Syntheses and evaluations of CdS with various morphologies for photocatalytically reducing CO<Subscript>2</Subscript>

A series of CdS with various shapes of microsphere, flower-like and leaf-like were templatefreely synthesized by a hydrothermal method. Powder X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM) and UV-vis absorption spectroscopy (UV-vis) were applied to characterize the morphology, optical and other physical properties of the as-prepared CdS. An optical spectrum analyzer was used to measure the wavelength of the illuminant on the slurry in the activity evaluations of photocatalytic reduction of CO₂ over CdS. Both sources of cadmium and sulfur had great impact on the CdS morphology as can be seen in the SEM images. By means of a series of activity evaluations, the microspheric CdS made from cadmium nitrate and thioacetamide showed better photocatalytic activity for the reduction of CO₂ to methyl formate (MF) in methanol than the flower-like and leaf-like CdS catalysts.     

Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Fabrication and photocatalytic activity of Ag<Subscript>3</Subscript>PO<Subscript>4</Subscript>-TiO<Subscript>2</Subscript> heterostructural nanotube arrays

To extend the absorption capability of TiO₂ into visible light region and inhibit the recombination of photogenerated electrons and holes, we put forward an effective strategy of the coupling of TiO₂ with a suitable semiconductor that possesses a narrow band gap. Meanwhile, Ag₃PO₄-TiO₂ heterostructural nanotube arrays were prepared by the two-step anodic oxidation to obtain the TiO₂ nanotube arrays and then by a deposition-precipitation method to load Ag₃PO₄. The samples were characterized by field emission scanning electron microscopy (FESEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD), and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The experimental results showed that Ag₃PO₄ nanoparticles were uniformly dispersed on the highly ordered TiO₂ nanotube arrays, which increased the visible-light absorption of TiO₂ photocatalyst. The photocurrent density and photocatalytic degradation of methyl orange indicated that the performance of Ag₃PO₄-TiO₂ heterostructural nanotube arrays was better than that of the TiO₂ nanotube arrays, which could be attributed to the effective electron-hole separation and the improved utilization of visible light.     

Characterization and photocatalytic activity of KSr<Subscript>2</Subscript>Nb<Subscript>5</Subscript>O<Subscript>15</Subscript> with tungsten bronze structure

Tungsten bronze (TB) type potassium strontium niobate KSr₂Nb₅O₁₅ was prepared by solid-state reaction method, and was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV-vis diffuse spectrum. The photocatalyst shows high photocatalytic activity of photodegrading acid red G. The effects of photocatalyst dosage and initial concentration of acid red G on the photodegradation process were studied. The kinetics of photocatalytic degradation of acid red G by KSr₂Nb₅O₁₅ catalyst follows the first order reaction.     

Facile synthesis of nanocrystalline Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> thin film

A novel and facile synthesis route for the manufacture of transparent and uniform self-assembled nanocrystalline Cr2O3 (nc-Cr2O3) thin films with different morphology was reported, utilizing chromium nitrate as the inorganic source and triblock copolymer F127 as the morphology-directing agent by the evaporation-induced assembly (EIA) method. X-ray powder diffraction (XRD), thermogravimetry-differential scanning calorimetry (TG-DSC), N2-sorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the as-prepared nc-Cr2O3 thin films. The Cr2O3 thin film with different morphology was obtained by changing the relative humidity. The possible formation mechanism of the nc-Cr2O3 thin films with different morphologies was discussed.     

Preparation and enhanced daylight-induced photo-catalytic activity of transparent C-Doped TiO<Subscript>2</Subscript> thin films

The transparent C-doped TiO₂ nanostructure films were fabricated on the silicate glass substrates by sol-gel spin-coated method. The as-prepared films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-visible absorption spectra (UV-vis) and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity was evaluated via the photo-catalytic oxidation of methylene blue in aqueous under daylight irradiation at room temperature. The results show that the daylight-induced photocatalytic activities of the as-prepared films are improved by the C-doping. The calcination temperatures significantly affect the morphology, microstructure and photocatalytic activity of the as-prepared samples. At 723 K, the C-doped TiO₂ films exhibit the highest photocatalytic activity due to the synergetic effects of good crystallization, appropriate oxygen vacancies and strong absorption in the near UV and visible-light region.     

