Synthesis and characterization of CePO_4 nanowires via microemulsion method at room temperature

Uniform CePO_4 nanowires with diameter of about 25 nm were synthesized by the water-in-oil microemulsion method at room temperature from cerous chloride,sodium orthophosphate,sodium chloride,cyclohexane,Triton X-100 and cetyltrimethyl ammonium bromide(CTAB).The crystal structure and morphology of the nanowires were characterized by XRD and TEM, respectively.The UV-vis absorption was detected by UV-vis spectrophotometer techniques.The results showed that as-prepared nanowires with the hexagonal phase have...     

高压条件下合成硅纳米线

Silicon nanowires (SiNWs) were synthesized with silicon monoxide as the only starting material. At the beginning, a protective gas argon was charged into the reaction chamber and the temperature ramp was controlled at 3 ℃·min^-1. The growth condition for SiNWs was controlled at 480 ℃ under the pressure of 2.8 MPa. The morphology and the structure of the products were characterized by TEM, HRTEM and XRD. The results revealed that SiNWs were diamond structure and their diameters were distributed from 5 to 25 nm. The SiNW was single crystal in the central core and was coated with amorphous silica shell at the exterior surface. Influenced by the quantum effect, Raman spectrum of the SiNWs was found to be redshifted. The oxide-assisted growth mechanism was suggested to explain the growth model of self-assembled SiNWs.     

Polyimide-silver nanocomposite containing phosphine oxide moieties in the main chain: Synthesis and properties

<正>New flame-retardant polyimide-silver nanocomposite containing phosphine oxide moiety in the main chain was synthesized by a convenient ultraviolet irradiation technique.A precursor such as AgNO_3 was used as the source of the silver particles.Polyimide 6 as a source of polymer was synthesized by polycondensation reaction of bis(3-aminophenyl) phenyl phosphine oxide 4 with pyromellitic anhydride 5 in the presence of iso-quinoline as base and in m-cresol solution.The resulting composite film was characterized by FTIR spectroscopy,X-ray diffraction(XRD),transmission electron microscopy(TEM),thermogravimetry(TGA) and differential scanning calorimetry(DSC).The average size of the nanometer Ag particles is about 10 nm.The temperature of 5 and 10%weight loss and also the char yield at 600℃of polyimide-silver nanocomposite 6a were higher than the pure PI 6.     

多面体倍半硅氧烷制备有序介孔氧化硅材料

Octa(tetramethylammonium)-polyhedral oligomeric silsesquioxane(TMA-POSS) with cage-like structure was synthesized, the structure was characterized by NMR, FTIR and Elemental analyses. The mesoporous silica was prepared under alkaline condition using TMA-POSS as the silicon source and hexadecyltrimethylammonium bromide (CTAB) as the template, the structures of these products were characterized by XRD, TEM and nitrogen adsorption and desorption methods. The results indicate that the synthesized silica exhibites a well-ordered hexagonal pore structure with larger specific surface area. With increasing of CTAB molar ratio, the spacing of the crystal plane d100 is increased. The effects of the pH values on the mesoporous structure in the reaction system with different molar ratio of nPOSS / nCTAB were investigated. The synthesis mechanism of mesoporous silica was also discussed.     

Synthesis and Characterization of NASICON Nanoparticles by Sol-gel Method

Na superionic conductor(NASICON) nanoparticles were synthesized by a modified sol-gel method and sintered at a temperature range of 800―1000 ℃.The performance of the samples was characterized by the analysis methods of X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),and transmission electron microscopy(TEM) as well as conductivity measurement.Compared with those sintered at other temperatures,the NASICON material sintered at 900 ℃ had the best crystalline structure and higher conductivi...     

Preparation and characterization of nitrogen-doped titanium dioxides

A type of high visible-light active titanium oxinitride(TiO2-xNx) powder was prepared by a simple proc-ess:the calcination of the hydrated titanium dioxide at the atmosphere of ammonia-argon using a tu-bular electric furnace at high temperatures. The hydrated titanium dioxide was synthesized as the precursor of TiO2-xNx using titanic acid as raw material,which came from sulfate technique of produc-ing titanium white. The effects of temperature and reaction time on the nitrogen content,grain size and crystal structure were studied. The visible-light activity and photocatalysis capability of the powder were also investigated.     

Synthesis,Crystal Structure and DFT Study of 6-Hydroxybentazon

6-Hydroxybentazon, a metabolite of bentazon, was synthesized and characterized herein. The structure of the title compound 11 was verified by single-crystal X-ray crystallography. The optimized crystal structure as well as the HOMO and LUMO levels of the title compound was determined by density functional theory calculations at the B3 LYP/6-311 G(d, p) level.     

