Preparation of Monodisperse Silica Mesoporous Microspheres with Narrow Pore Size Distribution.

The purpose of this study is to prepare monodisperse silica mesoporous microspheres with narrow pore size distribution to promote their application in the field of liquid chromatography. An improved emulsion method was used to prepare silica mesoporous microspheres, and the rotary evaporation temperature, emulsification speed, dosage of porogen DMF, and dosage of the catalyst NH3·H2O were optimized. Subsequently, these microspheres were respectively treated by alkali-heating, calcination, and sieving. The D50 (particle size at the cumulative particle size distribution percentage of 50%) of as-prepared silica mesoporous microspheres is 26.3 µm, and the D90/D10 (the ratio of particle size at a cumulative particle size distribution percentage of 90% to a cumulative particle size distribution percentage of 10%) is 1.94. The resultant silica mesoporous microspheres have distinctive pore structures, with a pore volume of more than 1.0 cm3/g, an average pore size of 11.35 nm, and a median pore size of 13.4 nm. The silica mesoporous microspheres with a large particle size, uniform particle size distribution, large average pore size and pore volume, and narrow mesopore size distribution can basically meet the requirements of preparative liquid chromatographic columns.

Microstructure and Properties of Hot Pressing Sintered SiC/Y3Al5O12 Composite Ceramics for Dry Gas Seals.

Silicon carbide (SiC) ceramics with high bending strength were prepared by hot pressing sintering (HPS) with yttrium aluminum garnet (Y3Al5O12, YAG) as sintering additive, and the effects of YAG content and sintering temperature on the sintering behavior, microstructure and mechanical properties of SiC ceramics were investigated in detail. The uniform distribution of YAG to form a liquid phase and the driving force provided by hot pressing sintering decrease the sintering temperature, improve the densification of SiC ceramics, and refine the crystal size. By means of suitable sintering conditions with the additional amount of YAG of 5 wt%, the sintering temperature of 1950 °C and a pressure of 30 MPa, the resultant SiC/YAG composite ceramics possesses high sintering and mechanical properties with the relative density of 98.53%, the bending strength of 675 MPa, the Vickers hardness of up to 17.92 GPa, and the elastic modulus of 386 GPa. The as-prepared SiC/YAG composite ceramics are promisingly used as the dry gas seal materials in the centrifugal compressors.

Cost-Effective Preparation of Hydrophobic and Thermal-Insulating Silica Aerogels.

The aim of this study is to reduce the manufacturing cost of a hydrophobic and heat-insulating silica aerogel and promote its industrial application in the field of thermal insulation. Silica aerogels with hydrophobicity and thermal-insulation capabilities were synthesized by using water-glass as the silicon source and supercritical drying. The effectiveness of acid and alkali catalysis is compared in the formation of the sol. The introduction of sodium methyl silicate for the copolymerization enhances the hydrophobicity of the aerogel. The resultant silica aerogel has high hydrophobicity and a mesoporous structure with a pore volume exceeding 4.0 cm3·g-1 and a specific surface area exceeding 950 m2·g-1. The obtained silica aerogel/fiber-glass-mat composite has high thermal insulation, with a thermal conductivity of less than 0.020 W·m-1·K-1. The cost-effective process is promising for applications in the industrial preparation of silica aerogel thermal-insulating material.

Sulfur-Assisted Surface Modification of Lithium-Rich Manganese-Based Oxide toward High Anionic Redox Reversibility.

Energy storage via anionic redox provides extra capacity for lithium-rich manganese-based oxide cathodes at high voltage but causes gradual structural collapse and irreversible capacity loss with generation of On - (0 ≤ n < 2) species upon deep oxidation. Herein, the stability and reversibility of anionic redox reactions are enhanced by a simple sulfur-assisted surface modification method, which not only modulates the material's energy band allowing feasible electron release from both bonding and antibonding bands, but also traps the escaping On - via an as-constructed SnS2- x - σ Oy coating layer and return them to the host lattice upon discharge. The regulation of anionic redox inhibits the irreversible structural transformation and parasitic reactions, maintaining the specific capacity retention of as-modified cathode up to 94% after 200 cycles at 100 mA g-1 , along with outstanding voltage stability. The reported strategy incorporating energy band modulation and oxygen trapping is promising for the design and advancement of other cathodes storing energy through anion redox.

Construction of an Amethyst-like MoS2@Ni9S8/Co3S4 Rod Electrocatalyst for Overall Water Splitting.

