溶胶凝胶自燃合成MgAl2O4超细粉体

以Mg(NO3)2·6H2O和Al(NO3)3·9H2O为原料,分别采用尿素和柠檬酸为燃料,NH4NO3为燃烧助剂,用溶胶凝胶自燃合成(Sol-gel Auto ignition Synthesis,SAS)法制备MgAl2O4超细粉体(平均粒径20 nm～30 nm).2个体系在300℃～600℃之间发生燃烧反应,经煅烧后得到白色疏松的单相MgAl2O4粉体.利用BET、XRD、TEM等各种分析技术对尿素和硝酸盐及柠檬酸和硝酸盐形成的2种溶胶凝胶体系燃烧合成的粉体进行了研究,并与固相反应获得的粉体进行了比较.考察了点火温度、保温时间等对最终产物的影响.     

Pb(Zr_(0.95)Ti_(0.05))O_3纳米粉的合成及其钙钛矿结构的稳定性（英文）

采用溶胶-凝胶技术合成了Pb(Zr_(0.95)Ti_(0.05))O_3纳米粉,并探讨了煅烧温度对PZT(95/5)钙钛矿相结构稳定性的影响。据TGA-DSC的实验结果,确定了干凝胶粉的煅烧温度范围为550~750℃。XRD实验结果表明,随着煅烧温度的升高,粉体主晶相的强度逐渐升高,杂质相的峰高逐渐减弱直至消失。当在750℃煅烧时,粉体结构为单一的钙钛矿相。利用SEM观察发现,随着煅烧温度的升高,所合成的粉体粒度逐渐变小、均匀。当在750℃煅烧时,单一钙钛矿结构的粉体的平均粒度为100 nm。     

Pb(Zr0.95Ti0.05)O3纳米粉的制备及其钙钛矿结构的稳定性

论文采用溶胶-凝胶技术合成了Pb（Zr0.95Ti0.05）O3纳米粉,并探讨了煅烧温度对PZT(95/5)钙钛矿相结构稳定性的影响。据TGA-DSC的实验结果,确定了干凝胶粉的煅烧温度范围为550℃-750℃。XRD实验结果表明,随着煅烧温度的升高,粉体主晶相的强度逐渐升高,杂质相的峰高逐渐减弱直至消失。当在750℃煅烧时,粉体结构为单一的钙钛矿相。利用SEM观察发现,随着煅烧温度的升高,所合成的粉体的尺寸逐渐变小、均匀。当在750℃煅烧时,单一钙钛矿结构的粉体的平均粒径尺寸为100 nm。     

柠檬酸盐溶胶凝胶法低温合成KBT粉体

以Ti Cl4、Bi(NO3)3和K2CO3为原料采用柠檬酸盐溶胶-凝胶法低温烧结制备了纳米钛酸铋钾(KBT)粉体。利用DSCTG、XRD、SEM、TEM分别对KBT粉体的形成过程、物相结构及晶粒尺寸进行表征。研究并讨论了Ti Cl4浓度、煅烧温度、柠檬酸盐量等对KBT粉体结构的影响。结果表明,TiCl4浓度为1.5 mol/L时,700℃煅烧2 h合成了单相的片状K0.5Bi0.5TiO3纳米粉体,粉体颗粒边长大约在100~300 nm,厚度为20~50 nm;与固相法相比,烧结温度降低了300℃;与未添加柠檬酸盐的KBT相比,柠檬酸盐改性后的KBT粒子具有良好的分散性,且能有效抑制晶粒长大。     

液相合成铌酸钾粉体的研究

以Nb2O5、KECO3、HF和（NH4）2C2O4为原料，以柠檬酸为配位剂，乙二醇为酯化剂，用氨水调节溶液的pH值，首先将Nb2O5在水浴条件下溶于HF，加入（NH4）2C2O4和氨水获得沉淀物，而后用柠檬酸溶解获得Nb-柠檬酸溶液。K2CO3与Nb-柠檬酸溶液在乙二醇的交联作用下形成了K-Nb凝胶前驱体。用XRD和SEM研究了不同pH值、不同柠檬酸与金属离子的摩尔比条件下所形成的凝胶前驱体在不同温度下煅烧所得粉体的相组成和形貌。研究发现当柠檬酸与金属离子的摩尔比为3：1，柠檬酸和乙二醇的摩尔比为1：2时，可形成稳定的K-Nb前驱体溶液和凝胶。分析结果表明，K-Nb凝胶前驱体在加热过程中分解成K2CO3相，K2CO3与Nb-柠檬酸溶液发生反应生成KNbO3凝胶，凝胶经800℃煅烧3h或160℃水热反应8h可以制备出颗粒分布均匀的纯钙钛矿型KNbO3粉体。IR谱表明。800℃煅烧或160℃水热反应都出现了Nb-O的特征峰。     

