用碘化钾滴定金基和钯基合金中的银

研究了在氨性介质中以碘化钾为滴定剂使用各种指示电极检测终点电位滴定银,讨论外来离子的干扰影响.提出以Ag—AgI指示电极(vs、SCE)、不经分离直接测定银的方法.方法适用于Au—Ag—Cu、Au—Ag—Cu—Gd、Pd—Ag、Pd—Ag—Cu—Au—Pt—Zn等合金中银的分析.     

电位滴定法测定银、铜、镍、锰合金中的锰

建立了高锰酸钾电位滴定测定锰的方法,研究了不同合金中测定锰的条件.结果表明:在焦磷酸钠介质中,采用Pt指示电极和Ag参比电极指示滴定终点,用KMnO_4溶液滴定Mn(Ⅱ)为Mn(Ⅲ),测定6.00～30.00 mg Mn,相对误差≤±0.33%,加标准回收率在99.60%～100.40%.方法准确度高,重现性和选择性好,操作简便,终点敏锐,已应用于锰质量分数为7%～98%的银、铜、镍、锰等合金中锰的测定,结果满意.     

硫脲和尿素在银电极上吸附行为的电化学和SERS研究

利用表面增强拉曼光谱(SERS)和极化曲线的方法研究了硫脲和尿素在H2SO4溶液中银电极上的吸附行为.结果表明:硫脲参与了银的阳极溶解反应.尿素在银电极表面上发生了缩合反应,产物为缩二脲,缩二脲以质子化的形式物理吸附在银表面上     

火焰原子吸收光谱法测定载银沸石中银

研究了载银沸石中银含量的火焰原子吸收光谱测定方法.样品在低温下用硝酸溶解,试液过滤后直接用火焰原子吸收方法进行测定.实验结果表明:大量沸石对银的测定产生干扰,可通过配制沸石基质标准工作溶液消除干扰.在最佳实验条件下,银的质量浓度在0.40～15.00 g/ml与10.00～100.00g/ml范围内分别符合比尔定律,检出限为0.11g/ml,样品加标回收率为97%～103%.该方法可用于载银沸石中银含量的测定.     

银锗合金的元素分析

为准确测定银锗合金中银和锗的含量,选择了滴定法和ICP - AES光谱法.得出以下结论:①采用常规的伏尔哈特法和电位滴定法测定银含量,锗元素不会产生干扰.2种方法均可用于日常检测,电位滴定法更适宜用于仲裁检验和监督抽查;②ICP - AES光谱法测定银合金中银含量的常规方法是先将样品用稀硝酸溶解后加盐酸沉淀银,再分析滤液中的其它金属杂质元素.使用含C1-试剂溶解银锗合金时,当温度≥86℃会引起GeCl4的挥发,对分析锗含量的影响较大,采用此法须严格控制温度;③尝试了用滴定后的溶液过滤定容后再测定锗含量.实际样品测试结果与其他元素含量分析结果的元素总合量趋于100％,由此表明测试滴定的滤液所得检测结果准确,选用该方法操作简单,结果更为理想.     

银电极组成对负温度系数热敏电阻电性能的影响

本工作通过研究含铅的银电极与无铅的银电极对负温度系数(NTC)热敏电阻电性能、结构的影响,探讨了含铅银电极中铅组分对NTC热敏电阻性能的影响机理.实验结果表明:含铅银电极的热敏电阻与无铅银电极的热敏电阻相比,在电性能上,阻值离散性较小,老化可靠性较好;在结构上,含铅的银电极与NTC陶瓷界面处扩散反应程度更大,银电极能够和NTC瓷体很好地结合.分析认为电极/陶瓷界面的结构质量是影响NTC热敏电阻阻值的离散性和老化可靠性的重要原因.在研究基础上,对NTC热敏电阻用高性能、无铅银电极浆料研制的工作方向进行了探讨.     

过硫酸钾氧化胭脂红催化光度法测定痕量银

基于α,α’-联吡啶作活化剂、过硫酸钾氧化胭脂红、Ag(I)的催化效应,拟定了催化光度法测定痕量银的新方法。本法的检出限为8×10~(-11)g/ml,线性范围为2.0×10~(-4)～2.4×10~(-2)μg/ml,可用于铅中银的测定。     

碘离子作库仑滴定剂的研究—银的滴定

详细研究了 Ag-AgI 膜电极阴极发生碘离子的电流效率同制备电极的各种条件和滴定介质之间的关系,根据膜的表面性质解释了产生系统滴定误差的原因并找到了获得电生碘离子100%或接近100%电流效率的最佳条件。应用电极产生的碘离子滴定了不同物料中的少量银,并研究了指示终点的各种方法。方法简便,测定银的准确度高,大量共存离子不干扰或能借 EDTA 掩蔽而消除其干扰。     

基于银氧化物电极的高比能电池研究进展

基于银氧化物电极(银电极)的高比能电池具有比能量大、输出功率高、放电平稳、安全可靠等优点;银电极作为此类电池的关键部件,决定着电池性能的优劣。简要介绍了银电极的工作原理和制备方法;详细分析了银电极中AgO分解、两坪阶电位、活性物质利用率和高倍率放电性能等研究现状;综述了锌银、铝银和锂银等几类基于银电极的高比能电池的原理与特点、发展与应用、性能与改进方法等;对基于银电极的高比能电池的发展方向进行展望。     

原料配比对银/卤化银参比电极性能的影响

使用热浸涂方法制备了不同AgCl/AgBr配比的银/卤化银(Ag/AgX)参比电极.通过SEM观察,不同含量的Ag/AgX电极表面形貌差别不大.XRD分析表明,各配比的AgX为角银矿晶型.电极的电位稳定性、耐极化性能以及内阻测试表明,原料配比对电极性能有影响.随着AgBr含量的减少Ag/AgX电极的内阻与极化电阻减小,在AgCl/AgBr为77/23时电极的电位稳定性与耐极化性能较好.Ag/AgX参比电极在海水中的电位漂移较小.     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

Thermodynamics Study on the Decomposition of Chromite with KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

Influence of Heat Treatment on Damping Behaviour of the Magnesium Wrought Alloy AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Quantitative Analysis of the Crystallographic Orientation Relationship Between the Martensite and Austenite in Quenching–Partitioning–Tempering Steels

The orientation relationships(ORs)between the martensite and the retained austenite in low-and medium-carbon steels after quenching–partitioning–tempering process were studied in this work.The ORs in the studied steels are identified by selected-area electron diffraction(SAED)as either K–S or N–W ORs.Meanwhile,the ORs were also studied based on numerical fitting of electron backscatter diffraction data method suggested by Miyamoto.The simulated K–S and N–W ORs in the low-index directions generally do not well coincide with the experimental pole figure,which may be attributed to both the orientation spread from the ideal variant orientations and high symmetry of the low-index directions.However,the simulated results coincide well with experimental pole figures in the high-index directions{123}_(bcc).A modified method with simplicity based on Miyamoto’s work was proposed.The results indicate that the ORs determined by modified method are similar to those determined by Miyamoto’method,that is,the OR is near K–S OR for the low-carbon Q–P–T steel,and with the increase of carbon content,the OR is closer to N–W OR in medium-carbon Q–P–T steel.     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.     

电化学噪声数据处理方法概述

综述了常见的电化学噪声数据处理方法,介绍了直流趋势剔除、统计分析、快速傅立叶变换(FFT)法计算功率谱密度(PSD)以及小波变换处理电化学噪声信号的基本过程,并阐释了各种数学处理及所得参数的物理意义。