Alkali induced morphology and property improvements of TiO<Subscript>2</Subscript> by hydrothermal treatment

Alkali induced morphology and property improvements of TiO2 by hydrothermal reaction were investigated. The products were characterized by SEM, TEM, XRD, TG, EDX, FT-IR and DRS. The results indicate that, with the phase transformation from anatase to rutile, the morphologies changed from high aggregated particles to nanofibers with the diameter of about 100 nm and the length up to several tens of micrometers, meanwhile the process is controllable by manipulating the nature of the alkali, alkalinity and hydrothermal temperature. DRS analysis shows the property improvement of the nanofibers in the UV-Vis light absorption compared with the raw materials, implying the products have potential application in photocatalysis.     

Manifestations in corrosion prophase of ultra-high strength steel 30CrMnSiNi2A in sodium chloride solutions

The corrosion behaviors of ultra-high strength steel 30CrMnSiNi2A in sodium chloride solution were studied by weight loss and electrochemical methods. The morphology of corrosion products was observed using scanning electron microscopy(SEM) and the composition was analyzed using an energy dispersive spectroscopy(EDS) and X-Ray diffraction(XRD). The experimental results showed that the corrosion came from pitting corrosion and the rust layer was composed of outer rust layer γ-FeOOH and inner rust layer Fe2O3 with a little β-FeOOH. The correlation between corrosion rate and test time accorded with exponential rule. The corrosion current measured by polarization methods was higher than that calculated by weight loss method after a long-time immersion, the main reason was that β-FeOOH and γ-Fe2O3 transformed by γ-FeOOH led to overestimating corrosion rate. The processes of corrosion prophase were obtained from XRD and EIS results. The corrosion product, Fe(OH)2 formed at the initial stage stayed at a non-steady state and then consequently transferred to γ-FeOOH, γ-Fe2O3 or β-FeOOH.     

Morphology tuning of mono-disperse silver nanoparticles by reaction temperature adjustment

Mono-disperse silver nanoparticles with tunable morphologies have been fabricated by reducing AgNO3 in the presence of N-dimethylformamide (DMF) and larger molecular weight poly(vinylpyrrolidone)(PVP). By adjusting the reaction temperature, the conversion of the morphology can be easily and effectively controlled. The crystal structures and growth mechanism of mono-disperse silver nanoparticles were studied by using TEM, HR-TEM, FFT, XRD and UV-Vis spectra data. The results show that the morphologies of nanoparticles with spherical shape can be adjusted to a truncated triangle/hexagon along with the change of reaction temperature from 80 to 120 ℃. It is found that the shape transformation from sphere to truncated triangle is caused by the difference in surface energy and the selective adsorption of PVP on silver atom.     

Effect of heat-treatment on crystalline phase and UV absorption of 60CeO2-40TiO2 thin films by magnetron sputtering

60CeO2-40TiO2 thin films were deposited on soda-lime silicate glass substrates by R.F. magnetron sputtering. The effects of heat-treatment on the UV-absorption of the thin films were studied on the 60CeO2-40TiO2 thin film with the largest UV cut-off wavelength. The sample films with CeO2:TiO2=60:40 were heated at 773 K, 873 K, 973 K for 30 min. These films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy and spectrometer (XPS). XRD analysis proves that the addition of TiO2 to CeO2 changed the crystalline state of CeO2. But the UV absorption effect of CeO2-TiO2 films with CeO2 crystallite phase is inferior to that of the amorphous phase CeO2-TiO2 films. XPS analysis also indicates that the amorphous phase CeO2-TiO2 films have the most Ce3+ content in these films. Amorphous phase and crystalline phase of the CeO2-TiO2 films have different effects on UV absorption of the thin films.     

Controlled Synthesis and Application of α-Al_2O_3 for Lu_3Al_5O_(12): Ce~(3+) Green Spherical Phosphors

Al_2O_3 powders with different morphologies,namely fibrous,sheet-like,and spherical,were prepared by the hydrothermal-thermolysis method.Subsequently,polycrystalline,transparent cerium doped lutetium aluminum garnet(Lu_3Al_5O_(12):Ce~(3+))green phosphors were synthesized by high temperature solidstate method using commercial lutetium(III)oxide,cerium(III)oxide,and as-prepared Al_2O_3 powders with different morphologies.The phases,morphologies,and photoluminescent properties of the prepared phosphors were investigated by X-ray diffraction(XRD),scanning electron microscopy(SEM),and photoluminescence spectroscopy(PL).Moreover,the influences of the morphologies ofα-Al_2O_3 on the types of crystal structure,morphologies,and photoluminescent properties of LuAG:Ce~(3+)green phosphors were investigated.The results indicated that the morphologies and particle sizes of theα-Al_2O_3 powders could be controlled by the additives and parameters.Notably,the sphericalα-Al_2O_3 powders with good dispersibility were found to be the excellent base materials of LuAG:Ce~(3+)green phosphors for white light emitting diodes.     