Fabrication of BiVO<Subscript>4</Subscript>: Effect of structure and morphology on photocatalytic activity and its methylene blue decomposition mechanism

BiVO₄ photocatalysts were synthesized by a surfactant free hydrothermal method without any further treatments, and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS), Raman spectroscopy, and Brunauer-Emmett-Teller (BET) surface area techniques. The photocatalytic activity was evaluated for the degradation of the methylene blue (MB) under visible light irradiation. Seen from the structural and morphological characterization, it is stated that the obtained samples present monoclinic phase, and the pH value has significant influence on the morphologies. The enhanced photocatalytic performance was associated with its crystallinity, unique morphology, band gap energy, BET specific surface area, surface charge and adsorption capacity. The recycle experiments results show that the BiVO₄ photocatalysts have excellent photo-stability, and we deduced a possible mechanism by examining the effects of the active species involved in the photocatalytic process for MB photocatalytic degradation.     

Biomolecule-assisted solvothermal synthesis and enhanced visible light photocatalytic performance of Bi<Subscript>2</Subscript>S<Subscript>3</Subscript>/BiOCl composites

Novel Bi₂S₃/BiOCl photocatalysts were successfully synthesized via a facile biomolecule-assisted solvothermal method and biomolecule L-cysteine was used as the sulfur source. The structures, morphology, and optical properties of the synthesized samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, transmission electron microscopy (TEM), and UV-vis diffuse reflectance spectroscopy (DRS). The presence of Bi₂S₃ in the Bi₂S₃/BiOCl composites could not only improve the optical properties but also enhance the photocatalytic activities for the degradation of Rhodamine B (RhB) under visible-light irradiation (λ > 420 nm) as compared with single Bi₂S₃ and BiOCl. Especially, the sample displayed the best performance of the photodegradation when the feed molar ratio of BiCl3 and L-cysteine was 2.4:1, which was about 10 times greater than that of pure BiOCl. The enhanced photocatalytic activities could be ascribed to the effective separation of photoinduced electrons and holes and the photosensitization of dye. Moreover, the possible photodegradation mechanism was also proposed, and the results revealed that the active holes (h⁺) and superoxide radicals (?O₂ ^?) were the main reactive species during photocatalytic degradation.     

Hydrothermal synthesis of WO<Subscript>3</Subscript> nanowires in the presence of guanidine sulfate and its photocatalytic activity

WO₃ nanowires were fabricated by a hydrothermal method, which proceeded at 170 °C for 48 h in a solution containing C₂H₁₀N₆H₂SO₄ as a dispersant and Na₂WO₄ as a starting material. The nanowires exhibit a well crystallized one-dimensional structure with 20 nm in diameter and several microns in length. The physicochemical properties of WO₃ were compared using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX) and UV-vis spectroscopy (UV-Vis). The photoactivity of the as-perpared WO₃ nanowires was evaluated through the photodegradation of methylene blue (MB) in aqueous solution. The experimental results demonstrate that addition of C₂H₁₀N₆H₂SO₄ salt in the WO₃ nanowires synthesis process can enhance its photocatalytic activity obviously.     

Electrochemical preparation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> from NaVO<Subscript>3</Subscript> and its reduction mechanism

Vanadium trioxide (V₂O₃) was directly prepared by NaVO₃ electrolysis in NaCl molten salts. Electrolysis products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The existing state and electrochemical behavior of NaVO₃ were also studied. The results indicated that V₂O₃ can be obtained from NaVO₃. VC and C were also formed at high cell voltage, high temperature, and long electrolysis time. During electrolysis, NaVO₃ was dissociated to Na⁺ and VO₃ ^? in NaCl molten salt. NaVO₃ was initially electro- reduced to V₂O₃ on cathode and Na₂O was released simultaneously. Na₂CO₃ was formed due to the reaction between Na₂O and CO₂. The production of C was ascribed to the electro-reduction of CO₃ ^2?. VC was produced due to the reaction between C and V₂O₃.     

Preparation of nanometer Nd<Superscript>3+</Superscript>, Y<Superscript>3+</Superscript> co-doped CaF<Subscript>2</Subscript> powder by coprecipitation-azeotropic distillation technique

The synthesis of Nd³⁺, Y³⁺:CaF₂ nanopowder was conducted by azeotropic distillation method, which effectively dehydrated hydrous CaF₂ and prevented forming hard agglomerates. X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning calorimetries-thermalgravimetry (DSC-TG), Fourier transform infrared spectroscopy (FT-IR) and absorption spectroscopy were performed to characterize the powder properties. The experimental results showed that products obtained by azeotropic distillation were single phased, rather monodispersed, successfully prevented the hard agglomerate formation and effectively removed the residual water inside the as-prepared precipitate than that of the direct drying. The absorption spectra showed a wider and stronger absorption bands around 792 nm, which should be profitable for LD pumping.     