Effect of Binder on the Structure and Properties of Silicon Powder-supported TiO_2 Photocatalysis Material

Recoverable TiO2 photocatalysis material supported by silicon powder was prepared with sol-gel method, afterwards the silica gol and sodium silicate were used as molding binder respectively to investigate their effects （including binder type and binder addition quantity） on the crystal structure and catalysis properties of photocatalyst. In this work, the catalysis activity was defined as the degradation rate of methyl orange solution upon ultraviolet lamp irradiation, and the specific areas were determined with nitrogen desorption method. TiO2 crystal form was measured with X-ray powder diffraction and their micro-morphology was observed with SEM. Experimental results indicate that these two binders do not affect the crystal form transformation of TiO2, but silica gol can increase the specific surface area of TiO2 photocatalyst obviously and the addition of sodium silicate can decrease it. In all, silica gol is a better candidate than sodium silicate for higher catalysis property. In conclusion, 6% silica gol is the optimal addition concentration. Under this condition, the ratio of anatase to rutile TiO2 is 64：36, the specific area is 29.67 m^2/g, and as expected, the degradation rate of methyl orange could be as high as 90% after irradiation for 5 days.     

Hexnut[12]arene and its derivatives: Synthesis,host-guest properties,and application as nonporous adaptive crystals

Hexnut[12]arene(HN[12])and its derivatives,a new class of sixfold macrocyclic arenes,were designed and synthesized in reasonable yield by a one-pot reaction at room temperature using dimethoxymethane as a methylene source.HN[12],which bears a large,symmetric,and rigid cavity,was easily functionalized at both the methylene bridges and the hydroquinone units.A water-soluble fluorescent HN[12]was synthesized and used as a host to encapsulate benzyl viologen dichloride in water with a high binding affinity of(3.4±0.2)×10⁶M^-1.The nonporous adaptive crystal(NAC)of HN[12]was found to capture not only inorganic molecules(iodine)but also trace amounts of large organic molecules(basic fuchsine)from water,which greatly expands the scope of NACs for adsorption.     

Modification of Montmorillonite through Intercalative Polymerization

Montmorillonite(MMT) was modified through intercalative polymerization of phenol and formaldehyde catalyzed by oxalic acid.The modified montmorillonite was delaminated at large,as demonstrated by XRD and TEM studies,It can disperse easily in epoxy resion to from exfoliated nanocomposites.The nanoscale silicate platelets dispersed in water can be metallized by silver deposition.     

Growth and Properties of Mid-infrared Single Crystal LiInS2

A Bridgman growth furnace was modified by adding adiabatic material between two furnace tubes. The appropriate temperature gradient of 10～30 ℃/cm at the growth interface was obtained by adjusting the distance between the two sections and controlling their temperature. The infrared nonlinear optical (NLO) crystal LiInS2 was successfully grown by the accelerated crucible rotation technique (ACRT). The crystal was characterized by using XRD and transmission microscopy. It is found that the UV-VIS-NIR and Mid-IR transmittances are about 40%.     

A novel way to synthesize Pb nanotapes in liquid ammonia

Lead nanotapes were synthesized in liquid ammonia solvent in the presence of sodium metal at low temperature.The process was template free.Transmission electron microscopy(TEM) observations and X-ray diffraction(XRD) characterizations revealed that the as-prepared Pb nanotapes have average diameters in the range of 40-50 nm.and lengths up to several hundred nanometers, and exhibit cubic crystal structures.     

Electrochemical properties of niobium and phosphate doped spherical Li-rich spinel LiMn2O4 synthesized by ion implantation method

Spherical Li-rich lithium manganese oxide(LMO) spinel material was synthesized by an ion implanted method assisted by polyalcohol doped with Niobium and Phosphate simultaneously.The material was characterized by scanning electron microscopy,X-ray diffraction and BET specific surface area analysis.The electrochemical performances were investigated with galvanostatic techniques and cyclic voltammetry.The synthesis process was investigated with TG/DSC.The results show that the lithium ion can be immersed into the pore of manganese dioxide at a low temperature with the ion implanted method.The prepared materials have a higher discharge capacity and better crystallization than those prepared by solid phase method.The doped Nb can improve the capacity of the Li-rich LMO spinel and reinforce the crystal growth along(111) and(400) planes.The crystal grains show circular and smooth morphology,which makes the specific surface area greatly decreased.Phosphate-doped LMO spinel exhibits good high-rate capacity and structure stability.The prepared Li_(1.09)Mn_(1.87)Nb_(0.031)O_(3.99)(PO_4)_(0.021)delivers a discharge capacity of 119mAhg~(-1) at 0.2C(1C=148mAg~(-1)) and 112.8 mAhg~(-1) at 10 C,the discharge capacity retention reaches 98% at 1 ℃ after 50 cycles at 25 ℃ and 94% at 55 ℃.     

XRD Analysis on the Fluorescence Material of Sm Doped Si-Ca-Mg System

Fluorescence material of Sm doped Si-Ca-Mg system was synthesized by using the method of solid phase reaction at high temperature. The phase composition and crystal structure of this material were analyzed with XRD method for its composition and the existence form of Sm atom. We aimed to exactly determine the phase composition of this fluorescence material and the doping position and environment of rare-earth Sm atom in the system because these factors have significant effects on the properties. The analytical results show that the Sm atoms dope in Ca2O26Si6Sm8 lattice in the form of atomic site-occupation in three different space positions with different occupancy rates. Therefore, based on the XRD analytical results, the fluorescence material of Sm doped Si-Ca-Mg system with high performance can be synthesized.     

