The synthesis of nitrogen doped carbon spheres and polythiophene/carbon sphere composites

摘要

This study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple syntheticudprocedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine.udDepending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % wasudobtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % whenudan ammonium solution and acetylene were used as reactants. The diameters of carbon spheresudwere found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can beudcontrolled by varying the flow rate, temperature, time, concentration and the reactor type. Theudsamples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA,udPXRD and ESR.udWe have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzedudoxidative polymerization. The average particle size was about 50 nm, within a narrow particlesizeuddistribution. The undoped carbon spheres (CSs) were reacted with thiophene to giveudpolymer/carbon composites containing polythiophene and carbon nanospheres via chemicaludoxidative polymerization reaction. Polythiophene molecules were either chemically bonded orudphysically adsorbed to the surface of carbon spheres. The microstructure and properties of theudtwo types of composites were compared. The thermogravimetric analysis data confirmed that theudpresence of CSs in the polymercarbon composites is responsible for the higher thermal stabilityudof the composite material in comparison with pristine polythiophene. The FTIR analysis showedudthat covalent functionalized nanocomposites exhibit a high intensity of a C-S bond This study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple syntheticudprocedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine.udDepending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % wasudobtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % whenudan ammonium solution and acetylene were used as reactants. The diameters of carbon spheresudwere found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can beudcontrolled by varying the flow rate, temperature, time, concentration and the reactor type. Theudsamples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA,udPXRD and ESR.udWe have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzedudoxidative polymerization. The average particle size was about 50 nm, within a narrow particlesizeuddistribution. The undoped carbon spheres (CSs) were reacted with thiophene to giveudpolymer/carbon composites containing polythiophene and carbon nanospheres via chemicaludoxidative polymerization reaction. Polythiophene molecules were either chemically bonded orudphysically adsorbed to the surface of carbon spheres. The microstructure and properties of theudtwo types of composites were compared. The thermogravimetric analysis data confirmed that theudpresence of CSs in the polymercarbon composites is responsible for the higher thermal stabilityudof the composite material in comparison with pristine polythiophene. The FTIR analysis showedudthat covalent functionalized nanocomposites exhibit a high intensity of a C-S bondThis study reports on the synthesis of N-doped carbon spheres (N-CSs) by a simple syntheticudprocedure. A horizontal CVD type reactor was used to synthesize N-CSs from pyridine.udDepending on the dilution of the pyridine with toluene, a nitrogen content of 0.13-5 mol % wasudobtained. The use of a vertical CVD reactor gave N-CSs with a N-content of 0.19-3 mol % whenudan ammonium solution and acetylene were used as reactants. The diameters of carbon spheresudwere found to be in the range of 40 nm to 1000 nm for both CVD reactors. The diameter can beudcontrolled by varying the flow rate, temperature, time, concentration and the reactor type. Theudsamples were characterized by TEM, HRTEM, elemental analysis, Raman spectroscopy, TGA,udPXRD and ESR.udWe have demonstrated that unsubstituted thiophene can be polymerized by Fe3+-catalyzedudoxidative polymerization. The average particle size was about 50 nm, within a narrow particlesizeuddistribution. The undoped carbon spheres (CSs) were reacted with thiophene to giveudpolymer/carbon composites containing polythiophene and carbon nanospheres via chemicaludoxidative polymerization reaction. Polythiophene molecules were either chemically bonded orudphysically adsorbed to the surface of carbon spheres. The microstructure and properties of theudtwo types of composites were compared. The thermogravimetric analysis data confirmed that theudpresence of CSs in the polymercarbon composites is responsible for the higher thermal stabilityudof the composite material in comparison with pristine polythiophene. The FTIR analysis showedudthat covalent functionalized nanocomposites exhibit a high intensity of a C-S bond at 695 cm-1 ,udwhich is not observed in the noncovalent functionalized nanocomposites