具有三维贯通多级孔道结构大孔氧化铝的制备与表征

采用铝溶胶晶种引入、结合相分离的方法制备了具有三维贯通多级孔道结构的大孔氧化铝材料。采用扫描电镜（SEM）、X射线衍射（XRD）、N₂吸附-脱附、压汞、核磁共振波谱（NMR）等测试方法对所得材料进行了表征。结果表明,该氧化铝材料具有200-600 nm的均匀分布且贯通的连续大孔孔道,经550℃焙烧即可得到结晶态γ-氧化铝。大孔氧化铝比表面积达到366 m²/g,具有以5 nm及400 nm为中心的较为集中的介孔-大孔多级孔道分布。焙烧后的样品中,铝具有四、六两种配位状态。制备过程中,聚环氧乙烷（PEO）作为诱导剂引发固-液两相分离,形成具有三维贯通多级孔道结构大孔氧化铝,而凝胶中引入铝溶胶时,AlOOH晶粒与铝交联水合物均相伴生,在凝胶过程诱导铝交联水合物转变为AlOOH,最终使大孔氧化铝在较低的焙烧温度即可转化为γ-氧化铝。     

Metal-organic frameworks with a three-dimensional ordered macroporous structure: dynamic photonic materials

Tuning MOFs: When a metal-organic framework (MOF) with an ordered three-dimensional macroporous structure is integrated into a film, the resulting materials have an additional optical element, which can be used as a general and effective signal transducer. This, in combination with the hierarchical pore structure, makes these films interesting dynamic photonic materials with potential applications in sensors.     

Synthesis and electrochemical performance of three-dimensionally ordered macroporous LiCoO2

Three-dimensionally ordered macroporous (3DOM) LiCoO₂ was synthesized by colloidal crystal templating method using poly(methyl methacrylate) with the diameter of 232 nm as the template. The effects of roasting temperature on properties of LiCoO₂ cathode materials were investigated by thermogravimetric analysis (TG-DTG), scanning electron microscope, X-ray diffraction, transmission electron microscopy, and electrochemical measurements. The results indicated that the synthesized 3DOM LiCoO₂ calcined at 700 °C had better crystal framework and electrochemical properties. The 3DOM LiCoO₂ samples presented higher rate capacity compared to commercial LiCoO₂ with a specific discharge capacity of 151.2 mAh g^?1 at a current density of 1 C, and 92 % of the specific discharge capacity was retained after 50 charge–discharge cycling.     

Facile oxygen reduction on a three-dimensionally ordered macroporous graphitic C3N4/carbon composite electrocatalyst

Honeycomb catalysis: a facile oxygen reduction reaction has been observed on a graphitic C(3)N(4)/carbon catalyst with three-dimensional interconnected macropores (see picture with SiO(2) template). This material not only shows catalytic activity that is comparable to that of commercial Pt/C, but also has much higher organic-fuel tolerance and long-term stability.     

Synthesis of ordered mesoporous carbon monoliths with bicontinuous cubic pore structure of Ia3d symmetry

Large-diameter-sized mesoporous carbon monoliths with bicontinuous cubic structure of Ia3d symmetry have been synthesized by using mesoporous silica monoliths as hard templates; such carbon monoliths show potential application of advanced electrodes and electrochemical double layer capacitors.     

三维贯穿大孔氧化铝的孔道改性、表征及转化机制

利用相分离技术制备了非晶三维贯穿大孔氧化铝初始材料,然后通过氨水水热改性处理,使其大孔形态发生了显著改变,孔壁边缘生长有尺寸为50-300 nm的片状聚集体,大孔尺寸由430 nm下降到250 nm,但仍然保持蠕虫状三维贯穿且空间分布均匀的特性。改性后的氧化铝材料经550℃焙烧转化为高结晶度γ氧化铝,比表面积达到331 m²/g,具有8.9 nm及250 nm两种集中的孔径分布,L酸度及抗压强度均有所提高。研究表明,无定形水合羟基铝离子聚合物与氨水发生再水合反应生成薄水铝石中间物,因此,可在较低的焙烧温度下转晶为γ态;大孔孔壁边缘的AlOOH晶粒受NH₄⁺模板诱导作用从里向外重排形成片状聚集体,从而改变了大孔的形态。     

Electrochemical polymerization of aniline inside ordered macroporous carbon

3D ordered macroporous multicomponent composite materials have been fabricated by electrochemical deposition of aniline on the inner surface of macroporous carbon; the maximum thickness of polyaniline (PANI) deposited is dependent on the concentration of the aniline as well as the dimension of the windows in the macroporous carbon.     

