Fabrication and characterization of highly ordered Ni_(0.5)Zn_(0.5)Fe_2O_4 nanowire/tube arrays by sol-gel template method

Highly ordered nanowire/tube arrays of Ni0.5Zn0.5Fe2O4were fabricated by the sol-gel method in the pores of anodic alumina membrane （AAM）. Whether nanowires or nanotubes were fabricated depends on immersion time. The immersion time was 15- 40 s for nanotubes and over 60 s for nanowires. The topography and crystalline structure of the nanowire arrays were characterized by scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, and X-ray diffraction （XRD）. It was found that the length and diameter of the Ni0.5Zn0.5Fe2O4 nanowires are related to the thickness of the AAM and the diameter of the pores. The results indicated that the Ni0.5Zn0.5Fe2O4 nanowires are uniform and parallel to each other.

Template synthesis of copper azide primary explosive through Cu2O@HKUST-1 core-shell composite prepared by “bottle around ship” method

Copper azide(CA), as a primary explosive with high energy density, has not been practically used so far because of its high electrostatic sensitivity. The Cu2O@HKUST-1 core-shell structure hybrid material was synthesized by the “bottle around ship” methodology in this research by regulating the dissolution rate of Cu2O and the generation rate of metal-organic framework(MOF) materials. Cu2O@HKUST-1 was carbonized to form a Cu O@porous carbon(CuO@PC) composite material. CuO@PC was synthesized into a copper azide(CA) @PC composite energetic material through a gas-solid phase in-situ azidation reaction.CA is encapsulated in PC framework, which acts as a nanoscale Faraday cage, and its excellent electrical conductivity prevents electrostatic charges from accumulating on the energetic material’s surface. The CA@PC composite energetic material has a CA content of 89.6%, and its electrostatic safety is nearly 30times that of pure CA(1.47 mJ compared to 0.05 mJ). CA@PC delivers an outstanding balance of safety and energy density compared to similar materials.

Synthesis and Characterization of Hollow Strontium Carbonate Pompons by Composite Soft Template Method

The hollow strontium carbonate pompons was synthesized for the first time by a controlled reaction precipitation method with sodium dodecyl benzene sulfonate(SDBS)and polyvinyl pyrrolidone(PVP)work together as template.The sampled particles were characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),nitrogen adsorption-desorption measurement,X-ray diffraction(XRD),Energy dispersive X-Ray spectroscopy(EDX),Fourier transform infrared spectroscopy(FTIR),Thermogravimetric analysis and differential scanning calorimetry(TGA-DSC),etc.It is shown that the assynthesized hollow strontium carbonate pompons with the size of about 2μm consist of flake-like particles under the optimal reaction conditions.The formation mechanism of hollow strontium carbonate pompons was preliminarily explored.

Fabrication and Characterization of LiFePO4 Nanotubes by a Sol-gel-AAO Template Process

The LiFePO4 nanotubes were successfully fabricated by a sol-gel method with porous anodic aluminum oxide as the template. Transmission electron microscopy and scanning electron microscopy showed that the synthesized LiFeP04 nanotubes were monodispersed and parallel to one another. Selected area electron diffraction pattern, X-ray diffraction and X-ray photoelectron spectroscopy investigations jointly demonstrated that the synthesized LiFePO4 nanotubes were pure olivine structure. This approach offered a potentially way for fabricating ordered LiFePO4 nanotubes at room temperature and ambient conditions, which might be expected to find promising application as a new cathode material in lithium ion battery,

Comparative structural and electrochemical properties of mixed P2/O′3-layered sodium nickel manganese oxide prepared by sol-gel and electrospinning methods:Effect of Na-excess content

The effect of Na-excess content in the precursor on the structural and electrochemical performances of sodium nickel manganese oxide(NNMO)prepared by sol-gel and electrospinning methods is investigated in this paper.X-ray diffraction results of the prepared NNMO without adding Na-excess content indicate sodium loss,while the mixed phase of P2/O′3-type layered NNMO presented after adding Na-excess content.Compared with the sol-gel method,the secondary phase of NiO is more suppressed by using the electrospinning method,which is further confirmed by field emission scanning electron microscope images.N_(2) adsorption-desorption isotherms show no remarkably difference in specific surface areas between different preparation methods and Na-excess contents.The analysis of X-ray absorption near edge structure indicates that the oxidation states of Ni and Mn are+2 and+4,respectively.For the electrochemical properties,superior electrochemical performance is observed in the NNMO electrode with a low Na-excess content of 5wt%.The highest specific capacitance is 36.07 F·g^(-1)at0.1 A·g^(-1)in the NNMO electrode prepared by using the sol-gel method.By contrast,the NNMO electrode prepared using the electrospinning method with decreased Na-excess content shows excellent cycling stability of 100%after charge-discharge measurements for 300 cycles.Therefore,controlling the Na excess in the precursor together with the preparation method is important for improving the electrochemical performance of Na-based electrode materials in supercapacitors.

SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

Synthesis of mesoporous carbon as electrode material for supercapacitor by modified template method

The pore structures and electrochemical performances of mesoporous carbons prepared by silica sol template method as electrode material for supercapacitor were investigated. The mean pore size and mass specific capacitance of the mesoporous carbons increase with the increase of mass ratio of silica sol to carbon source （glucose）. A modified template method, combining silica sol template method and ZnCl2 chemical activation method, was proposed to improve the mass specific capacitance of the mesoporous carbon with an improved BET surface area. The correlation of rate capability and pore structure was studied by constant current discharge and electrochemical impedance spectroscopy. A commercially available microporous carbon was used for comparison. The result shows that mesoporous carbon with a larger pore size displays a higher rate capability. Mesoporous carbon synthesized by modified template method has both high mass specific capacitance and good rate capability.

Template Polymerization Based on Stober Method:an Improved Method for Fabrication of Hollow Polysiloxane Spheres

A modified Stober method has been developed which permits the controlled growth of spherical hollow spheres with diameters between 197 and 208 nanometers by consecutively cocondensed methyltrimethoxysilane and dimethyldimethoxysilane monomers onto microemulsion of polydimethylsiloxane and subsequently removing the templated polydimethylsiloxane by exposure to solvents. Ammonia was used as a morphological catalyst. The morphology of the polymer spheres was demonstrated by transmission electron micrographs （TEM） and atomic force microscopy （AFM）.

Sol-Gel Template Synthesis and Photocatalytic Activity of TiO_2 Nanofibrils Loaded on Al_2O_3 Template

TiO2 nanofibrils were prepared within the pores of alumina template membrane by use of sol-gel chemistry. The TiO2 nanofibrils have good crystallinity and size. There is agglomeration free among the particulates of TiO2 and the fibrils show high catalytic activity.

Preparation and Characterization of Polyaniline Nanofibers by Template-free Method

In the presence of p-toluene sulfonic acid (TSA) as a dopant, polyaniline (PAni) nanofibers, (about 80^-65 nm in diameter) were successfully synthesized with a chemical template-free method. It was found that the formation probability, morphology, and diameter of the resulting PAni-TSA nanofibers were sensitive to the synthetic conditions, such as reaction temperature, the molar ratio of TSA to aniline, and the concentration of TSA in the polymerization media. The molecular structure was characterized by using the FT-IR, Raman spectra and X-ray diffraction, which shows that the main chain structure of PAni-TSA nanofibers was in agreement with that of granular PAni.

Structures and Properties of PEDOT Nanotubes Prepared by a Template Synthesis Method

PEDOT nanotubes were prepared by a template synthesis method. Based on our template, it was deduced that there are two successive processes in the formation of nanotubes. The first step is soakage of the porous templates by a polymer solution, and the second step is adsorption of free charged cationic groups and doped PEDOT onto the template surface with negative charges. XRD results showed that well orientated PEDOT chains were formed during the synthesis, moreover the arrange conductivity of molecular chains strongly affect the structures of PEDOT nanotubes. The nanotubes were measured to be about 5.5-17.6 S/cm, which is higher than that of nanotube pellet due to the high contact resistance between the adjacent nanotubes.

Sol-gel synthesis of nanometer silicon/silicon suboxide/carbon anode material

A stacked Si/SiO_(x)/C composite anode material with carbon-coated structure was prepared by sol-gel method combined with carbothermal reduction using organic silicon.The results of X-ray diffractometry, scanning electron microscopy, and elemental analysis show that the Si/SiO_(x)/C material is a secondary particle with a porous micronanostructure, and the presence of nanometer silicon does not affect the carbothermal reduction and carbon coating.Electrochemical test results indicate that the specific capacity and first coulombic efficiency of SiO_(x)/C composite with nanometer silicon can be increased to 1 946.05 mAh/g and 76.49%,respectively.The reversible specific capacity of Si/SiO_(x)/C material blended with graphite is 749.69 mAh/g after 100 cycles at a current density of 0.1 C,and the capacity retention rate is up to 89.03%.Therefore, the composite has excellent electrochemical cycle stability.

