One-dimensional gold nanofibers are good candidates for next generation nanoelectronic devices. Here, gold nanofibers were synthesized via electrospinning with subsequent in-situ thermal reduction. The thermal behavior of the precursor nanofibers was investigated by thermogravimetric/differential thermal analysis and fourier transform infrared. The polymer parts are decomposed and removed step by step, meanwhile, gold salt is decomposed and in-situ reduced to form gold nanoparticles in air without any reducing agent or gas due to its strong oxidation ability. The effects of gold content, polymers type (PVP, PVA, PAN), calcination atmospheres (Air, H2, H2/Ar) and temperatures (200 °C to 500 °C) on the morphology and structures of gold nanofibers were characterized by XRD, SEM, and TEM. The results shows that PVP is the optimal polymer with the gold content of 6:1 (PVP:Au) to fabricate the continuous gold nanofibers with good morphology and structures. The final gold nanofibers with average diameter of 60 nm and several hundred micrometers long, were fabricated after calcined at 500 °C in air for 2 hours. It was composed of gold nanoparticles that ranged from 5 to 30 nm.
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