高纯Ti2AlC粉末的无压制备及其在Ag基电触头材料的应用

Ag基电触头是低压开关的“心脏”, 触头无Cd化一直困扰着人们, 寻找新型环保电触头材料是目前低压开关领域研究的重点。本研究从Ag基电触头增强相材料设计入手, 利用简单快速的无压技术合成了高纯Ti₂AlC粉末(99.2%), 制备的Ag/Ti₂AlC复合电触头材料组织均匀、Ti₂AlC颗粒与Ag基体结合紧密、相对密度高(95.7%)、硬度适中(96HV)、导电性好(电阻率低至79.5 nΩ·m)、抗电弧侵蚀性能优良(5610次电弧放电后触头质量损失仅为4.4wt%)。Ag/Ti₂AlC优良的结构和性能主要归因于Ti₂AlC本身的导电导热性能和Ag/Ti₂AlC之间的润湿性。该复合材料在进一步深入研究后, 有望大面积应用并替代传统电触头材料。     

Shear strength and wettability of active Sn3.5Ag4Ti(Ce,Ga) solder on Al2O3 ceramics

The work deals with the study of wettability of Sn3.5Ag4Ti(Ce,Ga) solder on ceramic material of Al₂O₃. The Sn3.5Ag4Ti(Ce,Ga) solder is used for ultrasonic soldering of metallic and ceramic materials. The microstructure of Sn3.5Ag4Ti(Ce,Ga) solder consists of a tin matrix, where non-uniformly distributed constituents of partially dissolved Ti and uniformly distributed fine needles of Ag–Sn phase were observed. The solder was of heterogeneous composition. X-ray diffraction analysis has revealed the presence of following phases: Ag₃Sn, Ti₆Sn₅, Ti₃Sn. For determination of melting point, the Differential scanning calorimetry analysis (DSC) was performed. Wettability of Sn3.5Ag4Ti(Ce,Ga) solder was determined at temperatures 800, 850 and 900 °C in dependence on wetting time. The best wettability of solder Θ = 46° was achieved at 850 °C/43 min. The experiments with high-temperature activation were performed in vacuum of 10^?4 Pa. On the basis of experience attained by measurement of contact angle, the soldered joints of Al₂O₃/Al₂O₃ and Al₂O₃/metal were fabricated in conditions of high-temperature activation in vacuum at temperature 850 °C/10 min. For comparison, also the joints fabricated in the conditions of ultrasonic activation in the air at temperature 280 °C/1 min were applied. The shear strength of joints of Al₂O₃/Al₂O₃ and Al₂O₃/metal fabricated with Sn3.5Ag4Ti(Ce,Ga) solder varied from 17 to 35 MPa. The shear strength of joints fabricated in vacuum is slightly higher than in the case of joints fabricated by use of power ultrasound.     

Structural,electrical, and rheological properties of palladium/silver bimetallic nanoparticles prepared by conventional and ultrasonic-assisted reduction methods

Polyvinylpyrrolidone stabilized Pd/Ag bimetallic nanoparticles (NPs) with average particle sizes of 9 and 6 nm were synthesized by simultaneous reduction in the presence and absence of ultrasound waves, respectively. The prepared NPs were characterized by six methods including X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution-TEM (HRTEM), UV–vis spectroscopy, scanning tunneling microscopy (STM), and energy dispersive X-ray (EDX) analysis. The rheological properties of Pd/Ag NPs in ethylene glycol as a base fluid with various mass fractions of NPs from 2% to 5% at different temperatures were studied experimentally and theoretically. The experimental results showed that viscosity of Pd/Ag NPs in ethylene glycol increases with increasing particle mass fraction and decreases with increasing temperature. A maximum of 31.58% increase in viscosity of ethylene glycol at 20 °C was observed when 5% Pd/Ag NPs was added. Measurement of the electrical conductivity of nanofluids of Pd/Ag bimetallic NPs in distilled water at different mass fractions and temperatures was performed. A 3841% increase in electrical conductivity of distilled water at 25 °C was observed when 1% Pd/Ag NPs was added. Both the rheological and electrical properties of Pd/Ag bimetallic NPs were measured in ethylene glycol and distilled water, respectively for the first time.     

