纳米Ir／SPE电极的制备及其影响因素

首次选用镍作为中间催化剂,采用吸附还原成长法制备纳米Ir/SPE电极,并就镀浴温度和pH值、H2IrCl6浓度、NaBH4与H2IrCl6配比对电极制备的影响作了深入研究。研究表明:采用吸附还原成长法,以Ni作为中间催化剂,浓度为22mmol·L-1NaBH4与浓度为6mmol·L-1H2IrCl6的混合液作为镀浴,亦即NaBH4与H2IrCl6配比为3.6,pH值为8,镀浴温度为40℃,镀浴时间为24h的条件下,循环镀覆3次,可获得致密、均匀,具有良好电解性能的纳米级Ir/SPE电极。     

非晶对置换反应中Ag纳米晶生长的影响

研究在Zn、Cu置换AgNO3溶液反应中非晶膜的形成对纳米Ag晶体生长的影响.HRTEM的观察表明,置换反应中形成的纳米Ag晶体的生长前沿沉积有一层5～10 nm宽的非晶膜,纳米Ag晶体的长大取决于该非晶膜的自发晶化.非晶膜的自发晶化主要是在非晶层内原位成核、长大,也可在晶体和非晶的界面成核长大,还可观察到非晶层内的Ag原子直接排列到原晶体的界面上而不需要成核的过程.在纳米Ag晶体生长前沿沉积的非晶的稳定性取决于AgNO3溶液的浓度.在80 mmol·L-1或更低的AgNO3溶液中生成的Ag纳米晶的生长前沿沉积有较稳定的非晶膜,而在400 mmol·L-1的高浓度AgNO3溶液中Zn置换还原形成的纳米Ag晶体的生长前沿无非晶存在.     

Ag含量对钙钛矿型La-Ca-Co-O氧还原催化剂电催化特性的影响

为了提高钙钛矿型La-Ca-Co-O的氧还原催化性能,采用柠檬酸辅助的溶胶-凝胶法制备添加AgNO3的Lao0.4Ca0.6CoO3粉体.采用 XRD、SEM和EDAX分析手段研究凝胶在700℃焙烧后的产物,通过电位阶跃技术测定定不同Ag含量粉体的电化学有效表面积.通过线性扫描伏安法测定催化剂粉体催化氧还原反应的极化特性;通 过Tafel技术测定其催化氧还原反应的交换电流密度.采用粉末压片和直流电路测定催化剂的表观电导率.结果表明:Ag+固溶入La0.4Ca0.6CoO3晶格导致晶格膨胀;添加AgNO3的粉体中还有单质Ag颗粒析出.在La0.4Ca0.6CoO3中引入Ag+可显著提高其对氧还原的电催化活性,在Ag含量为2%时,催化氧还原的交换电流密度达到最大值0.2988 A/m2;而La0.4Ca0.6CoO3的表观电导率随着Ag含量增加而增大.     

Ag/SiO2核-壳结构球的制备与光学性质

采用St(o)ber方法,以AgNO3与柠檬盐钠还原反应所制备出的Ag纳米颗粒为种子,合成了Ag/SiO2核-壳结构的亚微米球.用透射电镜(TEM)观测所得产物的形貌和大小,并用光吸收谱仪测试了Ag纳米颗粒的表面等离子体共振(SPR)引起的光吸收峰.     

核壳结构聚苯乙烯/银复合粒子的制备研究

采用化学镀法,将金属Ag粒子致密镀覆在自制聚苯乙烯微球表面,制备了具有高导电特性的PS/Ag复合粒子,通过正交实验优化了制备工艺.结果表明:表面粗化处理、AgNO3/PS质量比和NH3·H2O浓度3个因素对复合粒子的体积电阻率产生了重要影响;粗化处理在PS微球表面引入了磺酸基团,提高了PS微球表面的电负性和亲水性,对包...     

纳米SCR催化剂Ce-V/TiO_2的制备与研究

采用溶胶-凝胶法和浸渍法制备选择性催化还原(SCR)脱硝反应复合纳米催化剂Ce-V/TiO_2,在不同的实验条件下制备出一系列的TiO_2凝胶用作催化剂载体.然后通过浸渍法依次负载CeO_2和V_2O_5于多孔TiO_2载体.用氨气作为还原性气体,对选择性催化还原NOx进行实验研究.在不同的TiO_2载体煅烧温度、CeO_2和V_2O_5负载量以及催化还原反应温度等条件下,对催化剂的表面结构和催化性能采用BET、XRD、SEM等手段进行表征分析.结果表明,纳米Ce-V/TiO_2固溶体复合催化剂以及对其制备工艺技术参数的优化可增大催化剂的比表面积和微孔体积,使催化剂的催化活性有很大的提高.此外,相当数量的多孔纳米TiO_2大大增加了光催化活性的有效面积,有利于增大与反应物的接触面积和提高光催化活性.当载体TiO_2 的煅烧温度和催化还原反应温度为500 ℃时,5%Ce-10%V/TiO_2催化剂反应的NO_x转化率可达96.2%.     