A Method for Preparation of Ordered Porous Silicon Based on a 2D SiO_2 Template

A new method for fabricating ordered porous silicon is reported. A two-dimensional silica nanosphere array is used as a template with a hydrofluoric acid-hydrogen peroxide solution for etching the nanospheres. The initial diameter and distribution of the holes in the resulting porous silicon layer are determined by the size and distribution of the silica nanospheres. The corrosion time can be used to control the depths of the holes. It is found that the presence of a SiO2 layer, formed by the oxidation of the rough internal surface of the hole, is the primary reason allowing the corrosion to proceed. Ultraviolet reflection and thermal conductivity measurements show that the diameter and distribution of the holes have a great influence on properties of the porous silicon.

Preparation of ZrO_(2) Fibers by Template Impregnation Method

Viscose fiber templates(15 cm×15 cm×1 cm)were put into ZrOCl_(2) solutions of different concentrations(1,2 and 3 mol·L^(-1))and impregnated at different temperatures(20,40 and 60℃)for 20 h.After washing,centrifugation and drying,ZrO_(2) fiber precursors were obtained.ZrO_(2) fibers were prepared by heat treatment of the precursors at different temperatures(600,800,1000 and 1200℃)for 2 h.The effects of the impregnation temperature,the impregnation solution concentration and the heat treatment temperature on the microstructure and the phase composition of the ZrO_(2) fibers were studied.The results show that with the increase of the impregnation temperature from 20℃to 60℃and the impregnation solution concentration increase from 1 mol·L^(-1) to 3 mol·L^(-1),the microstructure of fiber cross section changes from flat to cylindrical,and the average fiber diameter increases,indicating that the increase of the impregnation solution concentration and the impregnation temperature is beneficial to increasing the adsorption capacity of Zr4+on viscose fiber templates.After heat treatment,ZrO_(2) fiber mainly exists in the form of monoclinic ZrO_(2).With the increase of the heat treatment temperature,the grains in ZrO_(2) fibers become larger and the crystallinity degree increases,meanwhile the fiber surface undergoes a transition from smooth to small grains and then to cracks.

Preparation of long alumina fibers by sol-gel method using malic acid

The precursor sol of alumina was prepared by sol-gel method with aluminum nitrate and malic acid as raw materials.The effects of content of malic acid and polyvinylpyrrolidone （PVP） on sol spinnability were explored.The gel fibers with above 80 cm in length were obtained by mixing aluminum nitrate,malic acid and PVP on mass ratio of 10 3 1.5.Thermogravimetry-differential scanning calorimetry （TG-DSC）,Fourier transform infrared （FTIR） spectrum,X-ray diffractometry （XRD）,and scanning electron microscopy （SEM） were used to characterize the properties of the gel and ceramic fibers.The alumina fibers with a smooth surface and about 20μm in diameter were obtained by sintering at 1 200℃,and their main phase was indentified to be α-Al2O3.

A Novel Approach to Synthesizing Porous ZnO Films: Inorganic Chelating Sol-Gel Method

Porous ZnO films are synthesized by inorganic chelating sol-gel method,which is a novel sol-gel technique using zinc nitrate as starting materials and citric acid as the chelating reagent.The crystal structure,surface morphology,porous and optical properties of the deposited films are investigated.X-ray diffraction pattern analysis shows that crystal structure of the ZnO films is hexagonal wurtzite.Scanning electron microscopy (SEM) shows that the ZnO film is porous.The curve of pore size distribution has two peak values at about 2.02nm and 4.97nm and BET surface area of the ZnO film is 27.57m2/g.In addition,the transmittance spectrum gives a high transmittance of 85% in the visible region and optical bandgap of the ZnO film (fired at 500℃) is 3.25eV.