UV laser induced transmission change of pure and doped silica glass

Pure and F,GeO2-doped silica glass cut from fiber preforms prepared by plasma assisted chemical vapor deposition（PCVD） were investigated by ultraviolet absorption spectroscopy.The ultraviolet absorption characteristics of these glasses were also studied after UV laser irradiation and heating treatment.It was found that absorption band near 240 nm assigned to GODC was found both in GeO2-doped and F-GeO2 co-doped silica glass,but absorption intensity of the latter was lower than that of the former.It＇s because F can react with GODC and GeE′ simultaneously and reduce their concentration.After irradiation,UV absorption change of F-GeO2 co-doped silica glass was weaker than that of GeO2-doped silica glass,it thus can be concluded that introduction of F could depress the UV absorption of GeO2-doped silica core effectively.     

Microstructure of β-Dicalcium Silicate after Accelerated Carbonation

The present work presents the microstructure of β-Ca_2SiO_4(β-C_2S) after accelerated carbonation. The synthesis procedure of β-C_2S was examined first, and the crystalline and amorphous structure, the distribution and the pore structure of β-C_2S carbonation products were also determined by X-ray diffraction(XRD) quantitative analysis, simultaneous thermal analyzer(TG/DTA), Fourier transform-infrared spectroscopy(FT-IR), high resolution ~(29)Si magic angle spinning nuclear magnetic resonance(~(29)Si NMR), N_2-sorption techniques, and scanning electron microscopy(SEM), respectively. Test results indicate that carbonation products are dramatically formed in the initial 2 h. The main carbonation products are crystalline calcite and amorphous three-dimensional network silica gels, which contain nanometer-sized pores. The calcite, silica gels and un-carbonated β-C_2S are distributed hierarchically.     

Microbiological synthesis of nanophase PbS by Desulfotomaculum sp.

The uniform nanoparticles PbS with diameters about 13 nm could be synthesized by Desulfotomaculum sp. under mild condition. The effects of the processing vari-ables such as pH and temperature were investigated. The obtained products were in detailed by means of transmission electron microscopy(TEM) and X-ray diffraction(XRD) ,respectively. The results revealed that the PbS crystallites were identical in structure,shape and size under different temperatures while their morphology changed from rod to spheroidal with pH increasing. In the biological synthetic process for PbS nanoparticles,Desulfotomaculum sp. can use sulfate as a terminal electron acceptor to produce sulfide which acts as the source of sulfur for the formation of PbS nanoparticles.     

Phase transformation and reduction kinetics during the hydrogen reduction of ilmenite concentrate

The reduction of ilmenite concentrate by hydrogen gas was investigated in the temperature range of 500 to 1200°C.The microstructure and phase transition of the reduction products were studied by X-ray diffraction(XRD),scanning electron microscopy(SEM),and optical microscopy(OM).It was found that the weight loss and iron metallization rate increased with the increase of reduction temperature and reaction time.The iron metallization rate could reach 87.5% when the sample was reduced at 1150°C for 80 min.The final phase constituents mainly consist of Fe,M 3 O 5 solid solution phase(M=Mg,Ti,and Fe),and few titanium oxide.Microstructure analysis shows that the surfaces of the reduction products have many holes and cracks and the reactions take place from the exterior of the grain to its interior.The kinetics of reduction indicates that the rate-controlling step is diffusion process control with the activation energy of 89 kJ·mol-1.     

