Hydrothermal synthesis, structure and photocatalytic property of nano-TiO_2-MnO_2

TiCI4 and MnSO4.H2O as raw materials are hydrolyzed stiochiometrically, following the intermediate of oxide hydrating reacts at 150℃, 0.5 MPa in high-pressure reactor, after filtering, washing and drying, nanometric TiO2-MnO2 (Ti1-xMnxO2) is prepared. The effects of the reaction temperature and time on nanometric TiO2-MnO2 are also discussed. XRD shows that the product is TiO2-MnO2 with amorphous phase. After being sintered at above 780℃, it transfers into Ti1-xMnxO2 with a rutile structure. TEM shows that TiO2-MnO2 is the spherical particle. And the average diameter of the particles is 20 nm. The optical absorbance was determined by UV-265 spec-trophotometer after dispersing the sample in the mixture of water and glycerol with the ratio of 1 : 1 equably. It is found that the nano-material possesses the advantages of both nano-TiO2 and nano-MnO2, and it has strong absorption in the UV and visible region. Photodegradation of dyes in an aqueous solution is investigated using nanometricTiO2-MnO2 as a pho     

Electrodeposition of SnO2 nanocrystalline thin film using butyl-rhodamine B as a structure-directing agent

<正>Porous SnO_2 nanocrystalline thin films were successfully electrodeposited from an oxygen-saturated acid aqueous solution of SnCl_2 containing different concentrations of butyl-rhodamine B(BRhB) at 70℃.BRhB with substitute of amidocyanogen can be dissolved in the acid deposition solution,where HCl was added to suppress hydrolysis of SnCl_2.So it was used as a structure-directing agent to promote the crystal growth of SnO_2.The formed porous morphology and tetragonal rutile crystalline structure of the electrodeposited thin films were controlled by the addition of BRhB with different amounts.     

PREPARATION AND ADSORBABILITY OF DEXTRAN MICROSPHERES WITH UNIFORM DIAMETER

The method of preparing uniform dextran microspheres with a narrow diameter distribution was introduced and the adsorbability of these microspheres was evaluated. The microspheres were prepared in W/O microemulsion using 0.5% dextran solution as the aqueous phase and n-hexane as the oil phase. Characteristics of the prepared dextran microspheres were examined with laser light blocking technique, optical microscope and ultraviolet spectrometer. The results show that the prepared dextran microspheres have uniform morphology and narrow diameter distribution, nearly 92% of them having a diameter of 56.6μm. In vitro evaluation of adsorbability, wet dextran microspheres have good adsorption of 98.32mg/g of model drug methylene blue in 20.86mg/L methylene blue solution at 25℃, The adsorption of dried dextran microspheres under the same condition is 132.15mg/g, which is even higher. And the adsorbability of dextran microspheres has significant relationship with the concentration of methylene blue and temperature. The adsorbability is better at lower temperature and higher concentration of methylene blue.     

热化学法合成金属铋纳米棒(英)

Bismuth with rod-like shape was prepared by refluxing an aqueous dispersion of spherical colloids. The spherical colloids of bismuth were generated by reducing bismuth nitrate with ascorbic acid in the presence of cethyltrimethylammonium bromide (CTAB) and ethylene diamine tetraacetic (EDTA). The mixed solution was refluxed at temperature of 60～70 ℃ for about 5 hours to get bismuth nanorods with a diameter about 10～30 nm. Experimental results showed that this method could facilitate the growth of these rod-like nanomaterials. Various techniques such as transmission electron microscopy (TEM), selected-area-electron diffraction (SAED), and x-ray diffraction (XRD) have been used to characterize the nanorods.     

强烈阳极氧化法快速制备多孔氧化铝模板

In the electrolyte of oxalic acid/alcohol/aqueous solution, highly-ordered porous anodic aluminum oxide(AAO) template was fabricated by hard anodization. The surface morphology and the structure of AAO template were characterized by Field-Emission Scanning Electron Microscope(FE-SEM) and XRD, respectively. The effects of different factors including alcohol type, ratio of alcohol to water, and oxalic acid concentration on the ordering degree and pore diameter of AAO template were investigated. Under the glycol to water ratio of 1∶1(by volume) with an oxalic acid concentration of 0.5 mol·L^-1, and voltage at 160 V, the obtained AAO template was hexangular arrangement with pore diameter of 80 nm and pores spacing of 120 nm, the growth rate was 51.9 μm·h^-1.     

