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.     

Adsorption of l-histidine over mesoporous carbon molecular sieves

Mesoporous carbon, CMK-3, was prepared by large pore hexagonal mesoporous silica SBA-15. The structural order and textural properties of all the materials were studied by XRD, HRTEM, and nitrogen adsorption. Adsorption of l-histidine (His) over various porous adsorbents such as CMK-3, SBA-15, and activated carbon was studied from solutions with different pH. His adsorption was observed to be pH dependent with maximum adsorption near the isoelectric point of the amino acid. CMK-3 showed a larger amount of His adsorption as compared to SBA-15 and the conventional adsorbent, namely activated carbon. CMK-3 registers the total adsorption capacity of ca. 1350 μmol g⁻¹ which is ca. 12 times higher than the adsorption capacity of SBA-15. This large difference could be mainly due to the stronger hydrophobic interaction between the non-polar side chains of amino acids and the hydrophobic surface of the mesoporous carbon as compared to mesoporous silica. The influence of ionic strengths on the adsorption of His was also studied and the results are discussed. Nitrogen adsorption of CMK-3 after His adsorption confirmed that His molecules are tightly packed inside the mesopores.     

Carbon coating of anatase-type TiO2 through their precipitation in PVA aqueous solution

Fine particles of photocatalytic anatase-type TiO₂ prepared through hydrolysis of titanium-tetraisopropoxide were coated by carbon through their precipitation in poly(vinyl alcohol) (PVA) aqueous solution, followed by heat treatment at high temperatures of 400-1000 °C in a flow of high purity Ar. Without carbon coating, the phase transformation from anatase to rutile started above 600 °C, but it was suppressed up to 800 °C with carbon coating. Suppression of the phase transformation depended on the amount of carbon coated, apparent suppression being observed with carbon content above 5 mass%. The amount of carbon coated on anatase was controlled by changing the concentration of PVA in the solution. In order to have a carbon content of about 5 mass%, a PVA solution with more than 2 mass% had to be used.     

Pore structure of carbons coated on ceramic particles

Pore structure of carbon coated on ceramic particles by carbonization of precursor in a powder mixture at 900 °C was studied by focusing on the effects of substrate ceramics (MgO, TiO₂ and various phases of Al₂O₃) and of carbon precursor (poly(vinyl alcohol) (PVA), poly(ethylene terephthalate) (PET) and hydroxyl propyl cellulose (HPC)). By dissolving substrate MgO particles, carbon coated was found to have a high BET surface area, more than 1000 m²/g, which was almost the same as the value estimated from apparent surface area measured on carbon-coated MgO particles under the assumption of zero surface area of the substrate. The carbon separated was found to be rich in micropores from the analyses by DFT method and α_s plot. The dependence of the BET surface area on the amount of carbon coated on TiO₂ with a high surface area was the same for three carbon precursors, although the carbon yields from the precursors were slightly different. Porous Al₂O₃ substrates, γ-Al₂O₃as-received and that formed from Al(OH)₃ during carbonization, gave a high BET surface area, but dense Al₂O₃, α-Al₂O₃, gave a low surface area.     

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-coated lithium titanate: effect of carbon precursor addition processes on the electrochemical performance

In this paper,two carbon-coated lithium titanate(LTO-C1 and LTO-C2)composites were synthesized using the ball-milling-assisted calcination method with different carbon precursor addition processes.The physical and electrochemical properties of the as-synthesized negative electrode materials were characterized to investigate the effects of two carbon-coated LTO synthesis processes on the electrochemical performance of LTO.The results show that the LTO-C2 synthesized by using Li2CO3 and TiO2 as the raw materials and sucrose as the carbon source in a one-pot method has less polarization during lithium insertion and extraction,minimal charge transfer impedance value and the best electrochemical performance among all samples.At the current density of 300 mA·h·g^-1,the LTO-C2 composite delivers a charge capacity of 126.9 mA·h·g^-1,and the reversible capacity after 300 cycles exceeds 121.3 mA·h·g^-1 in the voltage range of 1.0–3.0 V.Furthermore,the electrochemical impedance spectra show that LTO-C2 has higher electronic conductivity and lithium diffusion coefficient,which indicates the advantages in electrode kinetics over LTO and LTO-C1.The results clarify the best electrochemical properties of the carbon-coated LTO-C2 composite prepared by the one-pot method.     