Measurements of the microhardness,electrical and thermal properties of the Al–Ni eutectic alloy

Al–5.7 wt% Ni eutectic alloy was directionally solidified upward with different temperature gradients (0.83–4.02 K/mm) at a constant growth rate (0.008 mm/s) and with different growth rates (0.008–0.483 mm/s) at a constant temperature gradient (4.02 K/mm). Microhardness (HV) and electrical resistivity (ρ) of directionally solidified samples were measured using microhardness test device and a standard d.c. four-point probe technique, respectively. Dependency of the microhardness and electrical resistivity on the solidification processing parameters (temperature gradient, G and growth rate, (V) were analyzed. According to these results, it has been found that the values of HV and ρ increase with the increasing values of G and V. Variations of electrical resistivity and electrical conductivity (σ) for casting Al–Ni eutectic alloy were also measured at the temperature in range 300–720 K. The enthalpy of fusion (ΔH) for the Al–Ni eutectic alloy was determined by differential scanning calorimeter (DSC) from heating trace during the transformation from solid to liquid.     

Synthesis and microstructural characterization of Al–Ni3Al composites fabricated by press-sintering and shock-compaction

Aluminum matrix composites reinforced with nanocrystalline Ni3Al intermetallic particles, were synthesized using powder metallurgy techniques. Nanocrystalline Ni3Al was obtained by mechanical alloying of Ni75–Al25 stoichiometric mixture from elemental powders after 900 ks of milling with a 5 nm grain size average. Mixture powders of aluminum with 0.007, 0.02 and 0.04 volume fractions of Ni3Al intermetallic particles were compacted using two different compaction methods, the cold isostatic press and sintered at 873 K and the shock-compaction technique. Microstructure of shock-compacted composites showed fine particles of a few microns and also coarse particles less than 100 μm homogeneously distributed on the matrix, also the presence of micro-cracks and low porosity. However the nanoscale features of intermetallic was retained. On the other hand, the press and sintered composites showed good densification. The densities of the composites were about 90% and 94% of the theoretical density for the shock-compacted and press-sintered process, respectively. Finally, the results of hardness measurements showed that the nanocrystalline Ni3Al reinforcement improves the hardness of Al matrix for all conditions. The highest hardness was obtained for the Al–4 vol.%Ni3Al shock-compacted composite.     

Silver diffusion and high-temperature lubrication mechanisms of YSZ–Ag–Mo based nanocomposite coatings

Yttria-stabilized zirconia (YSZ) nanocomposite coatings consisting of silver and molybdenum were produced by a hybrid process of filtered vacuum arc, magnetron sputtering and pulsed laser depositions for tribological investigations at different temperatures. The coatings with 24 at.% Ag and 10 at.% Mo contents showed a friction coefficient of 0.4 or less for all temperatures from 25 to 700 °C. The wear scar surfaces and coating cross-sections were studied using scanning electron, transmission electron, scanning transmission electron and focused ion beam microscopes, which also provided the information on chemical composition distributions of silver and molybdenum along with microstructure features. It was demonstrated that silver diffusion and coalescence on surfaces played an important part in the high-temperature lubrication mechanism of the YSZ–Ag–Mo coatings. Silver was found to be an effective lubricant at temperatures below 500 °C and its coalescence on the surface isolated molybdenum inside coatings from ambient oxygen. Lubricious oxides of molybdenum were formed and lubricated at temperatures above 500 °C when the silver was worn off the contact surface. For silver containment inside the coating at high temperatures, a multilayer architecture was built by inserting a TiN diffusion barrier layer in the composite coatings. Microscopic observations showed that this barrier layer prevented silver exit to the coating surface. At the same time, this enabled a subsequent lateral lubricant supply toward a wear scar location where the diffusion barrier layer was worn through and/or for a next thermal cycle. The multilayer coating maintained a friction coefficient of 0.4 or less for more than 25,000 cycles, while the monolithic coating lasted less than 5000 cycles. In addition, a TiN surface barrier layer with pinholes was deposited on the YSZ–Ag–Mo composite surface to control vertical silver diffusion. With this coating design, the coating wear lifetime was significantly increased beyond 50,000 cycles.     

Enhanced microwave absorbing properties of carbonyl iron-doped Ag/ordered mesoporous carbon nanocomposites

Microwave absorbing materials carbonyl iron (CI)-doped Ag/ordered mesoporous carbon (OMC) paraffin wax composites were prepared by colloidal deposition and impregnation methods, and their electromagnetic and microwave absorbing properties were investigated in the frequency ranging from 2 to 18 GHz. The microstructures and chemical compositions of the Ag/OMC and Ag/OMC-CI paraffin wax composites were characterized by TEM, XRD, XPS, SEM and EDS, respectively. The complex permittivity of the paraffin wax composites show dual resonance behavior, resulting from the multi-interfaces among Ag nanoparticles, OMC nanorods, CI and paraffin wax. The magnetic loss was mainly caused by natural resonance and eddy current loss, respectively. The minimum reflection loss (RL) value of Ag/OMC-CI was below ?10 dB at 12 GHz, which were superior to those of OMC-CI and Ag/OMC. This phenomenon is attributed to the enhancement of dielectric polarization and magnetic loss.     

