One-pot synthetic method to prepare highly N-doped nanoporous carbons for CO2 adsorption

A one-pot synthetic method was used for the preparation of nanoporous carbon containing nitrogen from polypyrrole (PPY) using NaOH as the activated agent. The activation process was carried out under set conditions (NaOH/PPY = 2 and NaOH/PPY = 4) at different temperatures in 600–900 °C for 2 h. The effect of the activation conditions on the pore structure, surface functional groups and CO₂ adsorption capacities of the prepared N-doped activated carbons was examined. The carbon was analyzed by X-ray photoelectron spectroscopy (XPS), N2/77 K full isotherms, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The CO₂ adsorption capacity of the N-doped activated carbon was measured at 298 K and 1 bar. By dissolving the activation agents, the N-doped activated carbon exhibited high specific surface areas (755–2169 m² g⁻¹) and high pore volumes (0.394–1.591 cm³ g⁻¹). In addition, the N-doped activated carbons contained a high N content at lower activation temperatures (7.05 wt.%). The N-doped activated carbons showed a very high CO₂ adsorption capacity of 177 mg g⁻¹ at 298 K and 1 bar. The CO₂ adsorption capacity was found to be dependent on the microporosity and N contents.     

Thermal conductivity anisotropy in polypropylene foams prepared by supercritical CO2 dissolution

Different relative density polypropylene foams were prepared by means of two foaming processes: chemical foaming by compression moulding and physical foaming by high pressure CO₂ dissolution. By controlling the foaming parameters, such as blowing agent concentration, foaming temperature, pressure drop and pressure drop rate, it was possible to regulate the cellular structure, foams showing from markedly isotropic-like cellular structures to ones with highly-elongated cells in the vertical foam growth direction (honeycomb-like cell orientation). The thermal conductivity was measured using the transient plane source method. Using this technique, it was possible to measure the global conductivity and the thermal conductivity in both the axial and radial directions of a given sample. Results show that the global thermal conductivity of foams was mainly regulated by their relative density. In addition, the honeycomb-like cell orientation of the CO₂ dissolution foams resulted in considerably higher values in axial direction when compared to radial, demonstrating that there was a direct influence of cellular structure on the thermal conduction behaviour of these foams, enabling the development of new polypropylene foams with direction-dependent thermal properties.     

Magnetic properties and methylene blue adsorptive performance of CoFe2O4/activated carbon nanocomposites

Owing to the unique microporous structure and high specific surface area, activated carbon (AC) could act as a good carrier for functional materials. In this paper, CoFe₂O₄/AC nanocomposites were prepared by a facile hydrothermal method for the adsorption of dyes in wastewater. The results indicated that CoFe₂O₄ nanoparticles presented the spinel structure and existed in the pores of AC. The saturation magnetization (Ms) increased with the CoFe₂O₄ content, while the surface area and pore volume decreased. For the larger magnetic moment, very few CoFe₂O₄ were needed to maintain the higher surface area of CoFe₂O₄/AC nanocomposites. The sample-5 (CoFe₂O₄:C = 1:200) possessed the surface area of 1096.85 m² g⁻¹ (close to 1243.35 m² g⁻¹ of AC) and Ms of 5.11 emu g⁻¹, which were sufficient for magnetic separation in wastewater treatment. 99% methylene blue could be adsorbed in 50 min, and then the CoFe₂O₄/AC nanocomposites could be separated from the solution easily by an outer magnet.     

Camphene-based freeze-cast ZrO2 foam with high compressive strength

Highly porous zirconia ceramic bodies with interconnected pores were fabricated by freeze-casting technique using camphene-based slurries. The pore volume fraction and pore size are controllable by adjusting the initial solid content in the mixed slurries. The pores are replicas of connected dendrites of frozen camphene, which sublimed during room temperature drying. As the solid content was increased from 10 to 20 vol.%, the compressive strength was significantly increased from 19 ± 2 to 58 ± 3 MPa, and the examined porosity was decreased from 81.5 to 66.5%. This technique is considered potentially useful in producing novel porous ceramics, and introduces a new application field of freeze-casting.     

Preparation and gases storage capacities of N-doped porous activated carbon materials derived from mesoporous polymer

In this report, the chemical activation of mesoporous carbon derived from mesoporous polymer is used to prepare N-doped carbon materials with high surface area and narrow pores size distribution. The porous carbons derived from the activation of mesoporous carbon generally possess high surface area up to 2400 m² g⁻¹ and narrow micropores/super-micropore size distribution and exhibit H₂ uptake capacity of up to 4.8 wt% at −196 °C and 20 bar and CO₂ sorption capacity of up to 3.7 mmol g⁻¹ at 25 °C and 1 bar. The measured isosteric heat of adsorption for H₂ sorption is 10 kJ mol⁻¹ and 58 kJ mol⁻¹ for CO₂ sorption, indicating a strong interaction between the carbon surface and adsorbed hydrogen and carbon dioxide respectively.     