循环伏安法制备Ag纳米线阵列

In this paper, highly ordered anodic aluminum oxide (AAO) template with hexagonal close-packed arrays was successfully fabricated through a two-step anodization process. Ag nanowire arrays with high aspect ratio were prepared using cyclic voltammetry within the confined nanochannels of AAO template. In addition, standing Ag nanowire arrays free-support of templates were also fabricated successfully by cyclic voltammetry method. The micrographs and crystal structures of Ag nanowires were studied by field emission scanning electron microscope (FESEM) and X-ray diffraction (XRD). FESEM observation showed that the Ag nanowire arrays with high aspect ratio lie orderly on the surface of the substrate. The diameter of the Ag nanowire is about 60 nm and the length up to 30 μm or more. While the controlled nanowire arrays exhibit highly ordered structure in large area and the standing Ag nanowire in the array has the length of 1 μm and good orientation. XRD results illustrated that the Ag nanowires in the arrays deposited by cyclic voltammetry method have a face centered cubic structure and are preferentially oriented in the (220) direction.     

Immobilization of Penicillin G Acylase on Calcined Layered Double Hydroxides

A hydrotalcite-like Mg2 /Al3 layered double hydroxide (LDH) material was prepared by means of amodified coprecipitation method involving a rapid mixing step followed by a separate aging process. LDH calcined at 500℃ , denoted as CLDH, was characterized by XRD, IR and BET surface area measurements.CLDH has a poor crystalline MgO-like structure with a high surface area and porosity. CLDH was used as asupport for the immobilization of penicillin G acylase(PGA). The effect of varying the immobilization conditions, such as pH, contact time and the ratio of enzyme to support, on the activity of the immobilized enzymein the hydrolysis of penicillin G has been studied. It was found that the activity of the immobilized enzyme decreased slightly with decreasing pH and reached a maximum after a contact time of 24 h. The activity of theimmobilized enzyme increased with increasing the ratio of enzyme to support. It was found that the adsorption of PGA inhibited the expected reaction of CLDH with an aqueous medium to regenerate a LDH phase. Itsoriginal activity(36%) after 15 cycles of reuse of the immobilized enzyme was retained, but no further loss in the activity was observed.     

Formation of Ultrafine Apatite Fibers by Sol-gel/Electrospinning

Ultrafine apatite fibers were prepared by electrospinning of sol-gel precursor/poly（ vinyl pyrrolidone） （PVP） solutions followed by subsequent calcination. The as-electrospun and calcinated fibers were observed under a scanning electron microscope and an optical polarizing microscope. Results show that the morphology and the diameter of as-electrospun fibers strongly depend on the viscosity and the surface tension of sol-gel precursor/PVP solutions. After calcination, the smooth as-electrospun fibers shrink and the fiber diameter decreases because of the removal of the polymer. The chemical evolution upon the transformation of the precursor from a gel to the final apatite fibers was investigated by thermogravimetric-differenfial thermal analysis, X-ray diffraction, and Fourier transform infrared spectroscopy. It is thus suggested that the crystalline structure of the calcined fibers is largely influenced by the calcination temperature. After being calcined at 600 ℃, the apatite fibers with a diameter of about 280 nm containing β-tricalcium phosphate were obtained.     

Electrospun Nanofibers Containing p-Nitrophenol Imprinted Nanoparticles for the Hydrolysis of Paraoxon

p-Nitrophenol imprinted nanoparticles with a size range of 150-300 nm in diameter were prepared through miniemulsion polymerization. The imprinted polymer exhibited higher adsorption capacity for p-nitrophenol than the nonimprinted polymer. The hydrolysis of paraoxon in aqueous phase can be accelerated in the presence of the p-nitrophenol imprinted nanoparticles. The hydrolysis rate of paraoxon incorporated with the imprinted nanoparticles was 2.83×10-7 mol/（L·min）, which was about 3.7 times higher compared to the non-imprinted nanoparticles, 12.7 times higher to the spontaneous hydrolysis. The nanoparticles have been mixed with polyacrylonitrile solution and electrospun into nanofibers, which can also be used to accelerate the hydrolysis of paraoxon and conveniently separated from liquid phase for further processing.     