Improvements of the Si3N4 brazed joints with intermetallics

The bonding of Si₃N₄ ceramics with Ag–Cu–Ti, Ni and Ti was performed. The influencing factors on joint strength were investigated. Cu–Ni–Ti intermetallic particles formed in situ were observed in the joints. Scanning electron microscopy photographs show that the interfacial reaction layer is constituted of two layers. The intermetallic particles are homogeneously distributed in the matrix so that they could contribute to the decrease in the residual stresses and the improvement of the joint strength. When bonded with proper parameters, the joint shear strength can reach more than 200 MPa, with a peak experimental value of 215.33 MPa.     

Electrical properties of Ni/silica gel and Pt/γ-alumina catalysts in relation to metal content in the frequency domain

AC electrical conductivity analysis for silica gel and silica gel-supported nickel (via 2, 5 and 8 wt.% Ni) and γ-alumina and γ-alumina-supported platinum (viz., 0.3 and 0.6 wt.% Pt) is carried out. Measurements were carried out in the frequency range from 0.1 Hz up to 100 kHz at room temperature (20 °C) and 1 V for estimating the effect of increasing Ni or Pt on its supports namely silica gel and γ-alumina. Electrical properties of such mesoporous materials reflect directly its ion exchange and interfacial catalytic activity. Assuming that Ni or Pt particles are optimally dispersed over the surface of its supports, this may give rise to an increase in the conductivity and dielectric constant of the studied system.Electrical properties of pure γ-Al₂O₃ and silica gel supports depend on metal content and frequency of the applied field. The observed increase in conductivity with the increase in metal loadings may be due to the increase in the mobility of the free charge carriers. These charge carriers diffuse in the bulk of pores and reach electrodes and discharge there giving rise to diffusion impedance (Warburg impedance).An equivalent circuit is deduced to describe the electrical behavior of the systems studied. It constitutes elements forming three mechanisms: ion exchange at interfaces, diffusion in the pores and high frequency effect (beyond the scope of this work). The study evidenced that the increase of metal content has a great effect on the electrical properties of the studied system.     

Ag基复合材料的研究进展

重点从银基复合材料的主要应用--电接触材料出发,总结了银基复合材料的研究状况,介绍了Ag-金属氧化物和Ag-Ni系列材料耐电弧腐蚀性能的研究进展.提出,复层合金多元化是银基复合材料发展的一大趋势,可改善材料性能以提高其硬度和耐磨性;从功能梯度的角度出发使结构多层化,提高复合材料的复合界面强度也是银基复合材料发展的新趋势.     

Structural and electrochemical properties of nanostructured nickel silicides by reduction and silicification of high-surface-area nickel oxide

Nanostructured nickel silicides have been prepared by reduction and silicification of high-surface-area nickel oxide (145 m² g^?1) produced via precipitation. The prepared materials were characterized by nitrogen adsorption, X-ray diffraction, thermal analysis, FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, magnetic and electrochemical measurements. The nickel silicide formation involves the following sequence: NiO (cubic) → Ni (cubic) → Ni₂Si (orthorhombic) → NiSi (orthorhombic) → NiSi₂ (cubic), with particles growing from 13.7 to 21.3 nm. The nickel silicides are ferromagnetic at room temperature, and their saturation magnetization values change drastically with the increase of Si content. Nickel silicides have remarkably low electrical resistivity and noble metal-like properties because of a constriction of the Ni d band and an increase of the electronic density of states. The results suggest that such silicides are promising candidates as inexpensive yet functional materials for applications in electrochemistry as well as catalysis.     

Toxicity assessment of three-component Fe–Cr–Ni biomedical materials using an augmented simplex design

This study firstly establishes the toxicity assessment of three-component Fe–Cr–Ni biomedical materials using Probit dose–response model and augmented simplex design. The individually determined toxicity rankings of these three cations is in the order Ni²⁺ ≥ Cr³⁺ > Fe³⁺. The ternary Fe–Cr–Ni system's EC₅₀ contour plot shows a hump with EC₅₀ = 897.5 mg/L, and a saddle with EC₅₀ = 637.5 mg/L. Ternary Fe–Cr–Ni biomedical implants may possess good biocompatibility when the chemical compositions of selectively leached metal ions approach the hump region, but present at increased toxic risk when close to the saddle region. Toxicity of Fe–Cr–Ni three-component biomedical materials with various chemical compositions can be predicted and verified economically and efficiently using an augmented simplex design.     