Preparation and characterization of polystyrene-based monolith with ordered macroporous structure

In this paper,polystyrene-based monoliths with highly ordered macroporous structure were synthesized by using SiO₂ colloidal crystal as template.SEM observation shows that the macropores are highly ordered and are interconnected by small windows.The BET surface area of PS monolith is about 36.17 m²/g.The polymer monoliths can resist 5 MPa pressure,showing high mechanical and compressive strength.     

Fluorinated carbon with ordered mesoporous structure

Fluorination and structural change of highly ordered mesoporous carbons were studied. Mesoporous and fluorinated carbons with ordered cubic structure were synthesized and characterized with TEM, FTIR, adsorption, and EDX.     

Synthesis of an ordered macroporous carbon with 62 nm spherical pores that exhibit unique gas adsorption properties

An ordered macroporous carbon with 62 nm spherical pores was synthesized using colloidal-crystal templating and found to exhibit unique gas adsorption properties that have been so far attributed to adsorption in mesopores (size below 50 nm).     

Free-standing mesoporous carbon thin films with highly ordered pore architectures for nanodevices

We report for the first time the synthesis of free-standing mesoporous carbon films with highly ordered pore architecture by a simple coating-etching approach, which have an intact morphology with variable sizes as large as several square centimeters and a controllable thickness of 90 nm to ～3 μm. The mesoporous carbon films were first synthesized by coating a resol precursors/Pluronic copolymer solution on a preoxidized silicon wafer and forming highly ordered polymeric mesostructures based on organic-organic self-assembly, followed by carbonizing at 600 °C and finally etching of the native oxide layer between the carbon film and the silicon substrate. The mesostructure of this free-standing carbon film is confirmed to be an ordered face-centered orthorhombic Fmmm structure, distorted from the (110) oriented body-centered cubic Im3?m symmetry. The mesoporosity of the carbon films has been evaluated by nitrogen sorption, which shows a high specific BET surface area of 700 m(2)/g and large uniform mesopores of ～4.3 nm. Both mesostructures and pore sizes can be tuned by changing the block copolymer templates or the ratio of resol to template. These free-standing mesoporous carbon films with cracking-free uniform morphology can be transferred or bent on different surfaces, especially with the aid of the soft polymer layer transfer technique, thus allowing for a variety of potential applications in electrochemistry and biomolecule separation. As a proof of concept, an electrochemical supercapacitor device directly made by the mesoporous carbon thin films shows a capacitance of 136 F/g at 0.5 A/g. Moreover, a nanofilter based on the carbon films has shown an excellent size-selective filtration of cytochrome c and bovine serum albumin.     

Flexible microfluidic devices with three-dimensional interconnected microporous walls for gas and liquid applications

This article presents a simple, low-cost method of fabrication and the applications of flexible polystyrene microfluidic devices with three-dimensional (3D) interconnected microporous walls based on treatment using a solvent/non-solvent mixture at room temperature. The complete fabrication process from device design concept to working device can be completed in less than an hour in a regular laboratory setting, without the need for expensive equipment. Microfluidic devices were used to demonstrate gas generation and absorption reactions by acidifying water with carbon dioxide (CO(2)) gas. By selectively treating the microporous structures with oxygen plasma, acidification of water by acetic acid (distilled white vinegar) perfusion was also demonstrated with the same device design.     