Transition metal sulphide electrocatalytic materials possess the bright overall water-splitting performance of practical electrocatalytic technologies. In this study, an amethyst-like MoS2@Ni9S8/Co3S4 rod electrocatalyst was constructed via a one-step hydrothermal method with in-situ-grown ZIF-67 nanoparticles on nickel foam (NF) as a precursor. The rational design and synthesis of MoS2@Ni9S8/Co3S4 endow the catalyst with neat nanorods morphology and high conductivity. The MoS2@Ni9S8/Co3S4/NF with the amethyst-like rod structure exposes abundant active sites and displays fast electron-transfer capability. The resultant MoS2@Ni9S8/Co3S4/NF exhibits outstanding hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) electrocatalytic activities, with low overpotentials of 81.24 mV (HER) at 10 mA cm-2 and 159.67 mV (OER) at 50 mA cm-2 in 1.0 M KOH solution. The full-cell voltage of overall water splitting only achieves 1.45 V at 10 mA cm-2. The successful preparation of the amethyst-like MoS2@Ni9S8/Co3S4 rod electrocatalyst provides a reliable reference for obtaining efficient electrocatalysts for overall water splitting.

The Voltage-Adaptive Effect in Lithium-Sulfur Batteries Integrated with an Electron-Conductive Interlayer.

Lithium-sulfur (Li-S) batteries are considered as one of the top competitors to go beyond Li-ion batteries. However, the shuttle effect triggered by soluble lithium polysulfides (LPSs) brings great troubles for understanding the solid-liquid-solid conversion process of the sulfur cathode. Herein, a new characterization technique is developed to deepen the understanding of such soluble LPSs shuttling, by integrating an electron-conductive interlayer. The voltage of the interlayer exhibits a voltage-adaptive effect to the cathode, indicating the true dependence of the open-circuit voltages on the LPSs instead of on the solid cathodes. Furthermore, a quantitative method can be introduced to monitor the shuttling LPSs by such interlayer design, and it shows great potential to be a new standard technique, providing direct comparison of the shuttle effect between different studies. The newly developed interlayer design paves an avenue to gain new insight into the reaction process and improve the performance of Li-S batteries.

Facile Preparation of Cellulose Aerogels with Controllable Pore Structure.

Cellulose aerogels are the latest generation of aerogels and have also received extensive attention due to their renewable and biocompatible properties. Herein, cellulose aerogel was facilely prepared by using NaOH/urea solution as solvent, raising the temperature to control gelation and drying wet gel sequentially. With NaOH/urea solution as solvent, the cellulose concentration has an important impact on the micromorphology of cellulose aerogels, while the aging time rarely affects the micromorphology. The appropriate solvent and drying method allow the formation of different cellulose crystalline structures. Different from the Cellulose Ⅰ crystalline structure of raw cellulose powder, the cellulose phase of as-prepared cellulose aerogels belongs to the Cellulose Ⅱ crystalline structure, and to some extent the pyrolysis temperature is also lower than that of raw cellulose powder. The resultant cellulose aerogel prepared by using NaOH/urea solution as solvent and freeze-drying has a uniform macroporous structure with a macropore size of 1~3 µm.

Construction of Macroporous Co2SnO4 with Hollow Skeletons as Anodes for Lithium-Ion Batteries.

Increasing the energy density of lithium-ion batteries (LIBs) can broaden their applications in energy storage but remains a formidable challenge. Herein, with polyacrylic acid (PAA) as phase separation agent, macroporous Co2SnO4 with hollow skeletons was prepared by sol-gel method combined with phase separation. As the anode of LIBs, the macroporous Co2SnO4 demonstrates high capacity retention (115.5% at 200 mA·g-1 after 300 cycles), affording an ultrahigh specific capacity (921.8 mA h·g-1 at 1 A·g-1). The present contribution provides insight into engineering porous tin-based materials for energy storage.

Construction of Petal-Like Ag NWs@NiCoP with Three-Dimensional Core-Shell Structure for Overall Water Splitting.

High-efficiency, good electrical conductivity and excellent performance electrocatalysts are attracting growing attention in the field of overall water splitting. In order to achieve the desirable qualities, rational construction of the structure and chemical composition of electrocatalysts is of fundamental importance. Herein, petal-like structure Ni0.33Co0.67P shells grown on conductive silver nanowires (Ag NWs) cores as bifunctional electrocatalysts for overall water splitting were synthesized through a facile hydrothermal method and phosphorization. The resultant three-dimensional core-shell petal-like structure Ag NWs@Ni0.33Co0.67P possesses excellent catalytic activities in alkaline conditions with the overpotential of 259 mV for the oxygen evolution reaction (OER), 121 mV for the hydrogen evolution reaction (HER) and a full cell voltage of 1.64 V to reach the current density of 10 mA cm-2. Highly conductive Ag NWs as cores and high surface area petal-like Ni0.33Co0.67P as shells can endow outstanding catalytic performance for the bifunctional electrocatalyst. Thus, the synthetic strategy of the three-dimensional core-shell structure Ag NWs@Ni0.33Co0.67P considerably advances the practice of Ag NWs toward electrocatalysts.