Fabrication of porous TiO2 nanofiber and its photocatalytic activity

Porous TiO₂-based nanofiber was fabricated via a combined electrospinning and alkali-dissolution method. TiO₂/SiO₂ composite nanofiber was firstly prepared by electrospinning and sintering, and then silica was leached out with alkaline solution from the bulk of TiO₂/SiO₂ composite nanofiber to produce porous microstructure. The thermal decomposition and phase structure of the composite nanofiber precursor was investigated with TG/DSC and XRD, and optimal sintering temperature was obtained. SEM-EDX and FT-IR characterization show that most silica can be dissolved out from the composite nanofiber and thus porous nanofiber with excellent microstructure can be spontaneously formed. The effect of composite nanofiber composition on porous microstructure was studied, and it is found that the composite nanofiber with 20wt% silica can produce better porous microstructure compared to those with 10wt% and 30wt% silica. Meanwhile, porous TiO₂ nanofiber with 20wt% silica shows higher degradation efficiency to Congo Red.     

Electrophoretic technique for hydrothermal synthesis of NaA zeolite membranes on porous α-Al2O3 supports

Uniform and dense NaA zeolite membranes were prepared on the α-Al₂O₃ support by electrophoretic technique. The membrane morphology and membrane thickness were investigated by XRD, SEM and pervaporation properties for dehydration of 95 wt.% isopropanol/water mixture at 343 K, respectively. Under the action of the applied electric field, the negatively charged zeolite particles could migrate to the support surface homogenously and rapidly, forming uniform and dense membranes in a short time. High quality NaA zeolite membrane, with a separation factor (water/isopropanol) of 3281 and a flux of 1.24 kg/m² h, could be prepared by electrophoretic technique with the electrical potential of 1 V. The formation mechanism of zeolite membrane in the electric field is discussed.     

Design,preparation, and application of ordered porous polymer materials

Ordered porous polymer (OPP) materials have extensively application prospects in the field of separation and purification, biomembrane, solid supports for sensors catalysts, scaffolds for tissue engineering, photonic band gap materials owing to ordered pore arrays, uniform and tunable pore size, high specific surface area, great adsorption capacity, and light weight. The present paper reviewed the preparation techniques of OPP materials like breath figures, hard template, and soft template. Finally, the applications of OPP materials in the field of separation, sensors, and biomedicine are introduced, respectively.     

Layered H2K2Nb6O17 exfoliation promoted by n-butylamine

We have been exploring experimental conditions to achieve the exfoliation of the layered niobate phase K₄Nb₆O₁₇ using alkyl amines. In this work, the exfoliation process of the niobate acidic form H₂K₂Nb₆O₁₇ was evaluated in aqueous solution media using n-butylamine. Different amine/H⁺-niobate molar ratios were used and for each one, two fractions were isolated: one that corresponds to the deposited solid (or sediment) and the second one that consists of an aqueous colloidal dispersion. Fractions were characterized by X-ray powder diffraction, electronic absorption spectroscopy and, scanning and transmission electron microscopies. It was observed that the hexaniobate exfoliation is very dependent on the amine/H⁺-niobate molar ratio utilized. The highest amount of exfoliated niobate particles was achieved by using a butylamine/H⁺-niobate molar ratio around 0.5. High molar ratios promote the intercalation preferred to the delamination, indicating that the interlayer region saturation precludes the hexaniobate sheets exfoliation. TEM images of delaminated sample showed nanosized particles with flat and tubular morphologies.     

Fabrication and characterization of gridded Pt/SiO2/Si MOS structure for hydrogen and hydrogen sulphide sensing

A gridded gate Pt/SiO₂/Si MOS capacitor has been fabricated for detection of Hydrogen (H₂) and Hydrogen Sulphide (H₂S) gases. The MOS device was fabricated on P-type Si <100> (1–6 Ω cm) wafer with thermal oxide layer of thickness about 100 Å, whereas, Platinum (Pt) gate of ∼350 Å was deposited by thermal evaporation technique. The C–V (capacitance vs voltage) and G–V (conductance vs voltage) measurements have been performed for the evaluation of gas sensing behavior of fabricated MOS capacitor structure in H₂ (250–4000 ppm) and H₂S (1000–6000 ppm) gases at both room and 120 °C temperatures, in a closed chamber in air atmosphere. It has been observed that the value of capacitance decreases with increase in gas concentration. The fabricated MOS capacitor sensor has shown better sensitivity towards H₂ (88.6%) at room temperature (∼25 °C) as compared to (∼45%) at 120 °C. Scanning electron microscopy (SEM) and Atomic force microscopy (AFM) studies have revealed the porous nature of the deposited metal film. The side wall diffusion, spillover of Hydrogen into oxide layer, increase in fixed oxide charge density, increase in surface area caused by gridded structure, the formation of dipole layer and change in interface state density on gas exposure, may be the mechanisms of gas sensing for improved sensitivity of the fabricated MOS device.     