纳米Ni(OH)2/Ni-Ti-O 纳米管阵列复合电极的制备及其对甲醇的催化氧化性能

阳极氧化NiTi合金板获得了Ni-Ti-O 纳米管阵列（NTOs）,并将其加热至500℃在氢气气氛中还原处理2h。采用简单的溶盐浸渍法,将Ni(OH)2纳米颗粒负载在NTOs上制备Ni(OH)2/NTOs/NiTi复合电极。采用场发射扫描电子显微镜（FESEM）,X射线光电子能谱（XPS）和循环伏安法（CV）表征电极的表面形貌、电极表面的元素价态和其对甲醇氧化的电催化性能。研究了不同浸渍时间和Ni源浓度等工艺参数对电极微观形貌和电催化氧化性能的影响。结果表明：随着浸渍时间的延长和Ni源浓度的增加,电极上负载的催化纳米颗粒尺寸逐渐增大,氧化峰电流密度先增后降。在25oC时,将NTOs依次浸渍在0.2M NiCl2?6H2O乙醇溶液和0.2M NH4OH乙醇溶液中各12h后,可得到电催化性能良好的纳米Ni(OH)2/NTOs电极,氧化峰电流达到38.41 mA?cm-2。经1000次循环后,电极峰电流密度为原来的75%,表明纳米Ni(OH)2/NTOs电极有良好的循环稳定性,可成为有前景的DMFC的阳极电极候选材料。     

液相还原法制备纳米晶Ag-50Ni合金的研究

采用液相还原法,随后在620 ℃、58 MPa下经真空热压,制备了纳米晶Ag-50Ni块体合金,并通过X射线衍射(XRD)仪、扫描电镜(SEM/EDX)和透射电镜(TEM)研究了其显微组织结构.结果表明,Ag-Ni粉末的最佳合成工艺条件为:反应体系温度为70 ℃;还原剂水合肼(N2H4·H2O)浓度为2.5 mol.L-1;反应物AgNO3浓度为1.5 mol.L-1;反应物NiSO4的浓度为1.5 mol.L-1;反应体系pH值为8.Ag-Ni粉末平均粒度约为45 nm,黑色无定形形状.Ag-Ni粉末经真空热压后,晶粒尺寸有所长大,但仍保持纳米级尺度.合金致密度很高,由双相组成,显微组织均匀且无Ag网出现.     

纳米Ni(OH)_2/Ni-Ti-O纳米管阵列复合电极的制备及其对甲醇的电催化氧化性能

阳极氧化NiTi合金板获得了Ni-Ti-O纳米管阵列(NTOs),并将其在氢气气氛中加热至500℃还原处理2 h。采用简单的溶盐浸渍法,将Ni(OH)_2纳米颗粒负载在NTOs上制备Ni(OH)_2/NTOs/Ni Ti复合电极。采用场发射扫描电子显微镜(FESEM),X射线光电子能谱(XPS)和循环伏安法(CV)表征电极的表面形貌、电极表面的元素价态和其对甲醇氧化的电催化性能。研究了不同浸渍时间和Ni源浓度等工艺参数对电极微观形貌和电催化氧化性能的影响。结果表明:随着浸渍时间的延长和Ni源浓度的增加,电极上负载的催化纳米颗粒尺寸逐渐增大,氧化峰电流密度先升后降。在25℃时,将NTOs依次浸渍在0.2 mol/L NiCl_2·6H_2O乙醇溶液和0.2 mol/L NH_4OH乙醇溶液中各12 h后,可得到电催化性能良好的纳米Ni(OH)_2/NTOs电极,氧化峰电流密度达到38.41 m A·cm~(-2)。经1000次循环后,电极峰电流密度为原来的75.7%,表明纳米Ni(OH)_2/NTOs电极有良好的循环稳定性。     

金属多孔球形银粉的制备

采用化学还原沉积法,以水合联氨为还原剂,在分散剂和自制的有机混和溶剂的保护下,控制溶液中银离子浓度为10～40 g.L-1,分散剂的加入量1.5～3 g.L-1,有机混合制剂60 g.L-1,还原反应在瞬间完成,还原出粒度为纳米级的银颗粒,在可控的条件下纳米颗粒聚集为多孔团粒银粉,快速从溶液中沉淀分离.采用扫描电镜检测,多孔团粒球体的粒度为40～80 μm;采用比表面积及孔隙度检测仪测试比表面积可以达到16 m2/g以上,其孔道具有很高的通透性,不同于常规的超细银粉.     

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。