Large-Scale Preparation of Silver Nanowire-Based Flexible Transparent Film Heaters by Slot-Die Coating.

Highly flexible silver nanowire-based transparent conductive films (AgNWs TCFs) were large-scale fabricated by slot-die coating AgNWs inks on a flexible polyethylene terephthalate (PET) substrate, and further fabricated into a transparent film heater. Appropriate flow rate, coating speed, and AgNWs concentration allow the construction of the 15 cm × 15 cm AgNW TCFs with a sheet resistance (Rs) of less than 20 Ω/sq, a transmittance (T) at 550 nm higher than 95%, and a haze less than 3.5%. The resultant AgNW TCFs heater possesses high uniformity and superior mechanical stability and can reach a Joule heating temperature of 104 °C with a voltage of 12 V. The slot-die coating method has great potential for large-scale production of AgNW based film heaters promisingly used in window defrost and deicer systems.

Rapid Preparation of Mesoporous Methylsilsesquioxane Aerogels by Microwave Heating Technology.

Microwave heating technology is known as an alternative to traditional gas and electric heating sources. In this work, mesoporous methylsilsesquioxane (MSQ) aerogels were prepared via a sol-gel process accompanied by microwave heating technology, and microwave heating was used in the gelation of sol and the drying of wet gels, respectively. The effects of hexadecyltrimethylammonium chloride (CTAC) as a surfactant and template, hydrochloric acid (HCl) as a catalyst, ethanol as a solvent, sodium hydroxide (NaOH) as a gelation agent, and microwave power on the pore structure of as-prepared MSQ aerogels were investigated in detail. Microwave heating at low power results in the acceleration of sol-gel transition and achieves the gelation within a few minutes. Appropriate amounts of chemical reagents and microwave heating at high power allow the preparation of mesoporous MSQ aerogels with a BET-specific surface area of 681.6 m2·g-1 and a mesopore size of 19 nm, and the resultant MSQ aerogel still has a BET specific surface area as high as 134 m2·g-1 after heat treatment at 600 °C for 2 h, showing high thermal stability. The MSQ aerogels/fibre composite possesses a low thermal conductivity of 0.039 W/(m·k)-1, displaying good thermal insulation. Microwave heating technology is a promising heating method for the preparation of other aerogels.

Construction and Transition Metal Oxide Loading of Hierarchically Porous Carbon Aerogels.

Hierarchically porous carbon aerogels (CAs) were prepared by organic condensation gelation method combined with atmospheric drying and pore-formation technology, followed by a carbonization process. With as-prepared CAs as substrate, the transition metal oxide nanoparticles loaded CAs composites (MnO2/Mn2O3@CA and Ni/NiO@CA) were achieved by means of liquid etching method combined with heat treatment, respectively. The catalyst, pore-forming agent and etching have important roles on the apparent density and pore structure of CAs. The hydrochloric acid (catalyst) significantly accelerates the gelation process and influences the size and distribution of macropores, whereas the addition of PEG2000 (pore-forming agent) and the etching of liquid solution leads to the formation of mesopore structure in CAs. Appropriate amounts of hydrochloric acid and PEG2000 allow the formation of hierarchically porous CAs with a BET surface area of 482.9 m2·g-1 and a macropore size of 11.3 µm. After etching and loading, the framework of CAs is etched to become a mesoporous structure, and the transition metal oxide nanoparticles can be uniformly loaded in CAs. These resultant composites have promising application in super capacitor, electrocatalysis, batteries and other fields.

Simulation of the Light Transmittance in Macroporous Silica.

This paper focuses on the light transmittance of macroporous silica as a photocatalyst carrier. In addition to the characteristics of photocatalysts, the structure of porous bulk is also important since it affects the propagation of light. Realistic porous structures are generated by a Voronoi-based approach. Four morphological parameters are highly controlled during generating, that is, porosity, coefficient of variation, diameter ratio and normalized curvature. Finite element method (FEM) is used to simulate the propagation of light in the porous models in the visible light range. The intensity shows a quadratic decrease with the increase of the depth of light propagation. The influences of the morphological parameters on the light transmittance are analysed. It turns out that the porosity has a great influence on the light transmittance while the coefficient of variation and the diameter ratio have small ones. Moreover, the influence of the normalized curvature is little. Besides, the effect of the wavelength of visible light can not be ignored. With the simulation, the depth of visible light entering the porous silica can be estimated, which is challenging to access experimentally.

