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Preparation, Characterization And Application Of Functional Nanoporous Carbon-based Materials

Posted on:2017-01-23Degree:DoctorType:Dissertation
Country:ChinaCandidate:J H ZhangFull Text:PDF
GTID:1221330482992130Subject:Inorganic Chemistry
Abstract/Summary:PDF Full Text Request
The porous carbon material are widely used in the field of catalyst, separating materials and advanced electronic materials, due to their high specific surface area and excellent physical and chemical properties. General methods for the synthesis of porous carbon materials include carbonization Organic-gel method, catalytic activation method and carbonization polymer, etc. Most of the porous carbon materials prepared by these methods have low specific surface area, and the pore size is not adjustable. In recent years, the preparation method of porous carbon has a new breakthrough, silica gel, zeolite molecular sieve, metal organic frameworks(MOFs)as the precursor of the template method prepared the high specific surface area and ordered mesoporous carbon nano materials, which generate excellence performance in selective gas adsorption, hydrogen storage, electrochemical and catalysis. and it has become one of the hot topic in this field.With the huge environmental problems caused by the consumption of fossil energy, the demand for new energy materials is increasing day by day. Non metal doped nano porous carbon and nano carbon based composite materials have been proved to be excellent electrochemical materials, which can be used as anode materials for lithium ion batteries, super capacitor materials and so on.This paper aims at the preparation, characterization and performance test of a nitrogen doped nano porous carbon with a low cost, easily synthetic biology coordination polymer(a small biomolecules amino acid as ligand) as precursor using the soft template method, M@C(M:Metal,C: Carbon)complex was synthesized by one step method, and the MO@C(M:Metal oxide,C: Carbon) complex was synthesized by two steps. The morphology and composition of the samples under different carbonization temperature were monitored by transmission electron microscope in situ heating technique. The relationship between the carbonization temperature and the final product was also discussed. The main content of this paper includes the following parts:The first chapter is the introduction part. The definition, classification, synthesisand application of nano-porous carbon materials are summarized. The preparation methods and applications of nitrogen-doped nano-porous carbon are mainly introduced. In addition, the related research of carbon based metal complexes and carbon based metal oxide composites were also introduced.The second chapter focus on the self assembling biological coordination polymer-glutamate synthetic zinc(Zn-Glu) as template to prepared nitrogen doped nano porous carbon without adding any carbon source and nitrogen source under the protection of nitrogen atmosphere. XRD, SEM, TG-DTA, TEM, XPS, N2adsorption-desorption, and Raman spectroscopy were used to characterize the products. The results show that the nitrogen content in the sample is 3.34%, the specific surface area of up to 1619.2 cm2?g-1, pore size distribution has a hierarchical structure, mainly concentrated in 1.1 and 2.9 nm and pore volume for 0.91 cm3- g-1.Finally, performance of the nitrogen doped nano porous carbon was also tested. The results show the specific capacitance can reach 140.8 F ? g-1 under the current density of 0.25 g-1, and the supercapacitors is very good.In the third chapter, the nitrogen doped nano porous carbon was prepared by the self assembly of the biological coordination polymer(Zn-Asp) as the template. The products were characterized by XRD, SEM, TEM, TG-DTA, N2 adsorption desorption and so on. The results show that the maximum specific surface area of the nitrogen doped nano porous carbon is 1397.84 cm2?g-1. The adsorption performance of CO2 gas shows that the sample with specific surface area of 884.32 cm2 ? g-1, nitrogen content of 1.50% has a relatively good adsorption properties for CO2(at 273 K temperature, CO2 adsorption capacity was 75.57 cm3/g).In the fourth chapter, we used a single two-step method to prepare NiO nanoparticles encapsulated into a highly ordered porous carbon matrix by selected Ni-ptca as template. The characterization of these materials was performed by X-ray diffraction, scanning electron microscopy, and TG-DTA. We have successfully prepared a uniform NiO nanoparticle@mesoporous carbon composite, it exhibited high surface area(240.25 m2?g-1), showed the pore size distribution centered at about10 nm, the NiO particle size range from 8 to 10 nm. Subsequently, we conductedthese materials for lithium-ion battery performance test, the initial charge capacity is as high as 900 mA h g-1 and the reversible charge capacity is as high as 545.3 mA h g-1at the current density of 200 mA/g, which suggesting highly stable cycling performance and good reversibility. The result indicated that the NiO nanoparticles encapsulated into a highly ordered porous carbon matrix, which can allow short ion diffusion paths, and consequently the rapid ion transport and adsorption, thus making this material superior to conventional metal-oxide.In the fifth chapter, the process of preparation of Cu@C using HKUST-1 as template was observed by the high resolution transmission electron microscope in situ heating reaction technique for the first time. The results show that the metal nano size becomes larger with the increase of the pyrolysis temperature using the MOFs as the template or the former system. Precise control of temperature is a key step in the preparation of size controllable carbon based metal nanoparticle composites.
Keywords/Search Tags:Nanoporous carbon, coordination polymer, nitrogen doping, supercapacitor, adsorption
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