电化学法制备硅纳米线

Silicon nanowires were synthesized from nanometer silicon dioxide powder under potentiostatic electrolysis at -1.20 V (vs Pt reference) for 4 h in molten CaCl₂ at 900 ℃. The morphology, structure and chemical composition of the samples prepared by electroreduction method were characterized by field-emission scanning electron microscopy(FE-SEM), High-resolution transmission electron microscopy(HRTEM) coupled with electron energy dispersive spectroscopy(EDS), laser Raman and X-ray diffraction(XRD). The results revealed that silicon nanowires were crystalline with a diamond cubic structure, the diameter was distributed from 50 nm to 80 nm and the length was generally several micrometers. The formed nanowires basically consisted of silicon monocrystalline and amorphous oxide sheath.     

Microwave-assisted synthesis of high aspect ratio ruthenium nanorods

<正>Poly(N-vinyl-2-pyrrolidone)(PVP)-stabilized ruthenium nanorods with high aspect ratio by refluxing ruthenium(Ⅲ) chloride in n-propanol have been successfully prepared by means of a facile and rapid microwave heating for the first time.The structure and morphology of the obtained products were characterized by transmission electron microscopy(TEM),select area electron diffraction(SAED),ultraviolet-visible spectrophotometry(UV-vis),X-ray photoelectron spectroscopy(XPS) and Fourier transform spectroscopy(FT-IR).XPS analysis reveals that the nanorods were in the metallic state.TEM images showed that ruthenium nanorods had an obvious one-dimensional structure with the aspect ratio ranged from 5 to 40 nm and length up to 600 nm.SAED patterns indicated that the nanorods were single-crystalline with a hexagonal structure.     

Synergistic effect of TiO_2 hierarchical submicrospheres for high performance dye-sensitized solar cells

The performance of dye-sensitized solar cells(DSCs) could be improved by using rationally designed mesoporous film structure for electron collection, dye adsorption and light scattering. The development of a novel double layer film prepared by TiO_2 hierarchical submicrospheres and nanoparticles was reported in this article. The submicrospheres were composed of rutile nanorods of 10 nm diameter and the length of 150–250 nm, which facilitated fast electron transport, charge collection and light scattering. Using a double layer structure consisting of the 10 wt% film as a dye loading layer and the 50 wt% film as the light scattering layer, C101 sensitizer and liquid electrolyte, DSC yielded power conversion efficiency of 9.68% under 1 sun illumination.     

Synthesis and Characterization of Titanium-doped Ordered Mesoporous Alumina

Titanium-doped ordered mesoporous alumina with specific structural properties has been prepared by the evaporation induced self-assembly sol-gel method. The results show that the doped titanium helps to stabilize the ordered mesoporous alumina material without influencing the ordered mesoporosity. The textural properties of the obtained sample are related to the amount of doped titanium. When the molar ratio of aluminum to titanium(n(Al)/n(Ti)) is controlled as 10.2, the titanium-doped ordered mesoporous alumina exhibits high surface area(up to 218 m2 g-1), large pore volume(0.42 cm3 g-1) and narrow pore diameter(6.1 nm) after treating at 900 ℃, showing high thermal stability. Moreover, the obtained sample calcined at 900 ℃ still maintains ordered mesoporous structure and exhibits high thermal stability.     

Synthesis and Gas-sensing Performance of Nanosized SnO2

Nanosized tin dioxide particles were prepared by sol-gel dialytic processes with tin(Ⅳ) chloride and alcohol as start materials. The nanoparticles of tin dioxide were charactered by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and BET. The results show that the average diameter of tin dioxide particles dried at 353 K was about 2nm. Even if the tin dioxide particles were calcined at 873 K, the average diameter of particles was less than 10 nm. The removal of Cl^- was solved by using this kind of method. The mechanism of the formation of tin dioxide nanosized particles was proposed and analyzed in this paper. We also measured the sensitivity of the sensor based on the tin oxide powder calcined at 673K to NH3, alcohol, acetone, hexane and CO. The gas-sensing performance results indicate that this sensor has a higher sensitivity to alcohol and acetone, and selectivity for NH3, hexane and CO at an operating temperature of 343 K.     