Self-assembled SnO<Subscript>2</Subscript> colloidal particles and their gas sensing performance to H<Subscript>2</Subscript>, C<Subscript>2</Subscript>H<Subscript>5</Subscript>OH and LPG

Using organo-tin Sn(OC4H9)4 as precursor, sodium dodecyl sulfonate (SDS) and SDS-gelatin (SDS-G) complex as template, two tin dioxide colloidal particles were prepared by a self-assembly method. Both SnO2 products were respectively labelled SnO2-B particles with SDS and SnO2-C particles with SDS-G, which are applied in fabricating SnO2 gas sensors corresponding to SnO2-B’ and SnO2-C’ sensors. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermo-gravimetry and different thermal analysis (TG/DTA) were used for characterizations. The experimental results show that SnO2-B colloidal particles are composed of mesoporous piece-like particles, while SnO2-C particles mainly consist of spherical particles. Gas sensing measurements show that SnO2-B’ sensor performs the best sensing response to all target gases, including H2, C2H5OH and liquid petroleum gas (LPG). In particular, the sensing response of SnO2-B’ sensor is achieved at 32 in H2 atmosphere at the concentration of 1000×10-6 M. The gas sensing mechanism was purposely discussed from the electron transfer process and the microstructures of the as-prepared SnO2 products. It is found that serious agglomerations in SnO2-B’ particles facilitate the high gas sensing performance of SnO2-B’ sensor, while mesoporous structures in SnO2-C’ particles decrease the gas sensing response of SnO2-C’ sensor.     

Preparation and characterization of CeO<Subscript>2</Subscript>-TiO<Subscript>2</Subscript>/SnO<Subscript>2</Subscript>:Sb films deposited on glass substrates by R.F. sputtering

CeO2-TiO2 films and CeO2-TiO/SnO2：Sb （6 mol%） double films were deposited on glass substrates by radio-frequency magnetron sputtering （R.F. Sputtering）, using SnO2：Sb（6 mol%） target, and CeO2- TiO2 targets with different molar ratio of CeO2 to TiO2 （CeO2：TiO2-0：1.0; 0.1：0.9; 0.2：0.8; 0.3：0.7; 0.4：0.6; 0.5：0.5; 0.6：0.4; 0.7：0.3; 0.8：0.2; 0.9：0.1; 1.0：0）. The films are characterized by UV-visible transmission and infrared reflection spectra, scanning electron microscopy （SEM）, Raman spectroscopy, X-ray photoelectron spectroscopy （XPS） and X-ray diffraction （XRD）, respectively. The obtained results show that the amorphous phases composed of CeO2-TiO2 play an important role in absorbing UV, there are Ce^3-, Ce^4- and Ti^4- on the surface of the films; the glass substrates coated with CeO2-TiO2 （Ce/Ti=0.5：0.5; 0.6：0.4）/SnO2：Sb（6 mol%） double films show high absorbing UV（〉99）, high visible light transmission （75%） and good infrared reflection （〉70%）. The sheet resistance of the films is 30-50 Ω/□. The glass substrates coated with the double functional films can be used as window glass of buildings, automobile and so on.     

Straight SiO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> nanorod Y junctions

Novel straight silicon oxide [SiO _x (1<x<2)] nanorod Y junctions have been synthesized on Si plate by thermal evaporation of mixed powders of silica and carbon nanofibers at 1300°C and condensation on a Si substrate without assistance of any catalyst. The synthesized samples were characterized by means of scanning electron microscopy, transmission electron microscopy, high resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy. The results suggested that the straight nanorod Y junctions are amorphous and consist only of elements Si and O, and these rods with diameters about 50–200 nm have a neat smooth surface. The growth of such silicon oxide nanorods may be a result of the second nucleation on the surface of rods causing a change in the growth direction of silicon oxide nanorods developed. Supported by the Academic Human Resources Development in Institutions of Higher Learning under the Jurisdiction of Beijing, and the Program of Science & Technology Activity for Chinese Homecoming Fellow Abroad and Research Program of Beijing Key Laboratory for Sensor (Grant No. KM200810772009)     

Photocatalytic degradation of rhodamine B dye with MWCNT/TiO<Subscript>2</Subscript>/C<Subscript>60</Subscript> composites by a hydrothermal method

Multi-walled carbon nanotube (MWCNT)/TiO2/C60 composite catalysts were prepared by hydrothermal method. TiO2 was deposited on the MWCNT surface. Their photocatalytic activities for degradation of Rhodamine B dye were studied. X-ray diffraction, field emission transmission electron microscopy, ultraviolet-visible light absorption spectrum and photoluminescence spectrum were carried out to characterize the composite catalysts. The results indicated that MWCNTs and C60 could greatly enhance the photocatalytic activity of TiO2.     