Dissimilar joining of Ti3Al-based alloy to Ni-based superalloy by arc welding technology using gradient filler alloys

In this study, Ti–Al–Nb, Ti–Ni–Nb and Ni–Cr–Nb system alloys were designed and incorporated in order to construct a gradient structure at the surface of the joined Ti₃Al base material. And the Ti₃Al-based alloy and Ni-based superalloy were successfully joined together using gas tungsten arc (GTA) welding technology. The microstructure evolution, mechanical properties and fractured behaviors of the joints were investigated. The gradient structure remarkably decreased the formation tendency of brittle phases within the joints compared with a single filler alloy and thus improved the joint strength effectively. The average room-temperature tensile strength of the Ti₃Al/In718 dissimilar joint reached 353 MPa, and the strength value at 873 K was 245 MPa. At the Ti–Ni–Nb/Ni–Cr–Nb interface, some Ni₃(Nb, Ti) + (Nb, Ti)Cr₂ and TiNi₃ phases were detected in the Ti–Ni–Nb matrix. It was believed that their presence decreased the room-temperature strength of the Ti–Ni–Nb alloy but improved its high-temperature strength.     

Improving the mechanical properties of Al2O3/Ni laminated composites by adding Ni particles in Al2O3 layers

The (Al₂O₃ + Ni) composite, (Al₂O₃ + Ni)/Ni and Al₂O₃/(Al₂O₃ + Ni)/Ni laminated materials were prepared by aqueous tape casting and hot pressing. Results indicated that the (Al₂O₃ + Ni) composite had higher strength and fracture toughness than those of pure Al₂O₃. The fracture toughness of (Al₂O₃ + Ni)/Ni and Al₂O₃/(Al₂O₃ + Ni)/Ni laminated materials was higher than not only those of pure Al₂O₃, but also those of Al₂O₃/Ni laminar with the same layer numbers and thickness ratio. It was found that the toughness of the Al₂O₃/(Al₂O₃ + Ni)/Ni laminated material with five layers and layer thickness ratio = 2 could reach 16.10 MPa m^1/2, which were about 4.6 times of pure Al₂O₃. The strength and toughness of the (Al₂O₃ + Ni)/Ni laminated material with three layers and layer thickness ratio = 2 could reach 417.41 MPa and 12.42 MPa m^1/2. It indicated the material had better mechanical property.     

Development of mixed conducting dense nickel/Ca-doped lanthanum zirconate cermet for gas separation application

La_1.95Ca_0.05Zr₂O_7-δ (LCZ) and Ni–LCZ cermet have been prepared by combustion synthesis and conventional solid state mixing methods respectively. Both the materials are sintered in air and controlled atmosphere (5% H₂ in Ar). The density obtained for the material sintered at 1400 °C in controlled atmosphere is found to be more than 99.5%. This sintering temperature (1400 °C) is considered to be much lower compared to the conventional sintering temperature. The corresponding total conductivity for such Ni–LCZ cermet materials is ～400 S/cm measured at 750 °C having 40 vol% of Ni and 60 vol% LCZ.     

Ti3AlC2陶瓷及其衍生物Ti3C2Tx增强的Ag基电接触材料

银基电触头在低压开关领域扮演重要角色。作为一种具有良好导电导热性能的新型二维碳化物材料,MXene家族典型代表材料(Ti₃C₂T_x)在多个领域显示出极大的应用潜力。Ti₃C₂T_x有望作为一种新型环保银基电触头增强相材料。本研究采用粉末冶金法制备了Ag/Ti₃C₂T_x复合材料,并对Ti₃C₂T_x和Ti₃AlC₂的物相和微观结构进行表征。同时研究了Ti₃C₂T_x增强Ag基复合材料的综合性能,包括电阻率、显微硬度、机械加工性能、抗拉强度和抗电弧侵蚀性能,并与Ti₃AlC₂增强Ag基复合材料进行了比较。Ag/Ti₃C₂T_x的电阻率(30×10 ^-3 μΩ·m)相对于Ag/Ti₃AlC₂(42×10 ^-3 μΩ·m)降低了29%。Ag/Ti₃C₂T_x硬度适中(64 HV),具有良好的可加工性,作为无毒电触头材料应用前景广阔。Ag/Ti₃C₂T_x复合材料导电性能的提高主要归因于Ti₃C₂T_x本身优异的金属性以及由Ti₃C₂T_x微观结构特征带来的可变形性。由于缺乏Al-Ag相互扩散,Ag/Ti₃C₂T_x复合材料的拉伸强度(32.77 MPa)明显低于Ag/Ti₃AlC₂复合材料(145.52 MPa)。正因为缺失Al层,Ag/Ti₃C₂T_x的抗电弧侵蚀性能也无法与Ag/Ti₃AlC₂相媲美。尽管Ag/Ti₃C₂T_x的抗电弧侵蚀性能有待进一步提高,但优异的导电性使其有望替代当下有毒的Ag/CdO电接触材料。该研究结果为开发新型环保电触头材料提供了新的探索方向。     

