多孔钛/TiO2纳米管复合薄膜制备及其电化学性能

目的 制备高比容量多孔钛/TiO2纳米管三维自支撑一体化复合电极材料。方法 采用非溶剂致相分离法与高温烧结相结合的方法制备出孔径小、空间利用率高的三维多孔钛平板膜,然后经阳极氧化法在其表面生长TiO2纳米管,从而制备出多孔钛/TiO2纳米管复合薄膜电极。结果 以3 μm粒径钛粉为原料,N-甲基-2-吡咯烷酮、聚乙烯吡咯烷酮、聚丙烯腈为添加剂制备钛膜生坯,经刮膜成型后,在氩气保护下经1000 ℃烧结,得到孔径约为2～6 μm的多孔钛平板膜。采用阳极氧化法在多孔钛平板膜上直接生长TiO2纳米管,制得多孔钛/TiO2纳米管复合薄膜电极。该复合薄膜电极在超级电容器中具有良好的电化学性能,其在2 mA/cm2电流密度下,比电容为385.34 mF/cm2,即使电流密度增加到10 mA/cm2,比电容仍能保持在125.14 mF/cm2。结论 相较于TiO2纳米颗粒,采用此方法制备的多孔钛/TiO2纳米管复合薄膜电极具有良好的电化学性能,可为下一代储能器件提供新的思路。     

TiO_2纳米管阵列的制备及其光催化产氢活性研究

采用阳极氧化法在乙二醇电解液中制备了高度有序的TiO2纳米管阵列,分别通过SEM、EDX表征其形貌及元素组成,并探讨了TiO2纳米管的生长过程。结果表明,TiO2纳米管的形成过程是一个由纳米多孔膜结构向独立有序的纳米管阵列转变的过程。同时以TiO2纳米管为光阳极,采用双室光电化学池制氢体系,利用光照TiO2产生的光电压与双室电解液pH差产生的化学偏压的协同效应可达到水的分解电压,充分实现高效率、低能耗制氢的目标。无外加电压及牺牲剂条件下,TiO2纳米管的光电流密度为6.51 m A/cm2,光照1 h产氢量高达108.9μmol/cm2。     

TiO2纳米管薄膜的屈曲图样（英文）

采用基体应变测试方法研究TiO2纳米管薄膜的屈曲图样。结果表明：TiO2纳米管薄膜室温样、250℃退火样和 400℃退火样的屈曲应变依次为2.5%、8.9%和7.8%,说明退火改善了纳米管薄膜/Ti 基体界面状况。从 SEM 观察可以看出,TiO2纳米管薄膜室温样、250℃退火样和400℃退火样的临界屈曲应力分别为180.4、410.2 和 619.5MPa;从 AFM 观察可以看出,TiO2纳米管薄膜 250℃退火样的临界屈曲应力为470.2MPa,两者吻合得很好。采用AFM计算250℃退火样的真实应力和能量释放率分别为840.3MPa和77.2J/m2,此结果与从裂纹角度计算出的250℃退火样的能量释放率102.6 J/m2吻合得很好。     

TiO_2纳米管薄膜的屈曲图样(英文)

采用基体应变测试方法研究TiO2纳米管薄膜的屈曲图样。结果表明:TiO2纳米管薄膜室温样、250℃退火样和 400℃退火样的屈曲应变依次为2.5%、8.9%和7.8%,说明退火改善了纳米管薄膜/Ti 基体界面状况。从 SEM 观察可以看出,TiO2纳米管薄膜室温样、250℃退火样和400℃退火样的临界屈曲应力分别为180.4、410.2 和 619.5MPa;从 AFM 观察可以看出,TiO2纳米管薄膜 250℃退火样的临界屈曲应力为470.2MPa,两者吻合得很好。采用AFM计算250℃退火样的真实应力和能量释放率分别为840.3MPa和77.2J/m2,此结果与从裂纹角度计算出的250℃退火样的能量释放率102.6 J/m2吻合得很好。     

TiO_2纳米管薄膜的裂纹起源、扩展与饱和(英文)

通过阳极氧化法在Ti基体上垂直定向生长TiO2纳米管,其直径为60-80nm,长度为4μm。采用基体应变测试方法研究TiO2纳米管薄膜裂纹起源、扩展与饱和的情况。结果表明:退火可明显改善TiO2纳米管薄膜/Ti基体界面状况;随着拉伸应变的增加,裂纹扩展迅速加快,在很小的应变范围内达到饱和;TiO2纳米管薄膜室温样、250℃退火样和400℃退火样的界面剪切强度估算值分别为163.3、370.2和684.5MPa,临界能量释放率分别为49.6、102.6和392.7J/m2,断裂韧性分别为0.996、1.433和2.803MPa.m1/2。TiO2纳米管薄膜的界面结合机制为化学键结合。     

