Surface modification of Ti-45Al-8.5 Nb alloys by microarc oxidation to improve high-temperature oxidation resistance

Microarc oxidation(MAO)electrolysis plasma deposition was used to prepare Al_2O_3coatings on Ti-45Al-8.5 Nb alloys to improve high temperature oxidation resistance.The surface and cross-section morphologies before and after high-temperature oxidation,the chemical composition,and the phase identification of the coatings were investigated by scanning electron microscopy(SEM),electron probe microanalyses(EPMA),and X-ray diffraction(XRD).The results show that Al_2O_3coatings with a thickness of approximately 8μm can be obtained on the Ti-45Al-8.5 Nb alloys by MAO for 600 s.The samples with the Al_2O_3coatings exhibited better high-temperature oxidation resistance.A minimal weight gain of only 0.396 g/m~2after 100 h oxidation at 900°C was observed for the coatings formed with a deposition voltage of 400 V and using a duty cycle of 3%.The deposition mechanism of the Al_2O_3coatings and the effect of the MAO parameters are also described.     

Experimental and theoretical studies of the reaction between cationic vanadium oxide clusters and acetylene

The time of flight mass spectrometer coupled with a laser ablation/supersonic expansion cluster source and a fast flow reactor was adopted to study the reactivity of cationic vanadium oxide clusters （VinOS,） toward acetylene （C2H2） molecules under gas phase （P, - 1.14 kPa）, under near room temperature （T, - 350 K） conditions. Association products, VmOnC2H2^＋ （m,n = 2,4; 2,6; 3,7-8; 4,9-11; 5,12-13; 6,13-16, and 7,17）, are observed. The oxidation of C2H2 by （V2Os）n^＋ （n = 1 -3） is experimentally identified. The reactivity of （V2O5）n^＋ decreases as n increases. Density functional theory （DFT） calculations were carried out to interpret the reaction mechanisms. The DFT results indicate that a terminal oxygen atom from V2O5^＋ can transfer overall barrierlessly to C2H2 at room temperature, which is in agreement with the experimental observation. Other experimental results such as the observation of V206C2H2^＋ and nonobservation of V2O7,8C2H2^＋ in the experiments are also well interpreted based on the DFT calculations. The reactivity of vanadium oxide clusters toward acetylene and other hydrocarbons may be considered in identifying molecular level mechanisms for related heterogeneous catalysis.     

Mechanism of electrochemical evolution of chlorine and oxygen at Ti/SnO2-IrO2 anode

The mechanisms of chlorine and oxygen electrochemical evolution at a novel Ti/SnO₂-IrO₂ anode were investigated using cyclic voltammetry and steady state current?potential measurements. For this study a laboratory constructed model cell was employed. Firstly, controlled potential electrolysis of 0.1 mol/L NaCl was performed and chlorine was observed to evolve at potential +1.2 V. The pH values of the solution decreased during electrolysis over the potential range of +1.0 V?+2.0 V, suggesting that oxygen evolution may involve in the reactions. Electrolysis with a de?oxygenated NaCl solution at a fixed potential of +2.0 V confirmed that O2 is one of the products generated at the anode. Further electrolysis of NaCl solution was conducted under steady state conditions. A potential?current density plot was constructed over the potential range of +1.00 V?+1.28 V. The slope of the plot at Tafel section was found to be 41 mV/decade. These results indicate that chlorine evolution at the anode is achieved via an intermediate layer formed by electrosorption of oxygen and chlorine on the electrode surface.     

A novel process for comprehensive utilization of vanadium slag

Traditional processes for treating vanadium slag generate a huge volume of solid residue and a large amount of harmful gas, which cause serious environmental problems. In this study, a new process for the comprehensive utilization of vanadium slag was proposed, wherein zeolite A and a V₂O₅/TiO₂ system were synthesized. The structural properties of the as-synthesized zeolite A and the V₂O₅/TiO₂ system were characterized using various experimental techniques, including X-ray diffraction, X-ray fluorescence, scanning electron microscopy, and infrared spectroscopy. The results reveal that zeolite A and the V₂O₅/TiO₂ system are successfully obtained with high purity. The results of gas adsorption measurements indicate that the prepared zeolite A exhibits high selectivity for CO₂ over N₂ and is a candidate material for CO₂ capture from flue-gas streams.     

A new process of extracting vanadium from stone coal

A new process of extracting vanadium from the stone coal vanadium ore in Fangshankou, Dunhuang area of Gansu Province, China was introduced. Various leaching experiments were carried out, and the results show that the vanadium ore in Fangshankou is difficult to process due to its high consumption of acid and the high leaching rate of impurities. However, the leaching rate can be up to 80% and the content of V₂O₅ in the residue can be between 0.22%–0.25% in the process of ore fine grinding→oxidation roasting→mixing and ripening→aqueous leaching→P₂O₄ solvent extraction→sulfuric acid stripping→oxidation and precipitation→decomposition by heat. Also, the quality of flaky V₂O₅ produced by this process can meet the requirements of GB3283–87. The total leaching rate of vanadium is 70%. Also, three types of wastes are easy to treat. The vanadium extraction process is better in relation to the aspect of environmental protection than the sodium method.     