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.     

The effect of silica template structure on the pore structure of mesoporous carbons

We have synthesized two kinds of mesoporous carbons using a spherical silica sol (SMC1 carbon) and an elongated silica sol (SMC3 carbon) as templates. Nitrogen isotherms and electrochemical experiments were performed to investigate the effect of the silica template structure on the pore structure of the resulting mesoporous carbons. When carbons produced using the same silica to resorcinol molar ratio were compared, both nitrogen isotherms and electrochemical studies revealed that the SMC3 carbons exhibit simpler pore connectivity than SMC1 carbons.     

Direct fabrication of mesoporous carbons using in-situ polymerized silica gel networks as a template

Mesoporous carbons were synthesized by in-situ polymerized silica gel networks as a template. The co-condensation of carbon precursor (sucrose) and silica precursor (sodium silicate) followed by heat treatment generated a carbon/silica nanocomposite. After etching the silica template, mesoporous carbons were obtained. Under optimum synthesis conditions a mesoporous carbon with a high surface area of >800 m²/g and a narrow pore size distribution centered at 3 nm was produced. The three-dimensionally interconnected silica structures effectively functioned as the template for the porous carbon materials.     

Titanium carbide derived nanoporous carbon for energy-related applications

High surface area nanoporous carbon has been prepared by thermo-chemical etching of titanium carbide TiC in chlorine in the temperature range 200-1200 °C. Structural analysis showed that this carbide-derived carbon (CDC) was highly disordered at all synthesis temperatures. Higher temperature resulted in increasing ordering and formation of bent graphene sheets or thin graphitic ribbons. Soft X-ray absorption near-edge structure spectroscopy demonstrated that CDC consisted mostly of sp² bonded carbon. Small-angle X-ray scattering and argon sorption measurements showed that the uniform carbon-carbon distance in cubic TiC resulted in the formation of small pores with a narrow size distribution at low synthesis temperatures; synthesis temperatures above 800 °C resulted in larger pores. CDC produced at 600-800 °C show great potential for energy-related applications. Hydrogen sorption experiments at −195.8 °C and atmospheric pressure showed a maximum gravimetric capacity of ∼330 cm³/g (3.0 wt.%). Methane sorption at 25 °C demonstrated a maximum capacity above 46 cm³/g (45 vol/vol or 3.1 wt.%) at atmospheric pressure. When tested as electrodes for supercapacitors with an organic electrolyte, the hydrogen-treated CDC showed specific capacitance up to 130 F/g with no degradation after 10 000 cycles.     

Hollow porous carbon microspheres obtained by the pyrolysis of TiO2/poly(furfuryl alcohol) composite precursors

Disordered carbon materials with high porosity were prepared through the pyrolysis of TiO₂/poly(furfuryl alcohol) composites, obtained by the sol-gel method. The composites were prepared starting from titanium tetra-isopropoxide (TTIP) and furfuryl alcohol (FA) as precursors. Two different synthetic procedures for our composites were carried out, based on the addition of furfuryl alcohol (FA) before or after the TiO₂ nanoparticles formation. Also, different TTIP/FA ratio was tested. The hybrid materials obtained by both synthetic routes were pyrolyzed, under argon flow, at 900 °C producing novel TiO₂/carbon composites. All samples were characterized by XRD, FT-IR, DR-FTIR, Raman spectroscopy and TEM. Results indicated the effective FA polymerization on TiO₂ (anatase) nanoparticles, and polymer conversion to disordered carbon after the pyrolysis, simultaneously with TiO₂ anatase-rutile phase transition. The resulting TiO₂/carbon composites were treated with HF solution aiming the oxide dissolution, yielding an extremely porous carbon material as insoluble fraction. The morphology of these porous carbon materials is strongly dependent on the synthetic route adopted for the composite precursor, varying from carbon foam to highly ordered hollow microspheres.     

Templated synthesis of mesoporous carbon from sucrose—the way from the silica pore filling to the carbon material

Mesoporous carbon materials were synthesized using sucrose as carbon precursor and commercial silica as template. Every step of the synthesis such as pore filling, loss of carbon precursor during carbonization and development of the carbon pore system during silica removal have been investigated in detail. As a criterion for the quality of the obtained carbon materials, the pore size distribution estimated by applying density functional theory was used.