Facile preparation of high conductive silver electrodes by dip-coating followed by quick sintering.

With polyol-synthesized silver nanoparticles (AgNPs) as raw materials, the silver electrodes with high conductivity were fabricated via a dip-coating method followed by sintering process, and the effects of the dip-coating and sintering process on the conductivity and surface roughness of silver electrodes were investigated in detail. The silver film with a thickness of 1.97 µm and a roughness of about 2 nm can be prepared after dip-coating at a pulling rate of 500 µm s-1 for 40 coating times. The non-conductive dip-coated silver films are transformed into conductive silver electrodes after conventional sintering in a muffle oven, infrared sintering and microwave sintering, respectively. Compared with high sintering temperature and long sintering time of conventional sintering and infrared sintering, microwave sintering can achieve quick sintering of silver films to fabricate high conductive silver electrodes. The silver electrodes with a sheet resistance of 0.75 Ω sq-1 and a surface roughness of less than 1 nm can be obtained after microwave sintering at 500 W for 50 s. The adjustable dip-coating method followed by quick microware sintering is an appropriate approach to prepare high conductive AgNPs-based electrodes for organic light-emitting diodes or other devices.

Preparation of macroporous transition metal hydroxide monoliths via a sol-gel process accompanied by phase separation.

Three-dimensional transition metal hydroxide monoliths were facilely fabricated by a sol-gel process accompanied by phase separation in the presence of polyacrylic acid (PAA) and propylene oxide (PO). In the typical ZnCl2-PAA-PO system, PAA is used as a phase separation inducer as well as a framework former to control the phase separation and the formation of macrostructures, whereas PO works as a proton scavenger to initiate the gelation of the system and freeze the macrostructures. Appropriate amount of PAA, PO and solvents allow the formation of zinc (Zn) hydroxide monolith with cocontinuous skeletons and interconnected macropores, and the construction mechanism and characteristics of macrostructure are also investigated. The resultant dried gels are amorphous Zn hydroxide monolith with a narrow macropore size distribution (~1 µm). This approach is further used to successfully prepare macroporous single or binary composite transition metal hydroxide monoliths.

Construction of Defect-Rich Ni-Fe-Doped K0.23 MnO2 Cubic Nanoflowers via Etching Prussian Blue Analogue for Efficient Overall Water Splitting.

Designing elaborate nanostructures and engineering defects have been promising approaches to fabricate cost-efficient electrocatalysts toward overall water splitting. In this work, a controllable Prussian-blue-analogue-sacrificed strategy followed by an annealing process to harvest defect-rich Ni-Fe-doped K0.23 MnO2 cubic nanoflowers (Ni-Fe-K0.23 MnO2 CNFs-300) as highly active bifunctional catalysts for oxygen and hydrogen evolution reactions (OER and HER) is reported. Benefiting from many merits, including unique morphology, abundant defects, and doping effect, Ni-Fe-K0.23 MnO2 CNFs-300 shows the best electrocatalytic performances among currently reported Mn oxide-based electrocatalysts. This catalyst affords low overpotentials of 270 (320) mV at 10 (100) mA cm-2 for OER with a small Tafel slope of 42.3 mV dec-1 , while requiring overpotentials of 116 and 243 mV to attain 10 and 100 mA cm-2 for HER respectively. Moreover, Ni-Fe-K0.23 MnO2 CNFs-300 applied to overall water splitting exhibits a low cell voltage of 1.62 V at 10 mA cm-2 and excellent durability, even superior to the Pt/C||IrO2 cell at large current density. Density functional theory calculations further confirm that doping Ni and Fe into the crystal lattice of δ-MnO2 can not only reinforce the conductivity but also reduces the adsorption free-energy barriers on the active sites during OER and HER.

Facile Synthesis of Methylsilsesquioxane Aerogels with Uniform Mesopores by Microwave Drying.