Electro-deoxidation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> in molten CaCl<Subscript>2</Subscript>-NaCl-CaO

The electro-deoxidation of V₂O₃ precursors was studied. Experiments were carried out with a two-terminal electrochemical cell, which was comprised of a molten electrolyte of CaCl₂ and NaCl with additions of CaO, a cathode of compact V₂O₃, and a graphite anode under the potential of 3.0 V at 1173 K. The phase constitution and composition as well as the morphology of the samples were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM). 3 g of V₂O₃ could be converted to vanadium metal powder within the processing time of 8 h. The kinetic pathway was investigated by analyzing the product phase in samples prepared at different reduction stages. CaO added in the reduction path of V₂O₃ formed the intermediate product CaV₂O₄.     

Structure of V2O5-P2O5-Sb2O3-Bi2O3 glass

The structure of V₂O₅-P₂O₅-Sb₂O₃-Bi₂O₃ glass and its state of crystallization were studied by means of infrared spectroscopy and X-ray diffraction analysis. The results indicate that, in this glass, V and P exist mainly in the form of a single-stranded linear (VO₃) _n and an isolated (PO₄) tetrahedral with no double bond. Partial V and P are connected through O, forming an amorphous structure of layered vanadium phosphate. Trivalent Sb³⁺ and Bi³⁺ open the V=O bond and appear in interlayers, so a weak three-dimensional structure is connected successfully. Along with the substitution of Sb₂O₃ for partial V₂O₅ or that of P₂O₅ for partial V₂O₅, the network structure of the glass is reinforced, and the crystallization is reduced.     

Effects of aluminum and titanium on the microstructure of ODS steels fabricated by hot pressing

Three oxide-dispersion-strengthened (ODS) steels with compositions of Fe-14Cr-2W-0.2V-0.07Ta-0.3Y₂O₃ (wt%, so as the follows) (14Y), Fe-14Cr-2W-0.2V-0.07Ta-1Al-0.3Y₂O₃ (14YAl), and Fe-14Cr-2W-0.2V-0.07Ta-0.3Ti-0.3 Y₂O₃ (14YTi) were fabricated by hot pressing. Transmission electron microscopy (TEM) was used to characterize the microstructures and nanoparticles of these ODS steels. According to the TEM results, 14Y, 14YAl, and 14YTi ODS steels present similar bimodal structures containing both large and small grains. The addition of Al or Ti has no obvious effect on the microstructure of the steels. The spatial and size distribution of the nanoparticles was also analyzed. The results indicate that the average size of nanoparticles in the 14YTi ODS steel is smaller than that in the 14YAl ODS steel. Nanoparticles such as Y₂O₃, Y₃Al₅O₁₂ and YAlO₃, and Y₂Ti₂O₇ were identified in the 14Y, 14YAl, and 14YTi ODS steels, respectively.     

Effects of synthetic conditions on the structure and morphology of open-ended vanadium oxide nanotubes and study of their growth mechanism

Vanadium oxide nanotubes (VOx-NTs) have been synthesized by using n-butylamine as structuredirecting template and V2O5 as precursor under hydrothermal conditions. XRD, FTIR, SEM, TEM, BET and TG-DTA characterizations have been performed to both optimize the synthetic conditions and understand the growth mechanism of VOx-NTs. The results showed that open-ended VOx-NTs were obtained under the optimized conditions (hydrothermal temperature: 150―160°C, hydrothermal time: 5―7 d, the molar ratio of V2O5 to n-butylamine is 1:1) with diameters ranging from about 30 to 100 nm and several micrometers in length. The BET surface area and the desorption cumulative pore volume of pores of the as-synthesized sample were about 27.4609 m2/g and 0.191087 cm3/g, respectively. The result presents that the synthesis of VOx-NTs is controlled by the "rolling" mechanism and temperature is primary driving force for rolling.     

Effect of sintering temperature on the electrolysis of TiO2

The effects of sintering temperature on the microstructure and the conductivity of TiO₂ cathodes were studied by examining the phase composition, microstructure, and element contents of the sintered cathodes and the cathodic products using X-ray diffraction and scanning electronic microscopy-energy dispersive spectrometry. The oxygen vacancy, conductivity, average pore diameter, and specific surface area of the sintered cathodes were detected by X-ray photoelectron spectroscopy, four-point probe, and ASPA 2010. The results showed that TiO₂ phase transformations occurred, and oxygen vacancies formed with the increase of sintering temperature. The cathodic conductivity improved, but the average pore diameter and the effective response area of the TiO₂ cathode were reduced when the sintering temperature increased. These phenomena could weaken the contact between reaction ions and electrons and also had the same effect on the cathodes and the molten salt. Moreover, they were disadvantageous to ion migration, so a lower sintering temperature was favorable for the microstructure of electrolysis. Consequently, the cathodic conductivity may be improved, but the microstructure became compact with the increase of sintering temperature. The cathodic products at different temperatures indicated that the cathodic conductivity was more important for electrolysis.     

