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Synthesis, Adsorption and Structural Properties of Carbons with Uniform and Ordered Mesopores

Posted on:2009-12-21Degree:Ph.DType:Thesis
University:Kent State UniversityCandidate:Gierszal, KamilFull Text:PDF
GTID:2441390005461450Subject:Chemistry
Abstract/Summary:
Various novel carbon mesostructures were explored with respect to their synthesis methods, adsorption properties as well as structural properties. Several important problems were studied including the structural ordering of ordered mesoporous carbons (OMCs), selection of carbon precursors, controlling the pore size, specific surface area and total pore volume of the resulting carbons. Ordered mesoporous silicas (OMSs) and silica colloidal templates were employed as hard templates. The obtained results have been divided into two major chapters dealing with: OMCs synthesized by using OMSs as templates and the mesoporous carbons templated by silica colloidal materials.;The first aforementioned chapter presents the following problems. Two different OMSs, SBA-15 and KIT-6, were employed as hard templates and various carbon precursors including mesophase pitches of different softening points were used for the purpose to investigate the relation between the structure of OMCs and their adsorption properties. One of the most important conclusions was that the softening temperature of mesophase pitch clearly affected the structural properties of the resulting OMCs through the formation of different amount of micropores.;The other studies involved the synthesis and characterization of OMCs templated by the SBA-16 silica with precisely controlled pore sizes. For this purpose, various carbon precursors were used - sucrose, acenaphthene and furfuryl alcohol. Two types of OMCs were prepared - the fully-filled inverse carbon replicas and the film-type inverse replicas of the SBA-16 silica.;The second chapter deals with mesoporous carbons templated by silica colloidal crystals (SCCs) and disordered colloidal silicas. These templates served for the synthesis of mesoporous carbons from mesophase pitch as carbon precursors. The SCC was formed by evaporation method using the aqueous suspension of 46 nm uniform silica colloids, whereas the same method applied to 16 and 31 nm silica nanoparticles afforded only disordered aggregates. Application of these templates showed for the first time that it is possible to achieve the faithful inverse carbon replica of the well-ordered SCC composed of such small colloids.;The other problem was devoted to graphitization of SCC-templated OMC. Here, well-graphitizable mesophase pitch as carbon source and SCC formed from 70 nm nanoparticles were employed. Carbonization at 1000 °C and subsequent graphitization of OMC at temperature as high as 2500 °C allowed one to obtain an excellent quality porous carbon ordered at nanoscale and at molecular level.;The most important achievement reported in this dissertation was the synthesis of mesoporous carbons with extremely large pore volume and narrow pore size distribution. The structure was synthesized with the use of colloidal silica and resorcinol-crotonaldehyde as template and carbon precursor, respectively. The large pore volume could be obtained by formation of uniform thin carbon film on the pore walls of the aggregates of silica nanoparticles. Such prepared carbons with uniform mesopores reached the highest ever reported value of the total pore volume of ~9 cm3/g. Also, new mathematical relations between basic adsorption parameters were derived.;Various measuring techniques were used in order to characterize the adsorption and structural properties of the studied nanoporous materials. Among them were nitrogen adsorption, elemental analysis, powder X-ray diffraction (XRD), small angle X-ray scattering (SAXS), transmission and scanning electron microscopy (TEM/SEM), thermogravimetric analysis (TGA), Raman spectroscopy.
Keywords/Search Tags:Carbon, Structural properties, Adsorption, Synthesis, Pore, Uniform, Ordered, Silica
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