Direct electrochemical reduction of solid vanadium oxide to metal vanadium at low temperature in molten CaCl2-NaCl

V₂O₅ sintered pellets and graphite rods were employed as the cathode and the anode, respectively; a molten CaCl₂-NaCl salt was used as the electrolyte. Then, V₂O₅ was directly reduced to metal vanadium by the Fray-Farthing-Chen (FFC) method at 873 K to realize low-temperature electrolysis. Two typical experimental conditions, electrolysis time and voltage, were taken into account to investigate the current efficiency and remaining oxygen content in electrolyzed products. The composition and microstructure of the products were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). SEM observations show that a higher voltage (1.8?C3.4 V) and a longer electrolysis time (2?C5 h) can improve the product quality separately, that is, a lower remaining oxygen content and a more uniform microstructure. The products with an oxygen content of 0.205wt% are successfully obtained below 3.4 V for 10 h. However, the current efficiency is low, and further work is required.     

Effects of sintering atmosphere on the physical and mechanical properties of modified BOF slag glass

This study proposes an efficient way to utilize all the chemical components of the basic oxygen furnace (BOF) slag to prepare high value-added glass-ceramics. A molten modified BOF slag was converted from the melting BOF slag by reducing it and separating out iron component in it, and the modified BOF slag was then quenched in water to form glasses with different basicities. The glasses were subsequently sintered in the temperature range of 600–1000℃ in air or nitrogen atmosphere for 1 h. The effects of different atmospheres on the physical and mechanical properties of sintered samples were studied by using differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM) and by conducting experiment on evaluating the sintering shrinkage, water absorption and bulk density. It is found that the kinetics of the sintering process is significantly affected by sintering atmosphere. In particular, compared with sintering in air atmosphere, sintering in N₂ atmosphere promotes the synergistic growth of pyroxene and melilite crystalline phases, which can contribute to better mechanical properties and denser microstructure.     

Effect of sintering temperature on the physical properties and electrical contact properties of doped AgSnO<Subscript>2</Subscript> contact materials

AgSnO₂ electrical contact materials doped with Bi₂O₃, La₂O₃, and TiO₂ were successfully fabricated by the powder metallurgy method under different initial sintering temperatures. The electrical conductivity, density, hardness, and contact resistance of the AgSnO₂/Bi₂O₃, AgSnO₂/La₂O₃, and AgSnO₂/TiO₂ contact materials were measured and analyzed. The arc-eroded surface morphologies of the doped AgSnO₂ contact materials were investigated by scanning electron microscopy (SEM). The effects of the initial sintering temperature on the physical properties and electrical contact properties of the doped AgSnO₂ contact materials were discussed. The results indicate that the physical properties can be improved and the contact resistance of the AgSnO₂ contact materials can be substantially reduced when the materials are sintered under their optimal initial sintering temperatures.     

Effect of SiO2 addition on the dielectric properties and microstructure of BaTiO3-based ceramics in reducing sintering

The effect of SiO₂ doping on the sintering behavior, microstructure, and dielectric properties of BaTiO₃-based ceramics has been investigated. Silica was added to the BaTiO₃-based powder prepared by the solid state method with 0.075mol%, 0.15mol%, and 0.3mol%, respectively. The SiO₂-doped BaTiO₃-based ceramic with high density and uniform grain size were obtained, which were sintered in reducing atmosphere. A scanning electron microscope, X-ray diffraction, and LCR meter were used to determine the microstructure as well as the dielectric properties. SiO₂ can form a liquid phase belonging to the ternary system of BaO-TiO₂-SiO₂, leading to the formation of BaTiO₃ ceramics with high density at a lower sintering temperature. The SiO₂-doped BaTiO₃-based ceramics can be sintered to a theoretical density higher than 95% at 1220℃ with a soaking time of 2 h. The dielectric constants of the sample with 0.15mol% SiO₂ addition sintered at 1220℃ is about 9000. Doping with a small amount of silica can improve the sintering and dielectric properties of BaTiO₃-based ceramics.     