Mechanism of improved electromigration reliability using Fe-Ni UBM in wafer level package

Fe-Ni films with compositions of 73 wt% of Ni and 45 wt% of Ni were used as under bump metallization (UBM) in wafer level chip scale package, and their reliability was evaluated through electromigration (EM) test compared with commercial Cu UBM. For Sn3.8Ag0.7Cu(SAC)/Cu solder joints, voids had initiated at Cu cathode after 300 h and typical failures of depletion of Cu cathode and cracks were detected after 1000 h EM. While the SAC/Fe-Ni solder joints kept at a perfect condition without any failures after 1000 h EM. Moreover, the characteristic lifetime calculated by Weibull analysis for Fe-73Ni UBM (2121 h), Fe-45Ni UBM (2340 h) were both over three folds to Cu UBM’s (698 h). The failure modes for Fe-Ni solder joints varied with the different growth behavior of intermetallic compounds (IMCs), which can all be classified as the crack at the cathodic interface between solder and outer IMC layer. The atomic fluxes concerned cathode dissolution and crack initiation were analyzed. When Fe-Ni UBM was added, cathode dissolution was suppressed due to the low diffusivity of IMCs and opposite transferring direction to electron flow of Fe atoms. The smaller EM flux within solder material led a smaller vacancy flux in Fe-Ni solder joints, which can explain the delay of solder voids and cracks as well as the much longer lifetime under EM.     

Corrosion investigation of the inlet section of REAC pipes in the refinery

The corrosion failure causes of the inlet section of reactor effluent air cooler (REAC) in the refinery was investigated by using Aspen software, HTRI Xchanger Suite simulator (HTRI), Computational Fluid Dynamics (CFD) technology and erosion corrosion experiments. The result shows that the severe erosion corrosion failure mainly occurs in the first row of REAC pipelines, and the field with localized corrosion is mainly distributed in a range of 5.8 m away from the inlet of air coolers and reveals an inhomogeneous thinning. At the REAC inlet, the NH₄HS concentration is about 12 wt% (> 10 wt%), the shear stress is high and oil phase is not appeared, thus the corrosion failure easily occurs at the inlet region. Meanwhile, the liquid phase fraction is larger at the bottom of the pipeline, forming corrosive solution and resulting in serious thinning. In the second and third passes, water and oil phase flow increases, i.e., both the NH₄HS concentration and the shear stress greatly decrease. In addition, the water in oil emulsion can segregate the contact between the tube wall and the corrosive medium. Therefore, beyond the range of corrosion failure region and in the second/third passes, the risk of erosion corrosion is markedly reduced.     

Cavitation erosion resistance of heat-treated NiTi

NiTi (Ti–50.8 at.% Ni) specimens were solution-treated at 1000 °C, followed by aging between 200 and 600 °C. The cavitation erosion resistance of all the aged specimens in deionized water was improved relative to the solution-treated specimen, with a maximum increase of about 8.7 times, which was achieved by aging at 500 °C. The results also indicate that both austenite and martensite contribute to the high cavitation erosion resistance of NiTi. It is also shown that a simple macro-indentation test employing a Rockwell indenter may be used for preliminary screening of heat-treated NiTi with respect to cavitation erosion resistance.     

Fabrication of Ag nanoparticles-coated macroporous SiO2 structure by using polystyrene spheres

Ag nanoparticles-coated macroporous SiO₂ structure was fabricated by a novel approach in which at first Ag nanoparticles were coated onto polystyrene (PS) spheres without a surfactant, then these Ag nanoparticles-coated PS beads (Ag/PS) were self-assembled by sedimentation-aggregation with tetraethyl orthosilicate (TEOS), and finally Ag nanoparticles-coated macroporous silica (Ag/SiO₂) was obtained after removal of the PS cores. The heat-treatment temperature and the gelation time were investigated to optimize the microstructural morphology, thermal decomposition of organic materials, matrix wall thickness and densification behavior. The three dimensionally assembled Ag/SiO₂ had 200 nm uniform macropores and a high specific surface area of 142 m² g⁻¹. The XRD, FE-SEM, EDX, BET and optical absorbance analysis indicated that the exactly three-dimensional structure of the template had been imprinted in the final samples and the walls of the macroporous SiO₂ were coated uniformly with Ag nanoparticles.