Formation of Na1＋xV3O8 Nanoribbon Thin Film from V2O5 Xerogel on Sodium Silicate Glass Substrate

Na1 xV3O8 nanoribbon thin film was successfully fabricated by annealing the V2O5 xerogel film on sodium silicate glass substrate at 450 ℃.It has been identified that the amount of sodium ions diffused into the V2O5 xerogel film increases with the high temperature of annealing treatment.The sodium glass substrate serves as a limited sodium source to induce the transformation from V2O5 to Na1 xV3O8.     

A new oxidovanadium(Ⅳ) Schiff base complex containing asymmetric tetradentate ONN0O0Schiff base ligand:Synthesis,characterization,crystal structure determination,thermal study and catalytic activity

After synthesis of an asymmetric tetradentate ONN0O0 Schiff base ligand(H2L) followed by reaction of the synthesized H2 L with an equimolar mixture of methanolic solutions of the VO(acac)2, a new oxidovanadium(IV) Schiff base complex(VOL) was synthesized. The Schiff base ligand and its complex were characterized by FT-IR and UV–vis spectra and C, H, N analysis. The crystal structure of VOL was also determined by single crystal X-ray analysis. The VOL complex crystallizes in monoclinic space group Cc. The Schiff base ligand acts as a tetradentate ligand through its two iminic nitrogens and two phenolic and acetylacetonate oxygens. Thermogravimetric analysis of the VOL showed that it decomposes in two steps and converts to mixed vanadium oxides at 477 8C. In addition, thermal decomposition of the VOL complex in air at 660 8C leads to formation of V2O5 nanoparticles with the average size estimated from XRD 49 nm. The catalytic activity of the VOL complex was investigated in the epoxidation reaction and different reaction parameters were optimized. The results showed that the cyclic alkenes were efficiently converted to the corresponding epoxides, whereas the VOL did not appreciably convert the linear alkenes.     

Synthesis and polarized photoluminescence of novel phosphorescent cyclometalated platinum dimer

A novel phosphorescent cyclometalated platinum dimer with bis-[2-(p-dodecyloxyphenyl) pyridyll-hexane-1,6-diol as ligand and 1,3-(1-n-hexyl,3-n-heptadecyl)diketone as ancillary ligand was synthesized.The chemical structure and liquid crystal property of the dimer were characterized by ~1H NMR,ESl-MS,polarizing optical microscopy(POM) and differential scanning calorimetry (DSC).The aligned film of title compound on the rubbed polyimide film is intensely emissive at room temperature with emission maximum at 516nm.The luminescence dichroic ratio((?) ) at 516 nm is 3.1.     

Synthesis,structure and catalytic activity of complexes [Ln(EDBP)_2(DME)Na(DME)_3](Ln=Er,Yb,Sm) for ring-opening polymerization of ε-caprolactone

Discrete ion-pair complexes [Ln(EDBP)2(DME)Na(DME)3] [Ln=Er (1), Yb (2), Sm (3)] have been synthesized by the reaction between sodium salt of 2,2'-ethylidene-bis(4,6-di-tert-butylphenol)(EDBPH2) and Ln(BH4)3·3THF (Ln=Er, Yb, Sm) followed by centrifugation and recrystalization. The complexes were characterized by elemental analysis and FT-IR, and the bonding model of these compounds was confirmed by X-ray single crystal diffraction for complex 1. It was found that four O atoms in two biphenol ligands as well...     

Synthesis of Strontium Carbonate by the Induction of Microbiology

Spherical strontium carbonate was synthesized by the induction of microbial bacillus pasteurii at ambient temperature with strontium chloride and urea as the raw materials. The phase composition, particle size and morphology of the product were studied by XRD and SEM. The results indicated that the strontium carbonate synthesized by the induction of microbial bacillus pasteurii was of good dispersion and uniform particle size. The spherical strontium carbonate particles obtained by adding different control agents were constructed by numerous flakes or olive-shaped nano-particles. The products were orthorhombic according to their XRD patterns.     

液相球化法合成新型正极材料磷酸钒锂

A novel cathode material lithium vanadium phosphate with the microstructure of submicro-particles aggregate was synthesized by liquid-phase sphericizing granulation. XRD pattern showed that the crystal structure of Li3V2(PO4)3 was monoclinic and belonged to P21/n space group. SEM revealed that the diameters of the particle and aggregated particle were in submicron range and about 10 滋m, respectively, with a narrowdistribution. The electrochemical testing showed that the obtained Li3V2(PO4)3 had the maximum discharge capacity of 126.67 mAh·g-1 and initial coulombic efficiency of 95.6%in the range of 3.0-4.3 V (vs Li/Li+), and 170.47mAh·g-1 and 97.5%in the range of 3.0-4.9 V (vs Li/Li+) at a density of 55.6 mA·g-1, respectively. Moreover, the material had a better cycle stability.