Carbon foams prepared from polyimide using urethane foam template

Polyimide and carbon foams were successfully prepared using polyurethane foams as a template. Impregnation of polyimide precursor, poly(amide acid), followed by imidization at 200 °C gave polyurethane/polyimide (PU/PI) composite foams, which resulted in PI foams by heating above 400 °C and then carbon foams above 800 °C. Foams carbonized at 1000 °C were graphitized by the heat treatment at 3000 °C, keeping foam characteristics. Two applications of these carbon foams, i.e., an adsorbent of ambient water vapor and a substrate of photocatalyst anatase TiO₂, were experimentally confirmed. For the former application, the present foam could be characterized by prompt adsorption of ambient water vapor. Some of carbon foams prepared were floating on water, even after loading photocatalyst anatase, which might be advantageous for photodecomposition of pollutants in water in respect to the UV rays efficiency.     

Preparation of porous carbons from thermoplastic precursors and their performance for electric double layer capacitors

Porous carbons with high surface area were successfully prepared from thermoplastic precursors, such as poly(vinyl alcohol) (PVA), hydroxyl propyl cellulose and poly(ethylene terephthalate), by the carbonization of a mixture with MgO at 900 °C in an inert atmosphere. After carbonization the MgO was dissolved out using a diluted sulfuric acid and the carbons formed were isolated. The mixing of the PVA carbon precursor with the MgO precursors (reagent grade MgO, magnesium acetate or citrate) was done either in powder form or in an aqueous solution. The BET surface area of the carbons obtained via solution mixing could reach a very high value, such as 2000 m²/g, without any activation process. The pore structure of the resultant carbons was found to depend strongly on the mixing method; the carbons prepared via solution mixing were rich in mesopores, but those produced via powder mixing were rich in micropores. The size of mesopores was found to be almost the same as that of the MgO particles, suggesting a way of controlling the mesopore size in the resultant carbons. Measurement of capacitance was carried out in 1 mol/L H₂SO₄ electrolyte. The porous carbon with a BET surface area of 1900 m²/g prepared at 900 °C through solution mixing of Mg acetate with PVA showed a fairly high EDLC capacitance, about 250 F/g with a current density of 20 mA/g and 210 F/g with 1000 mA/g. The rate performance was closely related to the mesoporous surface area.     

Carbon membranes from cellulose and metal loaded cellulose

The focus of this work was to find a low-cost precursor for carbon molecular sieve (CMS) membranes, and a simple way of producing them. In addition, several ways of modifying a carbon material are described. The modification method used in this study was metal doping of carbon. CMS membranes were formed by vacuum carbonization of cellulose and metal loaded cellulose. Metal additives include oxides of Ca, Mg, Fe(III) and Si, and nitrates of Ag, Cu and Fe(III).The carbon membrane containing Fe-nitrate has promising separation performance for the gas pairs O₂/N₂ and CO₂/CH₄. Carbon containing nitrates of Cu or Ag show high selectivity, but reduced O₂ and CO₂ permeability compared to carbon with Fe-nitrate. Element analysis indicates that Cu migrates to the carbon surface, creating an extra layer resistance to gas transport. A silver mirror is also seen on the surface of Ag-nitrate-containing carbon. However, the Ag- and Cu-containing membranes show a high H₂ permeability. Adding metal oxides makes the carbon membranes retard the transport of easily condensable gases (e.g. CO₂). This can be exploited for enhanced H₂/CO₂ separation efficiency.     

Influence of the matrix microstructure on the mechanical properties of CVI-infiltrated carbon fiber felts

The correlation between the matrix microstructure and the mechanical properties of CVI-infiltrated carbon fiber felts was studied by optical microscopy, scanning electron microscopy, and three-point bending tests. The results of these investigations show a correlation between (a) the content of highly textured pyrocarbon in the matrix and the quasi-ductile fracture behavior of the samples and (b) the thickness of the low textured pyrocarbon layers beneath the fibers and the measured flexural strengths. Fractographic investigations using SEM showed that toughness increase results from multiple crack deflections at the interface between numerous ‘sublayers’ forming the highly textured pyrocarbon. The increase of flexural strength could be explained by a thicker, so called ‘virtual’ fiber.     

Carbon foam matrices saturated with PCM for thermal protection purposes

In the present work, numerical and experimental studies are proposed to predict and investigate the thermal characteristics of a thermal protection system consists of carbon foam matrix saturated with phase change material, PCM. Several types of carbon foam matrices with different porosities and thermal properties were introduced for the sake of a parametric study. The composite (carbon foam matrix saturated with PCM) was introduced into a cylindrical enclosure while it experiences its heat from a heat source setting on the top of the enclosure. The numerical simulation was performed using the volume averaging technique and a finite volume technique was used to discretize the heat diffusion equation while the phase change process was modeled using the enthalpy porosity method. The results are portrayed in terms of temperature and heat absorption time history and the numerical and experimental results showed good agreement. The results illustrated that the higher the porosity the more stability of the thermal performance of the matrix composite. On the other hand, the thermal conductivity of the composite matrix acts sharply to increase or decrease its heat absorption rate.     