One-step synthesis route of the aligned and non-aligned single crystalline α-Si_3N_4 nanowires

This paper reports the bulk synthesis route of the aligned and non-aligned high-quality α-Si_3N_4 nanowires (NWS) which were grown directly from the Si substrate by vapor phase deposition at 1050℃. The as-grown products were characterized by employing XRD, SEM, HRTEM and photoluminescence. The microscopic results revealed that the products consist of single crystalline aligned and nonaligned α-Si_3N_4 NWs having a same diameter range of 30-100 nm and different lengths of about hundreds of microns. The XRD observation revealed that the products consist of α-phase Si_3N_4 NWs. The room temperature PL spectra indicated that the NWs have good emission property. The non-aligned NWs were formed at lower temperature as compared with aligned NWs. Our method is a simple and one-step procedure to synthesize the bulk-quantity and high-purity aligned and non-aligned α-Si_3N_4 NWs at a relatively low temperature. The possible growth mechanism was also briefly discussed.     

THE HYDRATES AND MICROSTRUCTURE OF PERMEABLITY RESISTING PORTLAND CEMENT

The hydrating products and microstructure of permeablity resisting portland cement have been studied by x-ray diffraction (XRD) and electron microscopy(EM). The hydrates such as calcium silicates hydrate and calcium sulphaluminate hydrate, ettringite crystal of needles can be observed under the EM, most of which were filled into pores of hardened cement paste.     

Sol-gel preparation and characterization of Co_3O_4 nanocrystals

A new citrate acid-hydrazine sol-gel route for preparation of Co3O4 nanoparticles has been developed. Co3O4 nanoparticles with different particle-sizes and morphology were prepared at different heat-treatment temperatures and the pure cubic nanocrystals of Co3O4 were obtained at 600℃. The synthesis process was monitored by infrared spectroscopy (IR), thermal gravimetric and differential thermal analysis (TG-DTA). The structure and morphology of Co3O4 nanocrystals were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and X-ray-photoelectron spectroscopy (XPS). The infrared absorption bands blue-shifted with particle size decreasing, which could be attributed to increasing surface effect. XPS results showed that predominant species at surface layers of Co3O4 nanocrystals are octahedral Co (Ⅲ).     

Erythrocyte-Like Mg(OH)2 Microspheres Self-Assembled by Nanocrystallites

The erythrocyte-like magnesium hydroxide microspheres were synthesized in large scale through a simple solution phase route. The structures and morphologies of the products were analyzed by the X-ray diffractometer (XRD),scanning electron microscope (SEM),transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM). The possible growth mechanism of the nanostructure was discussed briefly and the potential application was proposed.     

Self-assembly of Ag-TiO2 nanoparticles: Synthesis, characterization and catalytic application

The formation of Ag clusters on titanium oxide (TiO2) nanoparticles was achieved by self-assembly process and calcination. The obtained nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and ultraviolet visible spectroscopy (UV-Vis), and conventional techniques (XRD, TEM and UV-Vis) were used to identify Ag particles on the TiO2 surfaces. The results show that Ag-TiO2 particles can be applied to improve catalytic activity of the epoxidation of styrene oxides. Styrene oxide is the main product of catalytic reaction with H2O2 as the oxidant by using Ag-TiO2 nanoparticles as catalysts. High catalytic activitity of styrene oxide can be obtainable at 80 ℃. The reaction temperature, reaction time, the molar ratio of H2O2/styrene and solvent affect greatly the catalytic epoxidation of styrene.     

Formation of CuS pineal microspheres via a pyridine-solvothermal process

CuS pineal microspheres congregated from interleaving nanoflakes with thickness of 40 to 200 nm were synthesized by a pyridine-solvothermal process via the reaction between cupric chloride(CuCl2·2H2O) and thioacetamide(TAA,CH3CSNH2).The products were characterized by X-ray diffraction and scanning electron microscopy.UV-Vis absorption spectrum,excitation and photoluminescence spectra of CuS pineal microspheres were obtained at room temperature to investigate their optical properties.A possible growth mechanism on the formation of CuS pineal microspheres is proposed.The factors influencing the evolution of morphologies of CuS crystals including the dosage of the reactants,surfactant,and sulphur-source were also analyzed.     

Effect of UV irradiation on PAN precursor fibers and stabilization process

A low-cost rout for modification the polyacrylontrile(PAN) precursor fibers was developed.The approach involved pretreatment PAN precursor fibers with UV irradiation for various periods of time before the fibers were stabilized.The effect of UV irradiation on the chemical structure,orientation factor,density,crystallite size and morphology of the fibers in the process of stabilization was characterized by use of fourier transform infrared spectroscopy(FTIR),float-sink procedure,X-ray diffraction(XRD),scanning electron microscope(SEM),respectively.The results showed that UV irradiation could increase the density of the fibers in stabilization process.FTIR analysis indicated that the cyclization of nitrile groups was initiated at room temperature by UV irradiation.The transformation of C≡N groups to C=N ones was accelerated in the process of stabilization.The orientation factor of irradiated fibers was also increased.The crystallite size was decreased at first and increased later,and the better irradiation time of UV was 3 min according to the XRD test.SEM analysis indicated that irradiation could decrease the internal and surface defects of the stabilized fibers treated at 300 ℃.     