Synthesis,characterization and thermal stability of CeO<Subscript>2</Subscript> stabilized ZrO<Subscript>2</Subscript> ultra fine nanoparticles via a sol-gel route

CeO₂ stabilized ZrO₂ ultra fine nanoparticles were successfully synthesized via a simple and effective sol-gel synthetic approach by using zirconylchloride octahydrate, cerium nitrate hexahydrate, and citric acid as starting materials. A series of techniques, including X-ray diffraction (XRD), thermogravimetry (TG), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and N₂-sorption analysis, were used to characterize the structure and morphology of the as-prepared samples. XRD studies indicate that the as-synthesized sample is of well crystallized tetragonal phase of CeO₂ stabilized ZrO₂ with high purity. TEM images show that the as-synthesized sample is composed of a large number of fine dispersive nanoparticles with an average size about 10 nm. The as-synthesized tetragonal CeO₂ stabilized ZrO₂ sample was heated at different temperatures in order to evaluate its thermal stability. The exprimental results reveal that the as-synthesized tetragonal CeO₂ stabilized ZrO₂ sample exhibits excellent stability without the occurrence of phase transformation.     

Photocatalytic activity of lanthanum and sulfur co-doped TiO<Subscript>2</Subscript> photocatalyst under visible light

A novel lanthanum and sulfur co-doped TiO2 photocatalyst was synthesized by precipitation- dipping method, and characterized by X-ray diffraction（XRD）, transmission electron microscopy（TEM） and UV-Vis diffuse reflectance spectroscopy. Compared with the S-doped TiO, La-doped TiO2 and the standard Degussa P25 photocatalysts, the lanthanum and sulfur co-doped TiO2 photocatalyst （the molar percentage of La is 3.0%） calcined at 450 ℃ for 2 h showed the strongest absorption for visible light and highest activities for degradation of reactive blue 19 dye in aqueous solution under visible light（λ〉400 nm） irradiation. It was also discovered that the co-doping of lanthanum and sulfur hindered the aggregation and growth of TiO2 particles, and the doping of lanthanum reduced slightly the phase transition temperature ofTiO2 from anatase to rutile.     

Solvothermal synthesis and photocatalytic performance of Bi<Subscript>2</Subscript>S<Subscript>3</Subscript> hierarchical nanostructure

The synthesis of Bi₂S₃ hierarchical nanostructure was reported by a solvothermal reaction using ethylene disulfhydrate as the sulfur source and chelating reagent. The as-synthesized samples were characterized by X-ray diffraction (XRD), Raman, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and photoluminescence (PL). The XRD, Raman, and XPS data confirmed that the as-synthesized sample belongs to orthorhombic phase Bi₂S₃. The SEM observations displayed that Bi₂S₃ hierarchical nanostructure assembled from nanorods. A 410 nm ultraviolet photoluminescence (PL) emission of as-synthesized Bi₂S₃ was observed when the sample was excited with wavelength of 320-330 nm. The Bi₂S₃ hierarchical nanostructure also shows a significant enhancement of photocatalytic capability toward degrading methyl orange (MO) under UV light, the photodegradation of MO reaches 95% within 180 min.     

Influence of Aluminum Ions Implantation on Corrosion Behavior of Zircaloy-2 Alloy in 1M H2SO4

The specimens were implanted with aluminum ions with fluence ranging from 1× 10^16 to 1× 10^17 ions/cm^2 to study the effect of aluminum ion implantation on the aqueous corrosion behavior of zircaloy-2 by metal vapor vacuum arc source （MEVVA） at an extraction voltage of 40 kV. The valence states and depth distributions of elements in the surface layer of the samples were analyzed by X-ray photoelectron spectroscopy （XPS） and Auger electron spectroscopy （AES）, respectively. Transmission electron microscopy （TEM） was used to examine the microstructure of the aluminum-implanted samples. Glancing angle X-ray diffraction （GAXRD） was employed to examine the phase transformation due to the aluminum ion implantation. The potentiodynamic polarization technique was employed to evaluate the aqueous corrosion resistance of implanted zircaloy-2 in a 1 M H2SO4 solution. It is found that a significant improvement was achieved in the aqueous corrosion resistance of zircaloy-2 implanted with aluminum ions. Finally, the mechanism of the corrosion behavior of aluminum- implanted zircaloy-2 was discussed.     

Preparation and optical properties of Er<Superscript>3+</Superscript>: Na<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> transparent glass-ceramics

Na₂O-Al₂O₃-SiO₂ glass-ceramics doped with Er³⁺ ions were synthesized by the conventional melt quenching technique at a low melting temperature. The samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-vis-NIR scanning spectrophotometry, and fluorescence spectrometry. The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 °C for 2 h. Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu³⁺ are studied in detail.