Catalytic treating of gas pollutants over cobalt catalyst supported on porous carbons derived from rice husk and carbon nanotube

Porous carbons were prepared from rice husks, commercial coconut-shell-derived carbon, and carbon nanotube (CNT) by activation with CO₂, KOH, and ZnCl₂. Cobalt catalysts were supported on the six different porous carbons by excess-solution impregnation, and were used to carry out reactions with different constituents such as NO + CO, toluene, NO + toluene, and NO + CO + toluene in the presence of 6% O₂ at 250 °C to evaluate the activity of porous catalysts. The properties of the catalysts were analyzed by X-ray powder diffractometer (XRD), a field-emission scanning electron microscope (FESEM), transmission electron microscope (TEM), and an X-ray energy dispersive spectrometer (EDS). The cobalt catalysts supported on rice-husk-based carbon activated by CO₂ and those on commercial-activated-carbon re-treated by KOH showed 100% conversion on toluene oxidation. CNT-cobalt catalyst showed 63% NO conversion with CO and 46% with toluene at 250 °C. Among the six porous supported catalysts, the cobalt catalysts prepared with CNT and rice-husk-derived carbon by using CO₂ showed the best catalytic activity and thermal stability when compared to the others.     

Carbon membranes from precursors containing low-carbon residual polymers

Asymmetrical hollow-fibre carbon membranes with increased porosity were obtained by carbonization of polyacrylonitrile based precursors containing high quantities of polymers, such as polyethylene glycol and polyvinylpyrrolidone, which give low-carbon residue upon pyrolysis. The interaction between molecules of the two polymers, which could serve as evidence of at least partial miscibility of these polymers, occurred only with PVP-containing precursors. The narrowest pore-size distribution was inherent in carbon membranes produced from such precursors.     

Catalytic graphitization of templated mesoporous carbons

Graphitic porous carbons with a wide variety of textural properties were obtained by using a silica xerogel as template and a phenolic resin as carbon precursor. The synthetic procedure used to prepare them was as follows: (a) infiltration of the porosity of silica by a solution containing phenolic resin, (b) carbonization of the silica-resin composite, (c) removal of the silica skeleton, (d) impregnation of the templated porous carbon with a metallic salt and (e) catalytic graphitization of the impregnated carbon by heat treatment at 900 °C. The graphitization of the carbons thus prepared varies as a function of the carbonization temperature used and the type of metal employed as catalyst (Fe, Ni or Mn). The porous characteristics of these materials change greatly with the temperatures used during the carbonization step. These graphitized carbons exhibit high electrical conductivities up to two orders larger than those obtained for the non-graphitized samples.     

Structure and mechanical properties of nanofibrous ZrO2 derived from alternating field electrospun precursors

Nanofibrous zirconia (ZrO₂) meshes were prepared from precursor fibers which were synthesized using the method of free-surface, high-yield alternating field electrospinning (AFES). The weight ratio of zirconyl chloride salt to polyvinylpyrrolidone (PVP) polymer in liquid precursors was investigated for its effect on the spinnability and formation of precursor fibers as well as on the resulting fibrous ZrO₂. The precursor fiber generation measured at a rate up to 5.6 g/h was achieved with a single flat 25-mm diameter alternating current (AC) electrode, which corresponded to production of up to 1.5 g/h of fibrous ZrO₂. The calcination process involved annealing the fibers at temperatures which ranged from 600 °C to 1000 °C and produced 0.1–0.2 mm thick fibrous ZrO₂ meshes. Individual nanofibers were found to have diameters between 50 and 350 nm and either a tetragonal (t-ZrO₂) or monoclinic (t-ZrO₂) structure depending on the calcination temperature. The annealed meshes with total porosity between 98.0 ± 0.2% and 94.6 ± 0.2% showed little deformation or cracking. Tensile strength and modulus of fibrous t-ZrO₂ meshes strongly depended on porosity and varied from 0.07 ± 0.03 MPa to 1.05 ± 0.3 MPa and from 90 ± 40 MPa to 388 ± 20 MPa, respectively. The m-ZrO₂ meshes resulted similar moduli, but much lower strengths due to their brittleness. A power-law relationship between the elastic modulus and porosity of AFES-derived nanofibrous t-ZrO₂ meshes, in comparison with other porous zirconia materials, was also investigated. The results of this study have demonstrated the feasibility of free-surface AFES in sizeable production of zirconia nanofibers and highly porous nanofibrous ceramic structures.     

Reaction-bonded SiC derived from resin precursors by Stereolithography

A photo-curable resin with a high carbon yield after pyrolysis was developed in the present research. It consisted of phenolic epoxy acrylate resin, phenolic resin, triethylene glycol as pore forming agent and benzoin dimethyl ether as photoinitiator. The well-prepared mixed resin was used by Stereolithograpy to form resin prototypes. The influence of mixed resin composition on the process parameters was studied to meet the requirement for the cured thickness. Carbon preforms with open porosity of 27% and bending strength of 4.48 MPa were obtained after pyrolyzing the resin prototypes. After molten silicon infiltration at the temperature 2300 ?C, the carbon preform converted to reaction-bonded SiC. The maximum bending strength of the produced SiC samples was 127.8 ± 0.5 MPa as the pore forming agent content was 40 wt.%. Neither residual carbon nor silicon remained in the reaction-bonded SiC sample according to the XRD analysis.     