Studies on the effects of pre-firing and sintering temperature on NSDC nanocomposite electrolytes

Solid oxide fuel cells (SOFCs) technology, with fuel flexibility, is one of the most promising power generation technology. However, the high operating temperature of SOFCs has hindered their commercial applications. As a crucial requirement to enhance its performance, SOFCs electrolytes should operate at a low temperature. Carbonate/ceria composites are developed as electrolytes for low operating temperature SOFCs, and a better understanding of the mechanism of its ionic conductivity serves this purpose. In this work, ceria-carbonate composite electrolyte, Na₂CO₃/samarium doped ceria (NSDC) were synthesized by the co-precipitation method. The synthesized electrolytes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and UV–Vis spectroscopy. The XRD and SEM results showed that the sintered NSDC nanocomposite comprised a single-phase dense electrolyte structure. The crystallite size of the NSDC nanocomposite was greatly affected by the different pre-firing temperatures and different sintering temperatures. Also, the ionic conductivity of the prepared NSDC nanocomposite electrolytes was strongly dependent on the pre-firing and sintering temperatures. The NSDC nanocomposite electrolytes were pre-fired at 950 ?°C and 650 ?°C and sintered at 1200 ?°C and 900 ?°C respectively, had ionic conductivity in H₂ and air high as 0.36 ?S/cm and 0.3 ?S/cm.     

Microstructure and electrical conductivity of 10% Yb-doped SrCeO3 ceramics

As a candidate material for hydrogen separation, Yb-doped SrCeO₃ has attracted increasing attention in recent decades. In the present study, Yb-doped SrCe_0.9Yb_0.1O_3-α ceramics were prepared by the dry pressing and sintering approach, with the microstructure evolution and the micro morphology investigated. It was indicated that the ceramics sintered in air were of a pure perovskite structure, and that the sintering temperature had a significant effect on the growth of ceramic grains. The average grain size increased from 1 ​μm to 10 ​μm with an increase in sintering temperature from 1300 to 1500 ​°C. Further investigation of the thermodynamics and kinetics of grain growth revealed that the grain boundary diffusion was the main driving force of grain growth during solid phase sintering, with a grain growth index of 4 and an activation energy of approximately 61.23 ​kJ ​mol⁻¹. These results illustrate an obvious tendency of grain size growth. By electrochemical workstation with different atmospheres the effects of sintering temperature on the conductivity were characterized in the temperature range of 700–900 ​°C. The electrical conductivities σ of SrCe_0.9Yb_0.1O_3-α ceramics in different atmospheres were as follows: σ(wet hydrogen) ​> ​σ(dry hydrogen) ​> ​σ(dry air) ​> ​σ(wet air). In the test atmosphere containing water and hydrogen the conductivity of protons increased with increasing temperature because of the protons jump between lattices in the form of interstitial hydrogen ions or bare protons.     

Preparation and photo-catalytic activity of TiO2-coated medical stone-based porous ceramics

Medical stone-based porous ceramics as a carrier were prepared by ultra-fine grinding and low-temperature sintering method. Nano-TiO₂ thin films were loaded on the carrier by chemical liquid deposition method using titanium tetrachloride as a precursor. The micro-morphology and microstructure of the synthesized samples were characterized using X-ray diffraction, scanning electron microscopy with energy dispersive spectrometry, and mercury injection method. The photo-catalytic activity of the TiO₂ thin films was investigated by degrading formaldehyde. The main crystalline phase in the TiO₂ thin films calcined at 550°C is anatase with the average particle size about 10 nm. The specific surface area of the carrier-coated nano-TiO₂ increases from 3.68 to 5.32 m²/g. The formaldehyde removal rate of the TiO₂/medical stone-based porous ceramics irradiated under an ultraviolet lamp for 120 min reaches 85.6%.     

Manufacture of biomorphic Al2O3 ceramics using filter paper as template

Biomorphic Al₂O₃ ceramics were prepared through the surface sol-gel process with filter papers as bio-templates. The filter papers were infiltrated with γ-AlOOH sol and subsequently sintered in air at high temperatures to produce the biomorphic Al₂O₃ ceramics. The results show that the final materials have a hierarchical structure originated from the morphology of cellulose paper. The sintering temperatures exhibit a strong effect on the surface pore-size distribution of obtained Al₂O₃ ceramics. Differential scanning calorimeter, scanning electron microscopy, X-ray diffraction and BET analysis were employed to characterize the microstructure, morphology and phase compositions of the final products.     