氧化钛纳米管阵列的表面聚集控制及光电化学特性

采用阳极氧化法在有机介质中制备垂直排列的厚度达百微米的TiO2纳米管阵列,重点考察TiO2纳米管表面形貌特性的控制,以期从微观修饰角度来提高TiO2纳米管阵列膜的光电化学性能;在此基础上,考察不同处理条件下的TiO2纳米管阵列膜的光电化学特性。实验结果表明:采用无水乙醇作为超声液并结合二次蒸馏水进行漂洗能彻底清除纳米管表面聚集堵塞部分,得到清洁、规整有序的纳米管阵列表面,且不破坏纳米管阵列膜的最佳超声振动时间为20～30s。在对纳米管阵列的表面形貌特性进行控制后,采用一步阳极氧化法+无水乙醇超声制备的样品经500℃退火在全谱段的光转换效率达到1.48%,证实对纳米管阵列的表面形貌特性实施控制能有效提高其光电化学性能。     

阳极氧化法制备Zr-17Nb合金表面氧化物纳米管阵列及其性能研究

利用电化学阳极氧化技术,在含有丙三醇、0.35 mol/L NH4F和5%H2O (体积分数)的溶液中,在Zr-17Nb合金表面制备了高度有序的氧化物纳米管阵列。使用XRD、SEM、HRTEM、EDS和XPS对纳米管阵列的结构、形貌和成分进行了详细研究。结果表明,在恒定外加电压70 V的条件下,阳极氧化过程中Zr和Nb的氧化溶解速率保持一致。450℃退火处理后,纳米管膜层由无定型态转化为晶态,由正交相ZrO2和正交相锆铌氧化物(Nb2Zr6O17)组成。退火处理后,纳米管膜层弹性模量降低,硬度提高。同时,纳米管阵列表面水接触角减小,呈现更好的亲水性。     

非晶TiO2 纳米管形貌对其作为超级电容器电化学性能的影响

采用改进的两步电化学阳极氧化和电化学氢化法制备了不同管径、长度和壁厚的氢化无定型TiO₂纳米管阵列（H@am-TNAs）。结果表明,电化学氢化对TiO₂纳米管阵列的结构影响不大。经过电化学氢化后,纳米管在100 mV·s^-1时的比电容为4.05 mF·cm^-2,比未氢化的管长和管径相同的TiO₂纳米管的比电容大20倍。纳米管的比电容不仅与管长有关,还受管径的影响。通过指数函数拟合,纳米管的长径比呈线性关系。面积电容/长径比达到0.056,几乎相当于锐钛矿相TiO₂纳米管。阳极化处理后的纳米管具有最小的电荷转移阻力和最佳的离子扩散/输运动力学,具有最高的面积容量。此外,为了研究H@am-TNAs纳米管的电化学性能的润湿性,相同的H@am-TNAs电极在C-V和C-P测试前,在电解液中浸泡不同时间,结果表明,比电容随着浸泡时间的增加而减小。     

二氧化钛纳米管阵列电极的光电化学性能研究

采用阳极氧化法在钛片上制备了垂直排列的TiO2纳米管阵列，利用SEMXRD对纳米管阵列的形貌和结构进行了表征，并通过电化学交流阻抗谱、光照开路电位谱和瞬态光电流谱技术对纳米管阵列电极的光电化学特性进行了研究。实验结果表明，TiO2纳米管的内径约为90nm，管壁约为10nm，纳米管阵列厚度约为500nm，经600℃退火处理后，转变为锐钛矿型与金红石型的混晶结构。光电测试结果表明，随着退火温度升高，TiO2纳米管阵列电极的界面电荷转移电阻减小，光电流逐渐增大，光照开路电压增大，至600℃达到最大，当退火温度继续升高，电极的光电性能急剧下降。与TiO2纳米多孔膜电极相比，光电性能显著提高，这主要归因于TiO2纳米管阵列更大的孔隙率和比表面积。     

ZnO/TiO_2-纳米管光催化剂的制备与表征

采用改进的化学沉积法,用ZnO对TiO2-纳米管进行改性,制备ZnO/TiO2-纳米管的复合半导体材料。用X射线衍射仪、透射电镜、高分辨透射电镜、X射线能谱仪、比表面分析仪,紫外-可见光度计等研究样品的结构、表面形貌和化学组成。通过光降解甲基橙模拟污染物考察其光催化性能,并探讨ZnO粒子表面修饰增强TiO2-纳米管光催化活性的机制。结果表明:n(Zn)-n(Ti)为1-4的ZnO/TiO2-纳米管复合材料具有最佳的光催化活性;Zn和Ti的协同效应改善了复合材料的可见光响应性。     

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).     

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.     

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.     

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。