Carbon/carbon nanocomposites derived from phenolic resin-silica hybrid ceramers: microstructure, physical and morphological properties

Phenolic resin-silica hybrid ceramers were prepared through the sol-gel method. The hybrid ceramers with various inorganic contents were used as matrix precursors to fabricate silica containing carbon/carbon (C/C) composites. The effect of the organic-inorganic mixing ratio on the change of density and porosity was studied. The flexural strength and modulus of the C/C composites was also investigated. Results show that the density of the C/C composites increases with silica content. However, at higher silica content, the density of the composites does not change before and after carbonization. Silica increases the stiffness of the fabricated C/C composites from 2.4×10⁴ to 3.0×10⁴ MPa. However, it does not affect the flexural strength. XRD and Raman spectra studies show that the incorporation of inorganic silica into the phenolic resin influences the growth of ordered carbon structures. From SEM morphological observations, it was concluded that the silica particles are dispersed uniformly on the surfaces of the specimens with some particles located at the pores due to the decomposition of the polymer matrix.     

Simple synthesis of mesoporous carbon with magnetic nanoparticles embedded in carbon rods

Magnetically separable ordered mesoporous carbon containing magnetic nanoparticles embedded in the carbon walls was synthesized using a simple synthetic procedure. The resulting magnetically separable mesoporous carbon was denoted as M-OMC (magnetically separable ordered mesoporous carbon) poly(pyrrole) with residual Fe²⁺ ions in the mesoporous channel was converted to carbon material containing superparamagnetic nanoparticles. The size of the magnetic nanoparticles obtained was restricted by the channel size of the SBA-15 silica template, which resulted in the generation of superparamagnetic nanoparticles embedded in the carbon rods. The blocking temperature of M-OMC is 110 K. Pore size and textural property of M-OMC is similar to that of hexagonally ordered mesoporous carbon fabricated using SBA-15 silica as a template. The saturation magnetization of M-OMC is ca. 30.0 emu/g at 300 K, high enough for magnetic separation.     

Effect of oxygen functional groups on synthetic carbons on liquid phase oxidation of cyclohexanone

Synthetic carbons from phenolic resins were used as catalysts for the aqueous phase oxidation of cyclohexanone to C₄-C₆ dicarboxylic acids (adipic, glutaric and succinic acids) at 413 K under 50 bar total air pressure. The changes in microporous structure and surface chemistry, produced as a consequence of activation or heat treatment processes, were analyzed. Using CO₂ or air as activating agent increased significantly the surface area and the total pore volume responsible for the activity. The surface chemistry of the samples was also modified and was characterized by titration with bases of different strength and with HCl, by temperature programmed desorption, and by X-ray photoelectron spectroscopy. To determine the role of surface oxygen functionalities on the catalytic behavior of the carbons, heat treatments in nitrogen at different temperatures were used to selectively eliminate oxygenated groups. Thus, treatment at temperatures of 1173 K eliminating the carbonyl/quinone groups decreased the selectivity to adipic acid and dicarboxylic acids. Introducing quinone groups during the synthesis of the carbons also improved the selectivity to adipic acid, proving that the mechanism of oxidation involves the quinone type groups on the carbon surface.     

Microstructure of carbon derived from mangrove charcoal and its application in Li-ion batteries

In this study, the microstructure of mangrove-charcoal-derived carbon (MC) was studied using XRD, STM and TEM. MC was found to consist of aligned quasi-spherical structural units with diameters of around 5-20 nm. It shows typical hard carbon characteristics, including a strongly disoriented single graphene layer and BSU, formed by two or three graphene layers stacked nearly parallel. Some curved and faceted graphene layers, especially closed carbon nanoparticles with fullerene-like, were observed in the as-prepared samples. MC was also evaluated as an anodic material for Li-ion batteries. MC carbonized at 1000 °C possessed the highest available discharge capacity (below 0.5 V) of 335 mAh g⁻¹, the high first-cycle coulombic efficiency of 73.7%, good rate and cyclic capability and PC-based electrolyte compatibility. ⁷Li nuclear magnetic resonance (NMR) spectra of fully lithiated mangrove charcoal-derived carbons indicated the co-existence of three Li species.     

以煤焦油沥青为原料制备高性能活性炭的研究

以煤焦油沥青为原料,使用KCNS溶液活化处理,选择适宜的工艺条件,制备出优质的活性炭。讨论了煤焦油沥青热处理温度、中间相沥青的粒径、KCNS溶液的浓度、KCNS溶液与中间相沥青的液固比、炭化温度、炭化时间、活化温度、活化时间等主要因素对活性炭性能的影响。结果表明,在该适宜的工艺条件下制备的活性炭,强度为90.8%,比表面积为2 601.5 m2/g,吸碘值为2 217.0 mg/g,吸苯值为1 099.3mg/g,吸亚甲基蓝值为397.8mg/g,产品性能优良。