Microwave sintering of Ca<Subscript>0.6</Subscript>La<Subscript>0.2667</Subscript>TiO<Subscript>3</Subscript> microwave dielectric ceramics

Ca_0.6La_0.2667TiO₃ ceramics were prepared by conventional and microwave sintering techniques and their sinterability, microstructure, and microwave dielectric properties were investigated in detail for comparison. Densified Ca_0.6La_0.2667TiO₃ ceramics were obtained by microwave sintering at 1350°C for 30 min and by conventional sintering at 1450°C for 4 h. An unusual phenomenon was found that some larger grains (grain size range: 8–10 μm) inclined to assemble in one area but some smaller ones (grain size range: 2–4 μm) inclined to gather in another area in the microwave sintered ceramics. The microwave dielectric properties of Ca_0.6La_0.2667TiO₃ ceramics prepared by microwave sintering at 1350°C were as follows: dielectric constant (ɛ _r) = 119.6, quality factor (Qf) = 17858.5 GHz, and temperature coefficient of resonant frequency (τ _f) = 155.5 ppm/°C. In contrast, the microwave dielectric properties of the ceramics prepared by conventional sintering at 1450°C were ɛ _r = 117.4, Qf = 13375 GHz, and τ _f = 217.2 ppm/°C.     

Effect of sintering temperature on the microstructure and properties of foamed glass-ceramics prepared from high-titanium blast furnace slag and waste glass

Foamed glass-ceramics were prepared via a single-step sintering method using high-titanium blast furnace slag and waste glass as the main raw materials The influence of sintering temperature (900-1060℃) on the microstructure and properties of foamed glass-ceramics was studied. The results show that the crystal shape changed from grainy to rod-shaped and finally turned to multiple shapes as the sintering temperature was increased from 900 to 1060℃. With increasing sintering temperature, the average pore size of the foamed glass-ceramics increased and subsequently decreased. By contrast, the compressive strength and the bulk density decreased and subsequently increased. An excessively high temperature, however, induced the coalescence of pores and decreased the compressive strength. The optimal properties, including the highest compressive strength (16.64 MPa) among the investigated samples and a relatively low bulk density (0.83 g/cm3), were attained in the case of the foamed glass-ceramics sintered at 1000℃.     

Microwave sintering effects on the microstructure and mechanical properties of Ti-51at%Ni shape memory alloys

Ti-51at%Ni shape memory alloys (SMAs) were successfully produced via a powder metallurgy and microwave sintering technique. The influence of sintering parameters on porosity reduction, microstructure, phase transformation temperatures, and mechanical properties were investigated by optical microscopy, field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC), compression tests, and microhardness tests. Varying the microwave temperature and holding time was found to strongly affect the density of porosity, presence of precipitates, transformation temperatures, and mechanical properties. The lowest density and smallest pore size were observed in the Ti-51at%Ni samples sintered at 900℃ for 5 min or at 900℃ for 30 min. The predominant martensite phases of β2 and β19' were observed in the microstructure of Ti-51at%Ni, and their existence varied in accordance with the sintering temperature and the holding time. In the DSC thermograms, multi-transformation peaks were observed during heating, whereas a single peak was observed during cooling; these peaks correspond to the presence of the β2, R, and β19' phases. The maximum strength and strain among the Ti-51at%Ni SMAs were 1376 MPa and 29%, respectively, for the sample sintered at 900℃ for 30 min because of this sample's minimal porosity.     