Methylsilsesquioxane (MSQ) aerogels with uniform mesopores were facilely prepared via a sol⁻gel process followed by microwave drying with methyltrimethoxysilane (MTMS) as a precursor, hydrochloric acid (HCl) as a catalyst, water and methanol as solvents, hexadecyltrimethylammonium chloride (CTAC) as a surfactant and template, and propylene oxide (PO) as a gelation agent. The microstructure, chemical composition, and pore structures of the resultant MSQ aerogels were investigated in detail to achieve controllable preparation of MSQ aerogels, and the thermal stability of MSQ aerogels was also analyzed. The gelation agent, catalyst, solvent, and microwave power have important roles related to the pore structures of MSQ aerogels. Meanwhile, the microwave drying method was found to not only have a remarkable effect on improving production efficiency, but also to be conducive to avoiding the collapse of pore structure (especially micropores) during drying. The resulting MSQ aerogel microwave-dried at 500 W possessed a specific surface area up to 821 m²/g and a mesopore size of 20 nm, and displayed good thermal stability.

Fabrication and Characterization of MSQ Aerogel Coating on ePTFE Thin Films for Cable Sheaths.

With methylsilsesquioxane (MSQ) aerogels synthesized by the sol-gel method as a raw material and Si-Ti sol as a binder, an alcohol-based aerogel slurry consisting of only MSQ aerogel and Si-Ti sol was prepared and coated on expanded polytetrafluoroethylene (ePTFE) to form an MSQ aerogel coating layer, followed by low-temperature heat treatment. The effect of Si-Ti sol content on the microstructure of the MSQ aerogel coating layer was investigated, and the properties of a typical MSQ aerogel-layer-coated ePTFE film were evaluated. The results show that Si-Ti sol has an important role in terms of film-forming capability, surface smoothness, flexibility, and powder dropping of the MSQ aerogel coating layer. With a Si-Ti sol of 10.5 wt.% content as a binder and after heat treatment at 170 °C for 30 min, the coated ePTFE flexible thin film with a layer thickness of 30 µm shows high uniformity, integrity, and electrical insulation properties, with an elongation at break decrease over 130%, a thermal conductivity of 0.1753 W/(m·K) at 25 °C, a dielectric constant of 16.5674, and a dielectric loss of 0.06369, which can be promisingly applied in cable sheaths.

Facile Synthesis of Flexible Methylsilsesquioxane Aerogels with Surface Modifications for Sound- Absorbance, Fast Dye Adsorption and Oil/Water Separation.

New flexible methylsilsesquioxane (MSQ) aerogels have been facilely prepared by a sol-gel process with methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDMS) as co-precursors, followed by surface modification and ambient pressure drying. The microstructure, mechanical properties and hydrophobicity of these MSQ aerogels after surface modifications of hexamethyldisiloxane (HMDSO) and/or hexamethyldisilazane (HMDS) were investigated in detail, and the applications of surface-modified MSQ aerogels in sound-absorbance, fast dye adsorption and oil/water separation were evaluated, respectively. The MSQ aerogels surface-modified by HMDS possess flexibility, elasticity and superhydrophobicity, and demonstrate good performance in the mentioned applications. The resultant MSQ aerogel used in sound-absorbance has high frequency (about 6 kHz) acoustic absorptivity of up to 80%, benefiting from its macroporous structure and porosity of 94%, and it also possesses intermediate frequency acoustic absorptivity (about 1 kHz) up to 80% owing to its elasticity. This MSQ aerogel can selectively separate oil from oil/water mixtures with high efficiency due to its superhydrophobicity and superlipophilicity, resulting from a lot of methyl groups, density as low as 0.12 cm³·g-1 and a water contact angle as high as 157°. This MSQ aerogel can be assembled to be a monolithic column applied for fast dye adsorption, and shows selective adsorption for anionic dyes and removal efficiency of methyl orange of up to 95%.

Facile approach for a robust graphene/silver nanowires aerogel with high-performance electromagnetic interference shielding.

Robust graphene/silver nanowires (AgNWs) hybrid aerogels were fabricated by facile processes including mixing directly, reducing, and ambient pressure drying. The mechanical properties and electromagnetic interference (EMI)-shielding performance of the resultant hybrid aerogels were investigated in detail. Because silver nanowires with a high aspect ratio have been acting as crosslinkers to bridge two-dimensional graphene sheets, a highly porous and electrically conducting framework can resist high external loading to prevent major deformation and act as an express way for electron transport. Consequently, the hybrid aerogel exhibits large mechanical strength of 42 kPa, 35 times larger than that of the neat reduced graphene oxide aerogel (1.2 kPa), which can resist great damage. More importantly, the as-prepared aerogel possesses high EMI-shielding performance of up to ∼45.2 dB due to its unique nanostructure and good electrical properties. These results indicate that graphene/AgNWs hybrid aerogel prepared using this simplified method promises to be an ideal functional component for mechanically robust and high-performance EMI-shielding nanocomposites.