EDTA络合溶胶-凝胶法合成YAG:Ce黄色荧光粉及其性能

以金属硝酸盐为原料,乙二胺四乙酸(EDTA)为络合剂,采用溶胶-凝胶法制备YAG:Ce黄色荧光粉,利用X射线衍射仪、扫描电镜、荧光分光光度计等检测方法研究制备过程工艺参数对粉体结构、形貌和发光性能的影响。结果表明:EDTA络合所得的凝胶经1000℃煅烧就得到纯的钇铝石榴石相(YAG),其晶相转变温度比柠檬酸(CA)络合剂溶胶-凝胶法的降低约200℃,且所得YAG:Ce荧光粉的发光强度随着煅烧温度升高而增大;凝胶经1500℃高温煅烧所得荧光粉的发光强度比柠檬酸(CA)络合剂的提高66.2%,这是由粉体结晶度好、颗粒形貌更规整、呈球形且尺寸更加均匀所致;在原料液中添加Na2SO4-K2SO4复合熔盐后,凝胶经1500℃煅烧后所得荧光粉发光强度比采用非熔盐法所得荧光粉的增大约10%。     

不同溶胶组成对BaLa0．3Fe11．7O19纳米粉末生成过程的影响

利用溶胶-凝胶自燃烧高温合成法制备了稀土La掺杂钡铁氧体BaLa0.3Fe11.7O19纳米粉末.用X射线衍射仪、振动样品磁强计和透射电镜对不同溶胶组成下合成的粉末的结构、磁学性能、粒度及形貌进行了研究.试验表明用氨水调节溶液起始pH值以及加入适量的柠檬酸和乙二醇是合成结构纯净、性能优异的BaLa0.3Fe11.7O19纳米粉末的2个关键步骤.在溶液起始pH值呈弱酸性(7.0左右)、柠檬酸/硝酸盐=3、煅烧温度为850℃,保温1 h的条件下,利用溶胶-凝胶自燃烧高温合成法可以制备出粒径为36nm的磁铅石结构的BaLa0.3Fe11.7O19粉末,其磁学性能优异,比饱和磁化强度可达65.54 A·m2/kg,矫顽力可达433 kA/m.     

结晶析出法制备YAG超细粉

研究了结晶析出法制备YAG超细粉的工艺,采用铝和钇的硝酸盐或硫酸盐混合溶液为原料,蒸发去水获得硝酸盐或硫酸盐的混晶体.结果表明:硝酸盐混晶体经1 100℃煅烧可获得YAG粉体,加入Y2O3籽晶可使YAG相形成温度下降约100℃;硫酸盐混晶体经1 300℃煅烧2 h后也可获得YAG粉体;硝酸盐混晶体煅烧得到的YAG粉体团聚严重,烧结体最大相对密度仅为74.3%;硫酸盐混晶体煅烧得到的YAG粉体团聚较少,粉体平均粒径约为300 nm,烧结体密度为95.2%.     

两步无机盐-凝胶法制备PMN-PT弛豫铁电陶瓷粉体

0．65Pb（Mg1／3Nb2／3）O3—0．35PbTiO3（简称：PMN-PT）弛豫铁电粉体采用两步无机盐-凝胶法制备。以氧化镁，醋酸铅，钛酸丁脂为原料，柠檬酸为螫合剂，乙二醇为溶剂，分别合成稳定的Mg，Pb-Ti的有机化合物先驱体溶液。Nb2O5粉体与Mg先驱体溶液均匀混合，并采用溶胶-凝胶工艺制备MgNb2O6（MN）先驱体粉体；MN粉体与Pb-Ti先驱体溶液均匀混合，并制备PMN-PT粉体。通过XRD和SEM分析PMN-PT钙钛矿相形成的影响因素和微观形貌，研究全钙钛矿相PMN-PT铁电粉体的制备。结果表明：过量3％MgO前驱体经1050℃，4h煅烧可以得到纯相MgNb2O6先驱体粉体：过量5％PbO前驱体经900℃，4h煅烧可以得到全钙钛矿相PMN-PT粉体。     

Sm2O3和Nd2O3共同掺杂CeO2基电解质材料的研究

采用柠檬酸-硝酸盐法合成出单一相、均匀的Ce0.8SmxNd0.2-xO1.9粉体,XRD结果表明该粉体为单相萤石结构,粒径约在11.7 nm～20.1 nm之间.将粉体干压成型,在1400 ℃下无压烧结5 h可得到高致密度陶瓷.SEM照片显示陶瓷微观结构均匀,晶粒尺寸在2 μm～4 μm.经直流四端电极法测试得到该样品在500 ℃时电导率约在0.012 S/cm.该结果说明与单项掺杂相比,两相共掺杂会进一步提高材料的电导率.     

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。