机械合金化法制备的Cu/SiC纳米复合材料的组织、热性能和力学性能评估

Nano-sized silicon carbide (SiC: 0wt%, 1wt%, 2wt%, 4wt%, and 8wt%) reinforced copper (Cu) matrix nanocomposites were manufactured, pressed, and sintered at 775 and 875°C in an argon atmosphere. X-ray diffraction (XRD) and scanning electron microscopy were performed to characterize the microstructural evolution. The density, thermal expansion, mechanical, and electrical properties were studied. XRD analyses showed that with increasing SiC content, the microstrain and dislocation density increased, while the crystal size decreased. The coefficient of thermal expansion (CTE) of the nanocomposites was less than that of the Cu matrix. The improvement in the CTE with increasing sintering temperature may be because of densification of the microstructure. Moreover, the mechanical properties of these nanocomposites showed noticeable enhancements with the addition of SiC and sintering temperatures, where the microhardness and apparent strengthening efficiency of nanocomposites containing 8wt% SiC and sintered at 875°C were 958.7 MPa and 1.07 vol%?1, respectively. The electrical conductivity of the sample slightly decreased with additional SiC and increased with sintering temperature. The prepared Cu/SiC nanocomposites possessed good electrical conductivity, high thermal stability, and excellent mechanical properties.     

Ca(Sm0.5Nb0.5)O3介质陶瓷的微波烧结

通过改变微波烧结温度和保温时间,优化Ca( Sm0.5 Nb0.5) O3 (CSN)陶瓷的微波烧结工艺,用X线衍射仪(XRD)、扫描电镜(SEM)和微波网络分析仪等对试样进行表征.从相组成、显微结构及微波介电性能等方面对微波烧结试样与常规烧结试样进行对比分析.结果表明:微波烧结可大幅降低CSN的烧结温度,促进试样的致密化,其物相组成和传统烧结试样无明显差别;微波烧结还可以改善CSN陶瓷的微波介电性能,在1 375℃微波烧结30 min可获得优异的微波介电性能,介电常数(εr)=20.08,品质因数(Q×f)=37.03 THz,谐振频率温度系数(Tf)=-10.2×10-6℃-1.     

Effect of sintering temperature on the microstructure and thermal conductivity of Al/diamond composites prepared by spark plasma sintering

Spark plasma sintering was used to fabricate Al/diamond composites. The effect of sintering temperature on the microstructure and thermal conductivity (TC) of the composites was investigated with the combination of experimental results and theoretical analysis. The composite sintered at 550℃ shows high relative density and strong interfacial bonding, whereas the composites sintered at lower (520℃) and higher (580–600℃) temperatures indicate no interfacial bonding and poor interfacial bonding, respectively. High relative density and strong interfacial bonding can maximize the thermal conductivity of Al/diamond composites, and taking both effects of particle shape and inhomogeneous interfacial thermal conductance into consideration can give a fairly good prediction of composites’ thermal conduction properties.     

Preparation and magnetic properties of CoFe2O4/TiO2 composite films

Using （Ti（OC4H9）4） and metal chlorates as starting materials, CoFe2O4/TiO2 composite films were prepared by sol-gel method. The effects of heat treatment temperature and pH of the precursor on microstructure and magnetic properties were studied. The phase structure of the samples was examined by X-ray diffraction. The microstructure was examined by scanning electron microscope, atomic force microscope and polarized microscope. The magnetic property was measured by vibrating sample magnetometer. The results show that the crystals of different phases grow up independently. CoFe2O4 is uniformly embedded into the TiO2 matrix in the prepared composite films, and the growth of composite films is dependent on the heat treatment temperatures and PH of the precursor. The average size of CoFe2O4 crystal is 19 nm in Nanocomposite film prepared when the heat treatment temperature is 800℃ and the pH of the precursor is between 2 and 3. The magnetism of the composite films is enhanced as the heat treatment temperature increases.     

烧结页岩清水砖抗冻性能研究

广西科技大学新型建筑材料课题组前期试验数据作为理论依据,以烧结页岩砖的原料物理性质为基础,研制开发烧结页岩清水砖。为了进一步研究烧结页岩清水砖的抗冻性能,通过将烧结页岩清水砖与普通烧结页岩砖试件的理化成分与微观结构进行对比分析,再进行冻融循环对比试验,以及砖体在饱水状态下的导热系数测定,得出清水烧结页岩砖抗冻性能要优于普通烧结页岩砖。试验结论为:烧结页岩清水砖抗冻性能达到《墙体材料应用统一技术规范》GB 50574-2010相关指标。为后续试验提供相关数据,为烧结页岩清水砖的推广奠定基础,并建议将饱水状态下的砖体导热系数作为砖体抗冻性能指标之一。     