Synthesis and Structure of Polypyrrole Derivatives／V2O5 Nanocomposites

Poly ( N, N, N-trimethyl ( 2-pyrrol-l-yl ) ethyl ammonium iodide )/V2O5 ( PTPAI/V2O5) nanocomposites were synthesized by sol-gel method. This method involved formation of vanadium pentoxide xerogel in the prcscnce of polypyrrole derivatives solution. X-ray diffraction(XRD) indicated that the polypyrrole derivative particles encapsulated in the fibrous V2O5 network and the layered distance significantly increased from 1. 077 39 to 1. 354 56 nm. The interaction between polypyrrole and V2O5 in the ‘nanocomposites‘ was characterized by IR spectroscopy. The Scanning Electron Microscope(SEM) micrographs reveal the structural contrasts between the hybrid materials and the pristine vanadium oxide xerogel.     

Preparation of narrow band gap V2O5/TiO2 composite films by micro-arc oxidation

V₂O₅/TiO₂ composite films were prepared on pure titanium substrates via micro-arc oxidation (MAO) in electrolytes consisting of NaVO₃. Their morphology and elements were characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) analysis. Phase composition and valence states of species in the films were characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Ultraviolet-visible diffuse reflectance spectra (UV-Vis DRS) were also employed to evaluate the photophysical property of the films. The V₂O₅/TiO₂ composite films show a sheet-like morphology. Not only V₂O₅ phase appears in the films when the NaVO₃ concentration of the electrolyte is higher than 6.10 g/L and is loaded at the surface of anatase, but also V⁴⁺ is incorporated into the crystal lattice of anatase. In comparison with pure TiO₂ films the V₂O₅/TiO₂ composite films exhibit significantly narrow band gap energy. The film prepared in an electrolyte consisting of NaVO₃ with a concentration of 8.54 g/L exhibits the narrowest band gap energy, which is approximately 1.89 eV. The V₂O₅/TiO₂ composite films also have the significantly enhanced visible light photocatalytic activity. The film prepared in an electrolyte consisting of NaVO₃ with a concentration of 8.54 g/L exhibits the best photocatalytic activity and about 93% of rhodamine is degraded after 14 h visible light radiation.     

LF精炼过程中SAE8620钢所含MgO复合夹杂物分析

采用非水溶液电解的方法,萃取分离出SAE8620齿轮钢中含MgO复合夹杂物,利用扫描电镜、能谱分析仪对夹杂物的组成、类型和形貌特征进行分析。结果表明,SAE8620齿轮钢在LF精炼过程中,含MgO复合夹杂物中MgO、CaO含量逐渐增加,SiO2含量逐渐减少,Al2O3含量呈先上升后下降的趋势;夹杂物的形貌多不规则,呈块状且棱角分明;夹杂物类型主要为SiO2-Al2O3-MgO、SiO2-MgO、SiO2-Al2O3-CaO-MgO等,此类夹杂物的尺寸较大、熔点较高,直接影响钢材的质量和使用性能。     

机械合金化-热处理制备V5Si3材料

[目的]为了获得V/Si类化合物基本结构和性能,拟合成V/Si系金属间化合物V_5Si_3。[方法]采用V粉和Si粉作原料,按照原子比V∶Si=5∶3进行称量,通过机械合金化与热处理制备V_5Si_3,再利用XRD,SEM/EDS等方法对球磨粉体试样和热处理试样的物相组成、微观形貌和微区成分进行分析与表征,并测量其抗压性能和硬度。[结果]V/Si粉体经过球磨后颗粒度减小,逐渐非晶化,最终得到以原子比V∶Si=5∶3结合的非晶态物质;经过热处理,非晶态结构转变为V_5Si_3晶体。[结论]随着热处理温度的升高,晶体结晶度提高,材料的抗压强度和显微硬度增加,抗压强度达到640 MPa,显微硬度最高为656 MPa。     

Synthesis mechanism of LiNiVO4 by wet chemical method and mixed valence of nickel and vanadium

The single phase LiNiVO₄ has been successfully synthesized by adopting a new mild liquid route with oxalic acid as both complexant and precipitant, and this method is named the CPG method. The products were obtained by sintering the dry gel precursor which was prepared by the CPG method at 200—850℃ for 2—10 h in air. The products were tested by XRD, XPS, ESR and TGA-DTA, and the results indicate that the single phase LiNiVO₄ could be obtained at 450℃ for 2—3 h in air and LiNiVO₄ was still steady at 850℃ for 10 h. The valence analyses show that in LiNiVO₄ the valence of lithium is +1, both nickel and vanadium have the mixed valence, namely +2, +3 for nickel and +4, +5 for vanadium respectively. The LiNiVO₄ can be expressed as LiNi³⁺_xNi²⁺_1-xV⁴⁺_xV⁵⁺_1-xO₄ (0≤x<1). The pyrolysis mechanism of the dry gel is also discussed.     