Fast and efficient synthesis of ZSM-5 in a broad range of SiO2/Al2O3 without using seeding gel

ZSM-5 zeolite were synthesized in a wide range of SiO₂/Al₂O₃ molar ratios at temperature ranging from 220 to 230 °C without adding seeding gel in 4-6 h of autoclavation time.     

One-pot synthesis of hierarchically macro/mesoporous Al2O3 monoliths from a facile sol–gel process

Based on the preparation of ordered mesoporous Al₂O₃ powder using P123/isopropoxide aluminum/HNO₃ reaction system, hierarchically macro/mesoporous alumina monoliths were successfully fabricated by introducing PEG8000 as the phase-segregation initiator to generate macropores. The effects of PEG8000 and P123 contents on the monolithic and hierarchical morphology were investigated systematically. With appropriate selection of the starting composition, monolithic skeletons with bimodal macropores interconnected by mesostructured walls can be synthesized in both the dried gels and calcined samples. The well-defined macropores are in close-celled structure dispersed in large-sized mesoporous matrix. The mesopore size can be regulated by adjusting the PEG8000 content while its shape is governed by P123 content. The well-developed alumina monolith, MMA-P20, exhibits high surface area of 287 m²/g and narrowly distributed mesopores with median size of 13 nm after calcinaton.     

Effect of ZrO2 addition on crystallization behaviour, porosity and chemical-mechanical properties of a CaO-TiO2-P2O5 microporous glass ceramic

2-6 mol% ZrO₂ was added to a base glass composition of P₂O₅ 31.25, CaO 43.75, TiO₂ 25 (mol%) at the expense of TiO₂. The prepared glasses were crystallized to bulk glass ceramics containing the major phases of β-Ca₃(PO₄)₂ and CaTi₄(PO₄)₆. DTA was utilized to determine the appropriate phase separation-nucleation and crystallization temperatures. The crystalline products and resulting microstructures were examined by XRD and SEM. The β-Ca₃(PO₄)₂ phase was dissolved out by leaching the resulting glass ceramics in HCl, leaving a porous skeleton of CaTi₄(PO₄)₆. It was shown that ZrO₂ addition resulted in reduction of volume porosity and mean pore diameter while the specific surface area was increased. The smallest median pore diameter and largest surface area were 8.6 nm and 32 m² g⁻¹ respectively obtained for the specimen containing 6 mol% ZrO₂. The ZrO₂ addition also improved the chemical durability and bending strength of porous glass ceramics.     

Preparation and characterization of TiO2 nanosponge

A procedure was developed to coat functionalized polystyrene spheres with well-defined layer of amorphous titanium dioxide. The core–shell particles can be turned into TiO₂ nanosponge by calcining the dried particles in a furnace. The phase transformation temperature of TiO₂ hybrid microspheres from anatase to rutile was increased by about 200 °C due to the blocking function of the calcined polymer remainder.     

Facile fabrication of ZrO2 hollow porous microspheres with yeast as bio-templates

ZrO₂ hollow porous microspheres have been fabricated successfully using living yeast cells as bio-templates through a facile ageing process at lower crystallizing temperature. XRD, SEM, FT-IR and N₂ adsorption-desorption were used to characterize ZrO₂ hollow microspheres. The results showed that the inorganic-organic hybrid hollow microspheres were fabricated at 100 °C and ZrO₂ hollow microspheres with tetragonal phase and porous structure were obtained at 300 °C. The crystallization temperature of ZrO₂ decreased obviously due to the inducting of bio-molecules. The as-prepared hollow microspheres are approximately ellipsoid. The shells of these hollow microspheres are porous, which are composed of some nanoparticles with size of ∼20 nm. The formation mechanism of ZrO₂ hollow microspheres was proposed and discussed tentatively.     

Preparation and characterization of porous ultrafine Fe2O3 particles

Porous ultrafine Fe₂O₃ particles were prepared by homogeneous precipitation method. Fe³⁺ and urea were chosen as starting materials and anionic surfactant as the template. It is shown that the reaction results in the precipitation of a gelatinous hydrous iron oxide/surfactant mixture, which gives ultrafine Fe₂O₃ particles after drying and calcinations. The products were characterized by XRD, TEM, TG/DTA and BET. Conventional XRD patterns show that the products are mixture of γ-Fe₂O₃ and α-Fe₂O₃ phase after being sintered at 350 °C, and γ-Fe₂O₃ transforms entirely to α-Fe₂O₃ when sintered at 650 °C. The low-angle XRD patterns indicate that the mesostructure can only exist between 350 and 400 °C. TEM results show that the Fe₂O₃ particles have diameters of about 30 nm and lengths ranging from 100 to 120 nm; in each particle, there are several vermiculate-like mesopores with diameter of about 20-25 nm. The BET surface areas in excess of 50 m²/g are obtained after calcinations at 350 °C. The BJH desorption average pore width is around 22 nm, which is in agreement with the TEM results. The results show that anionic surfactant and sintering temperature are important to obtain this special morphology.     

