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Triethylamine catalyst was used to increase the§molecular weight of poly(amic acid). In§electrospinning, diameter of PAA nanofibers was§controlled by molecular weight of poly(amic acid) and§concentration of poly(amic acid)/N-N§dimethylformamide solution. The diameters of§polyimide based carbon nanofibers reached to a§minimum value of around 100 nm. The conductivity of§the carbon nanofiber papers increased with the§decreasing of fiber diameters, while the mechanical§strength of polyimide and carbon nanofiber paper was§diameter independent. Further more, Pt was§successfully impregnated in carbon nanofiber.§Reduction accompanied with carbonization in Ar gas at§up to 1000 degree C produced small and well-dispersed§Pt nanoparticles (3-5 nm). Carbon dioxide treatment§exhibited the effective ability of removal of§carbonaceous overlayers to promise a potential§enhancement Pt catalyst activity. The reduction rate§of Pt ion is different at heating rate of 2 and 5§degree C/min. Thus, the heating rate and time at high§temperature strongly affected Pt nanoparticle size.