C in an argon atmosphere, resulting in highly crystalline ZrB2 nanofibres using graphite as an external supplemental carbon source. The crystallite size of ZrB2 nanofibres decreased from 47 to 37 nm with increased pre-oxidation heating rate. The specific surface area of the nanofibres, calculated by the multipoint BET-equation, was 19.5 m2/g with a mean pore diameter of 34 nm.
ISSN:0272-8842