Mechanism research on arsenic removal from arsenopyrite ore during a sintering process

The mechanism of arsenic removal during a sintering process was investigated through experiments with a sintering pot and arsenic-bearing iron ore containing arsenopyrite; the corresponding chemical properties of the sinter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray diffraction (XRD), and scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). The experimental results revealed that the reaction of arsenic removal is mainly related to the oxygen atmosphere and temperature. During the sintering process, arsenic could be removed in the ignition layer, the sinter layer, and the combustion zone. A portion of FeAsS reacted with excess oxygen to generate FeAsO₄, and the rest of the FeAsS reacted with oxygen to generate As₂O₃(g) and SO₂(g). A portion of As₂O₃(g) mixed with Al₂O₃ or CaO, which resulted in the formation of arsenates such as AlAsO₄ and Ca₃(AsO₄)₂, leading to arsenic residues in sintering products. The FeAsS component in the blending ore was difficult to decompose in the preliminary heating zone, the dry zone, or the bottom layer because of the relatively low temperatures; however, As₂O₃(g) that originated from the high-temperature zone could react with metal oxides, resulting in the formation of arsenate residues.     

甘氨酸-硝酸盐法合成纳米YSZ微粉及其性能

用甘氨酸-硝酸盐法合成了纳米级钇稳定化氧化锆（YS Z）微粉. 用粉末X射线衍射方法对合成产物和煅烧粉体进行物相分析, 并计算了YSZ合成粉 体的平均晶粒尺寸. 用热膨胀仪和交流阻抗谱分别研究了合成原粉的烧结收缩率和烧结样品 的电学性能. 研究结果表明, 当金属离子与甘氨酸的摩尔比为1∶2时, 用甘氨酸-硝酸盐 法可直接合成纳米级YSZ微粉, 600 ℃和1 000 ℃煅烧粉体的平均晶粒尺寸分别为9.8 5和40.5 nm. 经1 000 ℃预烧的YSZ样品的烧结性能明显高于1 200 ℃预烧YSZ样品. YSZ样 品在1 400 ℃烧结6 h的相对密度分别为99.3%和98.6%, 烧结温度范围为1 400~1 450 ℃ . 经1 450 ℃烧结后的样品在850 ℃时电导率分别为0.037和0.021 S/cm.     

利用反应烧结法制备多孔碳化物陶瓷

利用反应烧结的方法,通过甲烷碳化还原三种过渡金属氧化物( Cr2 O3、TiO2和WO3)压坯,制备了其相应的多孔形态的碳化物( Cr3 C2、TiC和WC)陶瓷。通过扫描电子显微镜观察检测,对反应烧结产物的表面和截面形貌进行了分析,并对这三种过渡金属碳化物的孔隙结构进行了初步的表征。通过物相分析研究了反应烧结的动力学过程,发现利用含体积分数10%甲烷的混合气体碳化还原制备多孔TiC和WC陶瓷的起始温度分别为1200℃和1000℃,低于这两个温度时发生其他相变,有其他中间产物生成。利用反应烧结的方法制备多孔Cr3 C2陶瓷时,反应烧结温度越高,碳化铬陶瓷的骨架和孔隙平均尺寸越大。     

镀钨碳纳米管增强铜基复合材料的制备及性能

采用羰基热分解法对多壁碳纳米管表面进行镀钨处理,并以镀钨碳纳米管和电解铜粉为原料,进行机械球磨混粉和放电等离子体烧结,制备了镀钨碳纳米管/铜基复合材料.采用场发射扫描电镜观察了粉体和复合材料的组织形貌,并对复合材料物相进行了X射线衍射分析.探讨了镀钨碳纳米管含量和放电等离子体烧结温度对复合材料致密度、抗拉强度、延伸率和电导率的影响.结果表明,镀钨碳纳米管质量分数为1%和烧结温度为850℃时,复合材料的致密度、抗拉强度和电导率最高.与烧结纯铜相比,复合材料的抗拉强度提高了103.6%,电导率仅降低15.9%.