Synthesis of LiMnPO_4/C composite material for lithium ion batteries by sol-gel method

The LiMnPO4/C composite material was synthesized via a sol-gel method based on the citric acid. The X-ray diffraction （XRD）, scanning electron microscopy （SEM） and electrochemical performance tests were adopted to characterize the properties of LiMnPO4/C. The XRD studies show that the pure olivine phase LiMnPO4 can be obtained at a low temperature of 500 °C. The SEM analyses illustrate that the citric acid used as the chelating reagent and carbon source can restrain the particle size of LiMnPO4/C well. The LiMnPO4/C sample synthesized at 500 °C for 10 h performs the highest initial discharge capacity of 122.6 mA-h/g, retaining 112.4 mA-h/g over 30 cycles at 0.05C rate. The citric acid based sol-gel method is favor to obtain the high electrochemical performance of LiMnPO4/C.

Photocatalytic Activity of Nanosized ZnWO_4 Prepared by the Sol-gel Method

Nanosized ZnWO4 photocatalysts were successfully synthesized via the sol-gel process in a temperature range of 450-800℃. The grain size, crystal size, and crystallinity of ZnWO4 particles increased with the increase of calcina- tion temperature and prolonging calcination time. The photocatalytic activity was measured for the degradation of an aqueous Rhodamine-B（RhB） solution and gaseous formaldehyde（FAD）. With the increase of calcination temperature and time, the activities increased to a maximum and then decreased. ZnWO4 photocatalyst prepared at 550℃ for I0 h showed the highest activity, which is similar to the photocatalytic activity of P25TiO2 for the degradation of gase-ous FAD. High crystallinity, large surface area, and good dispersion are responsible for the high photocatalytic per- formance of the prepared ZnWO4.

Direct Synthesis of Diphenyl Carbonate with Heterogeneous Catalyst and Optimal Synthesis Conditions of the Support Prepared by Sol-gel Method

The support of catalyst for the direct synthesis of diphenyl carbonate （DPC） by heterogeneous catalytic reaction was prepared by the sol-gel method. Compared with activated charcoal, molecular sieve, porous ceramics, hopcalite, the support prepared by the sol-gel method has higher activity. The characterization of the support by X-ray diffraction （XRD） and transmission electron microscope （TEM） show that the mare crystal phase is Co2MnO4 and the average particle diameter is about 40 nm. The optimum conditions for synthesis of the support were determined by orthogonal experiments, which indicate that the proportion of Cu, Mn, and Co is the first important factor influencing the yield and selectivity of DPC. Temperature of calcination is the second one. The optimum conditions are： molar proportion of Cu, Mn, and Co being 1 ： 1 ： 1, temperature of calcination 700℃, drying at 100~C, temperature of water bath 85~C. The yield and selectivity of DPC in the process can reach 38% and 99% in the batch operation, respectively. The copper cobalt manganese mixed oxides chosen as the support contribute more to the high catalytic activity than the sol-gel method.

Preparation and CO conversion activity of ceria nanotubes by carbon nanotubes templating method

Ceria nanotubes with high CO conversion activity by means of carbon nanotubes as removable templates in the simple liquid phase process were fabricated under moderate conditions. The pristine CNTs were first pretreated by refluxing in a 30% nitric acid solution at 140 ℃ for 24 h, then dispersed in an ethanolic Ce（NO3）3.6H2O solution with ultrasonic radiation at room temperature for 1 h. Under vigorous stirring, NaOH solution was added drop by drop into the above ethanolic solution until the pH value was 10. The product was collected and repeatedly washed with ethanol and on drying at 60 ℃, the CeO2/CNT composites were obtained. Then, the as-prepared composites were heated at 450 ℃ in an air atmosphere for 30 min to remove CNTs. The ceria nanotubes were characterized by X-Ray Diffraction （XRD）, Transmission Electron Microscopy （TEM）, and X-Ray Photoelectron Spectrum （XPS）. The results showed that the ceria nanotubes were polycrystalline face-centered cubic phase and were composed of lots of dense cefia nanoparficles. The diameter of cefia nanotubes was about 40-50 nm. Catalytic activity of the product for CO oxidation was carded out at the region of 30-300 ℃ in a U-shaped quartz reactor with feeding about 0.15 g of the catalyst, which was loaded on Al2O3 carder. The inlet gas composition was 1.0% CO and 28% O2 with N2 as balance, and the rate of flow was kept at 40 ml/min. The catalytic products were analyzed by gas chromatography. The as-repared CeO2 nanotubes showed higher CO oxidation activity, which indicated that the morphology of ceria products affected the catalytic performance. The ceria nanotubes supported on Al2O3 demonstrated that conversion temperature for CO oxidation to CO2 was lower than that for bulk catalysts.