SnO2纳米粒子的制备与表征

The SnO2 nano-particles with rutile structure were prepared by a Water/Oil (W/O) microemulsion system, composed of Triton X-100 1-hexanol/Cyclohexane/Water. The particles were also compared with that synthesized by citric acid method. The powders were characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and infrared spectroscopy (IR). The result showed that the SnO2 particles prepared by microemulsion had fine shape and narrow range of particle size distribution. The crystallite size calcined at 600℃ was 11.49 nm,while the crystallite size prepared by citric acid method was about 17.4 nm.     

原子力显微镜研究囊泡在云母表面形成的结构

The vesicle structures of egg yolks phosphatidylcholine/didodecyldimethylammonium bromide （1 ： 1, mass ratio） deposited on mica were studied by atomic force microscopy （AFM） both in aqueous phase and air. In aqueous phase both bilayer and domelike vesicles with a mean diameter of 45 nm were observed, whereas in air the structure was more complicated depending on the initial concentration of vesicles. Vesicles with the original size could only be visualized at very low concentration with a mean diameter of 55 nm, which is a little larger than the result obtained in aqueous phase. At higher concentrations, fused large aggregates and multiple bilayer with a thickness ca. 4 nm of each bilayer were dominated. A plausible adsorption mechanism was proposed based on the experimental results.     

纤维状硬脂酸银的合成及其表征

A new type of fibrous silver stearate (AgSt) was synthesized using double-jet method with KOH as pH regulator in water solution system. The structure, morphology and phase transiton behavior of the fibrous AgSt were characterized by FTIR, SEM, XRD and TG-DTA. SEM images showed that the diameter of the fibrous AgSt was about 150 nm and the length was 5～8 μm. XRD data indicated its layered structure and TG-DTA showed its high themal stability. In addition, the possible growth mechanism of the fibrous AgSt is also discussed.     

N 掺杂TiO2光催化剂的制备及其可见光活性研究

A visible-light-active photocatalyst was prepared by calcination of the hydrolysis product of tetrabutyl titanate with ammonia as precipitant. The photocatalyst was characterized by X-ray diffraction (XRD), UV-Vis diffuse reflection spectra (DRS), thermal gravimetric-differential thermal analysis (TG-DTA), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM). The color of the photocatalyst was yellow and could absorb light wavelength under 550 nm as measured by DRS. The catalyst calcined at higher temperature will give lower absorbance for visible light. Structures of the sample were characterized mainly to be anatase by XRD except for the sample calcined at 700 ℃ which gave mixtures of anatase and rutile. TG-DTA results showed that temperature for anatase formation was 415 ℃. XPS results showed that doped-nitrogen was presented in the sample, they are important to show visible-light absorbency. The photocatalytic activities were evaluated using methyl orange and phenol as model pollutants, the results showed that over 90% of phenol could be degraded under visible light using N/TiO₂ as the catalyst after 4 hours reaction. Almost the same activity was found for the TiO₂ photocatalyst calcined at different temperature under sunlight but activities were different when the treatment was under UV light.     

Synthesis of Poly（N-vinylpyrrolidone） Nanofibers Containing Gold Nanoparticles via Electrospinning Technique

Poly(N-vinylpyrrolidone)(PVP)nanofibers containing gold nanoparticles were prepared by electrospinning method.This simple route was used to prepare composites on a large scale,and the syntheses are simple.The optical property of gold nanoparticles in PVP aqueous solution was investigated by UV-Visible absorption spectra.The morphology of the fibers and the distribution of particles were characterized by transmission electron microscopy.The structure of the composite was characterized by Fourier transform infrared spectroscopy.     

由乙氧基铅配合物制备纳米PbO

Lead complex was directly synthesized by electrochemical dissolution of lead in a cell without separating the cathode and anode. The product was characterized by FTIR, Raman spectra and ¹H NMR. The xerogel was prepared by a direct sol-gel of the electrolyte solution and then dryness of it. The xerogel was heated at 450 ℃ for 2 h to obtain the nano-PbO powder. FTIR, XRD, and TEM were used to investigate the structure of nano-PbO. The results show that the lead complex is Pb(OEt)₂(acac)₂, which contains acac- group and could prevent the precursor from hydrolysis and sintering during the calcinations process. The nano-PbO of 20～30 nm was thus obtained in a high purity by drying at 450 ℃.