Synthesis of Mg2B2O5 whiskers via coprecipitation and sintering process

Mg₂B₂O₅ whiskers with high aspect ratio were synthesized by coprecipitation and sintering process using MgCl₂·6H₂O, H₃BO₃, and NaOH as raw materials and KCl as a flux. Their formation process was investigated by thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), and scanning electron microcopy (SEM). It is found that the products synthesized at 832°C are monoclinic Mg₂B₂O₅ whiskers with a diameter of 200?C400 nm and a length of 50?C80 ??m. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) analyses show that the whiskers obtained at 832°C are single crystalline and grow along with the [010] direction. The growth mechanism of Mg₂B₂O₅ whiskers was also presented.     

Effect of SiO<Subscript>2</Subscript> addition on the microstructure and electrical properties of ZnO-based varistors

The microstructure and electrical properties of ZnO-based varistors with the SiO₂ content in the range of 0–1.00mol% were prepared by a solid reaction route. The varistors were characterized by scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray spectrometry, inductively coupled plasma-atomic emission spectrometry, and X-ray photoelectron spectroscopy. The results indicate that the average grain size of ZnO decreases with the SiO₂ content increasing. A new second phase (Zn₂SiO₄) and a glass phase (Bi₂SiO₅) are found. Element Si mainly exists in the grain boundary and plays an important role in controlling the Bi₂O₃ vaporization. The electric measurement shows that the incorporation of SiO₂ can significantly improve the nonlinear properties of ZnO-based varistors, and the nonlinear coefficients of the varistors with SiO₂ are in the range of 36.8–69.5. The varistor voltage reaches the maximum value of 463 V/mm and the leakage current reaches the minimum value of 0.11 μA at the SiO₂ content of 0.75mol%.     

电Fenton法处理DDNP废水的试验研究

针对二硝基重氮酚(DDNP)废水难于被微生物降解的问题,采用电Fenton法处理DDNP废水,通过试验考察不同反应条件对其COD和色度去除率的影响.试验结果表明:电解时间为3.5h,pH为4,H2O2(质量分数为30％)的投加量为10mL/L,电解电压为12 V时,去除效果最佳,COD去除率可达97.24％,色度去除率可达93.75％.     

Microstructure and electrolysis behavior of self-healing Cu-Ni-Fe composite inert anodes for aluminum electrowinning

The microstructure evolution and electrolysis behavior of (Cu₅₂Ni₃₀Fe₁₈)-xNiFe₂O₄ (x=40wt%, 50wt%, 60wt%, and 70wt%) composite inert anodes for aluminum electrowinning were studied. NiFe₂O₄ was synthesized by solid-state reaction at 950℃. The dense anode blocks were prepared by ball-milling followed by sintering under a N₂ atmosphere. The phase evolution of the anodes after sintering was determined by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The results indicate that a substitution reaction between Fe in the alloy phase and Ni in the oxide phase occurs during the sintering process. The samples were also examined as inert anodes for aluminum electrowinning in the low-temperature KF-NaF-AlF₃ molten electrolyte for 24 h. The cell voltage during electrolysis and the corrosion scale on the anodes were analyzed. The results confirm that the scale has a self-repairing function because of the synergistic reaction between the alloy phase with Fe added and the oxide phase. The estimated wear rate of the (Cu₅₂Ni₃₀Fe₁₈)-50NiFe₂O₄ composite anode is 2.02 cm·a-1.     

Transition-metal-doped Fe2O3 nanoparticles for oxygen evolution reaction

Hematite(α-Fe_2O_3)has been extensively studied as a promising photocatalyst,with the capacity to split water under visible light.To tune its electronic structure and improve the performance for oxygen evolution reaction(OER),high-quality single crystals ofα-Fe_2O_3nanoparticles were synthesized and doped by various transition metals(M=V,Cr,Mn,Zn,Co,Ni,Cu,Nb,Mo,Ti)by a molten-salt flux method.Optical,electronic and catalytic properties of transition-metal-dopedα-Fe_2O_3(TM-dopedα-Fe_2O_3)have been systematically investigated.Cobalt has been identified as the best dopant forα-Fe_2O_3,reducing the OER overpotential by 0.16 V with respect to the undoped.