Synthesis and characterization of three-dimensionally ordered macroporous ternary oxide

A three-dimensionally ordered macroporous (3DOM) ternary oxide, CsAlTiO₄, with a framework related to ‘stuffed-tridymite’ has been synthesized at temperatures 500-700 °C using a sol-gel precursor solution and templating with polystyrene spheres. The 3DOM material displayed pore diameters of 0.5-0.8 μm with the walls composed of anhedral and acicular CsAlTiO₄ crystals whose dimensions ranged from 16 to 25 nm. Microanalysis confirmed near-stoichiometric proportions (1:1:1) of Cs, Al and Ti. The effect of sintering temperature on the macroporous structure and on the CsAlTiO₄ walls was studied. As the sintering temperature increased from 500 to 600 °C the unit cell parameters varied through dilation (a and b) and contraction (c-axis), followed by a reversal of these trends from 700 to 900 °C. This behaviour in non-equilibrated CsAlTiO₄ can be attributed to distortion of the (Al, Ti)O₄ tetrahedral framework, however at the highest temperature the cell constants stabilized close to those reported for single crystal CsAlTiO₄. X-ray amorphous content was significant in all materials varying from 73 wt% after 500^oC and reducing to 44 wt% at 900 °C.     

Ordered porous carbon with tailored pore size for electrochemical hydrogen storage application

Ordered porous carbon with tailored pore size represents an innovative concept in electrochemical hydrogen storage. This work deals with physical characteristics and electrochemical hydrogen storage behavior of the ordered porous carbons with well-tailored pore size, synthesized by a replica technique using hexagonal mesoporous silica as templates. By using a mixture of two surfactants (HTAB and C16EO8) at different ratios, it is possible to control the wall thickness of silica and, consequently, the pore diameter of carbons within a narrow range of 2.1-2.8 nm. In addition, highly developed ultramicroporosity (pore size smaller than 0.7 nm), which plays a predominant role in hydrogen storage, can be produced in the ordered porous carbons. A discharge capacity of up to 527 mAh/g (corresponding to 1.95 wt % hydrogen storage) has been achieved in 6 M KOH for the ordered porous carbon. Furthermore, the ordered porous carbons also possess excellent capacity retainability after charge-discharge cycles and rate capability.     

Highly ordered three-dimensional macroporous FePO4 as cathode materials for lithium–ion batteries

Highly ordered three-dimensional macroporous 3DOM FePO₄ cathode material was prepared by using a colloidal crystal template. The effects of the annealing temperature on the morphology changes and the electrochemical properties of the composite were investigated. The 3DOM FePO₄ prepared at 400 °C shows the excellent cycling stability and good rate capability as a cathode for lithium–ion batteries.     

Easy synthesis of iron doped ordered mesoporous carbon with tunable pore sizes

Precise control of the pore sizes for porous carbon materials is of importance to study the confinement effect of metal particles because the pore size in nanosize range will decide the physical and chemical properties of the metal nanoparticles.In this paper,we report a new approach for the synthesis of iron doped ordered mesoporous carbon materials with adjustable pore size using Fe-SBA-15 as hard template and boric acid as the pore expanding reagent.The pore size can be precisely adjusted by a step of 0.4 nm in the range of 3-6 nm.The carbonization temperature can be lowered to 773 K due to the catalytic role of the doped iron.The present approach is suitable for facile synthesis of metal imbedded porous carbon materials with tunable pore sizes.     

Synthesis of ordered mesoporous NiO with crystalline walls and a bimodal pore size distribution

A mesoporous solid with crystalline walls and an ordered pore structure exhibiting a bimodal pore size distribution (3.3 and 11 nm diameter pores) has been synthesized. Previous attempts to synthesize solids with large ordered mesopores by hard templating focused on the preparation of templates with thick walls (the thick walls become the pores in the target materials), something that has proved difficult to achieve. Here the large pores (11 nm) do not depend on the synthesis of a template with thick walls but instead on controlling the microporous bridging between the two sets of mesopores in the KIT-6 template. Such control determines the relative proportion of the two pore sizes. The wall thickness of the 3D cubic NiO mesopore has also been varied. Preliminary magnetic characterization indicates the freezing of uncompensated moments or blocking of superparamagnetism.     

Synthesis, characterization and optical properties of ordered macroporous organosilicas

Ordered macroporous organosilica materials with uniform pore size in the range of 0.2-1.35 [micro sign]m have been fabricated by using self-assembled colloidal crystals as templates, and characterized with SEM, TGA, FTIR, MAS NMR, and optical reflectance spectrometry.