Synthesis and characterization of CePO4 nanorods via solvothermal process

One-dimensional cerium phosphate(CePO4) nanorods were successfully synthesized by a facile and simple solvothermal method at 150 ℃ for 12 h, using Ce(NO3)3·6H2O and NaH2PO4·2H2O as the starting materials. Phase and morphologie of the as-synthesized CePO4 products, characterized by XRD, FESEM, and TEM, were proved to be perfect and uniform hexagonal CePO4 nanorods with aspect ratio of more than 100. The photoluminescence(PL) spectrometer was used to investigate the optical properties of the assynthesized hexagonal CePO4 nanorods.     

Preparation of V-doped TiO2 photocatalysts by the solution combustion method and their visible light photocatalysis activities

A series of nanocrystalline V-doped （0.0-3.0 at.%） TiO2 catalysts have been successfully prepared by the one-step solution combustion method using urea as a fuel. The obtained powders were characterized by XRD, SEM, Raman, XPS and UV-Vis DRS. The effects of V doping concentration on the phase structure and photocatalytic properties were investigated. XRD, Raman, and XPS show that V doping diffuses into TiO2 crystal lattice mainly in the form of V5＋ and causes a phase transition from anatase to mille. V doping can widen the light absorption range of TiO2, with the absorption threshold wavelength shifting from 425 to 625 nm. The photocatalytic activity of V-doped TiO2 powders were evaluated by the photocatalytic degradation of methyl orange （MO） under visible light irradiation. It is found that V doping enhances the photoeatalyilc activity under visible light irradiation and the optimal degradation rate of MO is about 95.8% with 1.0 at% V-doped TiO2.     

The coupling agents’ effects on the BSA intercalated into montmorillonite

The effects of surface modification on montmorillonite （MMT） were illustrated in order to produce the composite material with premium properties. MMT was treated with two coupling agents： glutaraldehyde （GA） and 7-methacryloxy-propyl-trimethoxy silane （KH570）. The effects of different coupling agents on MMT and protein interaction were investigated by XRD, FT-IR, TGA, UV-Vis, etc. The results of structure characterization indicated that KH570 modification could change the surface crystal structure of MMT. However, GA reacted with amino groups of Bovine serum albumin （BSA） and the ordered layer structures of MMT were not completely destroyed. Coupling agents could greatly increase the amounts of BSA intercalated and the effect of KH570 is better than that of GA. And, the optimum concentrations of KH570 and GA were 2% and 6%, respectively. The rate of weight loss increased by about 12% after MMT was pretreated with coupling agents. The possible reason is that coupling agent treatment makes the structure of MMT more accessible to protein absorption and helps to stabilize the protein structure. Moreover,the presence of coupling agents can reduce the direct chemical interaction between BSA and MMT, which results in increasing protein desorption.     

Influence of chemical liquids on the fatigue crack growth of the AZ31 magnesium alloy

The fatigue crack growth behavior of an AZ31 magnesium alloy was investigated by comparing the effect of zirconate and phos-phate chemical liquids.The morphology,components,and phase compositions of the chemical depositions at the fatigue crack tip were analyzed by employing scanning electron microscopy(SEM),energy dispersive spectroscopy(EDS),and X-ray diffraction(XRD),respectively.For samples with and without the chemical liquids,their stress-intensity factor values at the fatigue crack tip were compared by using a stress-strain gauge.The results demonstrated that a zirconate film(ZrxOy·ZnxOy) and a phosphate film(Zn3(PO4)2·4H2O and MgZnP2O7) could be formed on the fatigue crack-surface at the fatigue crack tip.The stress distribution was changed because of the chemical depositions and the causticity of the chemical liquids.This could decrease the stress-intensity factor value and thus effectively cause fatigue crack closure,which reduces the fatigue crack growth rate.Moreover,it was found that the fatigue crack closure effect of zirconates was more positive than that of phosphates.