Polyethyleneimine-loaded bimodal porous silica as low-cost and high-capacity sorbent for CO2 capture

In this work, bimodal (meso-macro) porous silicas with different mesopore diameters synthesized by using rice husk ash as a low-cost silica source and chitosan as a natural template were used as a polyethyleneimine (PEI) support for CO₂ capture. Unimodal porous silica supports with equivalent mesopore diameters to bimodal porous silica supports have been prepared for purpose of comparison. Effects of different PEI contents (10, 20, 30, 40 and 50 wt%) on CO₂ sorption capacity have been systematically investigated. The porous silica supports and the PEI-loaded porous silica supports were characterized by N₂-sorption analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and thermal gravimetric analysis. CO₂ sorption measurements of all PEI-loaded porous silica supports were performed at different adsorption temperatures (60, 75, 85, 90, 95 and 105 °C). At low PEI contents (10–20 wt%), the CO₂ sorption of all adsorbents was found to decrease as a function of adsorption temperature, which was a characteristic of a thermodynamically-controlled regime. A transition from the thermodynamically-controlled regime to a kinetically-controlled regime was found when the PEI content was increased up to 30 wt% for PEI-loaded unimodal porous silicas and 40 wt% for PEI-loaded bimodal porous silicas. At high PEI contents (40–50 wt%), the CO₂ capturing efficiency of the PEI-loaded bimodal porous silicas was found to be considerably greater than that of the PEI-loaded unimodal porous silicas, indicating that most of the amine groups of PEI molecules loaded on the unimodal porous silica supports was useless, and thus the appeared macroporosity of the bimodal porous silica supports could provide a higher effective amine density to adsorb CO₂.     

Preparation of granular X-type zeolite/activated carbon composite from elutrilithe by adding pitch and solid SiO2

The preparation of granular X-type zeolite/activated carbon composites from a locally available elutrilithe by adding pitch powder and solid SiO₂ was studied, and the variations in the synthesis process of zeolite X were investigated. The preparation steps of the composite involved (1) calcination of pre-shaped mixture (2) activation of the carbonaceous material from elutrilithe and pitch to prepare activated carbon and (3) hydrothermal conversion (zeolitisation) of aluminosilicate in elutrilithe and additional SiO₂ to zeolite X in alkaline medium. The adding of additional SiO₂ in the reaction system to adjust SiO₂/Al₂O₃ ratio of the reaction mixture was necessary for the formation of zeolite X. The characterization of XRD, SEM and N₂ adsorption of the resulting composites had a hierarchical pore structure, which shows that pure X-type zeolite phase with high crystallinity could be obtained regardless of the content of carbon in the composites.     

Several shape-controlled TiO2/TiB2 hybrid materials with a combined growth mechanism

Several kinds of TiO₂/TiB₂ hybrid materials with different morphologies, including hollow bipyramid structure with truncations, pineapple structure, urchin structure and nanowall structure, have been successfully synthesized by a facile solvothermal approach in the aqueous solution of ethylenediamine. The effect of ethylene ediamine on the shape change of the final products was investigated in detail. With the increase of ethylenediamine, anatase TiO₂ on the TiB₂ core is gradually evolved from nanoparticles, nanorods to nanosheets. Based on attachment theory, Oswald ripening phenomenon, chelating effect and Kirkendall effect, a possible formation mechanism for such TiO₂/TiB₂ hybrid materials was proposed to explain the morphology evolution.     

Fabrication and characterization of porous unidirectional Si2N2O-Si3N4 composite

Porous unidirectional Si₂N₂O-Si₃N₄ composite was fabricated by in-situ nitriding of a porous unidirectional Si substrate. The porous unidirectional Si substrate having a diameter of 450 μm, was prepared by forming ethanol bubbles in a slurry which contained Si, Y₂O₃, Al₂O₃ and methylcellulose powder. After nitridation at 1400 °C, the Si substrate was transformed into Si₂N₂O-Si₃N₄ composite and the pore surface of the unidirectional Si₂N₂O-Si₃N₄ composite was covered throughout with Si₂N₂O fibers, which had a diameter of about 55 nm. The Si₂N₂O fibers were orthorhombic single-crystals with an amorphous layer having a thickness of about 1 nm. The compressive strength of the in-situ synthesized Si₂N₂O-Si₃N₄ composite was about 30 MPa.