纳米级ITO粉体对烧结法制备靶材的影响

采用化学共沉淀法制备ITO前驱物,分别于600及1000℃下热处理前驱物,得到两种ITO粉体.粉体模压成型得到素坯,在400～1550℃内采用烧结法、氧气氛下烧结素坯制备出ITO靶材.对粉体及靶材进行表征和分析,研究了烧结过程中晶粒生长情况、靶材微结构与温度之间关系及靶材的失氧现象.得出600℃粉体为单相ITO固溶体、粒径为15 nm,1000℃粉体有少量SnO2析出、粒径为28 nm且其分散性和晶化程度优于600℃的粉体.两种粉体烧结制备靶材过程符合Coble固相烧结理论,1550℃时晶体出现类似二维成核生长方式的生长台阶.靶材密度随温度升高而增加,1550℃时随保温时间延长而增加.靶材致密化过程由团聚程度及团聚体大小决定,1000℃粉体制备的靶材密度高于600℃粉体所制靶材.两类靶材含氧量均低于理论值,1000℃粉体所制靶材含氧量高于600℃的含氧量.     

升温速率对烧结ITO靶材密度和组织的影响

采用化学共沉淀法制备ITO粉体前驱物,在600℃煅烧粉体前驱物4h,得到粒径为20~30nm的ITO粉体。添加1%的聚乙烯醇(PVA)造粒,模压成型制备ITO靶材素坯,设置不同的升温速率,在1550℃氧气氛下烧结素坯,得到ITO靶材。研究了烧结过程升温速率对ITO靶材密度和微观组织的影响。结果表明,在低温阶段(0~500℃)升温速率为3℃/min,高温阶段(500~1550℃)升温速率为8℃/min时,ITO靶材相对密度为99.58%,孔洞极少,近乎完全致密,且靶材宏观上无裂纹。     

纳米针状ITO的FESEM与TEM研究

采用近水沸点沉淀和煅烧工艺制备了纳米针状ITO粉末并采用场发射扫描电镜、透射电镜和X射线衍射等手段对ITO粉末进行表征.分析结果表明ITO前驱体纳米针的直径大体上分布在20 nm～100 nm之间,其长径比主要分布在3～8之间;ITO纳米针的直径主要分布在20 nm～60 nm之间,而其长径比则分布在4～12之间.ITO前驱体针是由相当细长的直径为3 nm～4 nm的纳米丝组成的,且这些纳米丝非常规整的排列成平行于ITO前驱体纳米针的轴向,而ITO纳米针却是由其平坦面垂直于针的轴向的薄片状亚单元组成的.ITO前驱体针是由In(OH)3和Sn3O2(OH)2组成的,且ITO前驱体针中的纳米丝是沿In(OH)3的[100]晶向择优取向生长.     

Co/Al2O3金属陶瓷材料的制备及热性能

采用共沉淀法制备了Co/Al2O3复合粉体的前驱体,经过煅烧、原位选择还原得到平均粒径为20 nm～30 nm尺寸可控、分布均匀的Co/Al2O3纳米多相复合粉体.最后复合粉体在Ar气氛保护下,1250℃～1550℃,30 MPa保温1 h烧结得到Co/Al2O3陶瓷基复合材料.试验过程中用到的测试与表征手段有TG-DSC,XRD,TEM等,用激光微扰法(laser flash)测量样品的热扩散系数,从而计算得到复合材料的热导率,其最大值接近理论值45.29 W/m.K.金属Co的添加有效的提高了Al2O3基陶瓷材料的导热性能.     

液相共沉淀法制备纳米ITO粉体

采用化学共沉淀法,以InCl3?5H2O和SnCl4?5H2O为原料,在掺杂浓度In2O3与SnO2的质量比为9:1的条件下,合成了平均粒径80nm的ITO粉体。利用TEM,XRD,DSC-TG,IR,ζ电位分析仪等实验方法对粉体的形貌、物相、结构等进行了表征。实验结果表明,当前驱体煅烧温度为600℃时,可以获得晶化良好的立方In2O3结构的In2O3和SnO2固溶体。根据ζ电位测定和TEM的观察结果,当反应的最终pH值为9时,粉体的分散性较好。     

尿素均相沉淀法制备纳米粉体Ce0.8Sm0.2O1.9的烧结性能

以尿素为沉淀剂,Sm2O3和Ce(NO3)3.6H2O为起始原料,采用均相沉淀法制备Sm3+掺杂CeO2基纳米固溶体Ce0.8Sm0.2O1.9(SDC)。利用TG-DTA、XRD、SEM和BET等手段对前驱体的热分解行为和SDC粉体的性能进行表征,研究焙烧温度对SDC粉体粒径和烧结性能的影响。结果表明:随焙烧温度的升高,晶粒尺寸逐渐增大;700℃焙烧的前驱体是具有良好结晶性能的类球形萤石型结构固溶体,晶粒尺寸为15 nm,粒子间仅有较弱的软团聚;该粉体具有较好的成型和烧结性能,将素坯在1 400℃保温2 h,得到相对密度高于95%、平均粒径约为0.6μm的固体电解质陶瓷体。     

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%.     

纳米SrCe0.95Y0.05O3-x陶瓷粉的制备与烧结

采用基于Pechini法的低温燃烧工艺制备了SrCe0.95Y0.05O3-x(SCY)前驱物.前驱物在900℃经0.5 h的煅烧处理即可得到纯的粒度在7～25 nm范围内的SrCe0.95Y0.05O3-x固体电解质纳米粉.将煅烧的粉体在18 MPa压力下压成片状的素坯,在900～1 500℃的温度范围内于空气中烧结索坯10 h.用X射线衍射(XRD)表征煅烧粉体的晶体结构,用扫描电镜(SEM)和透射电镜(TEM)表征了煅烧粉体和烧结体的形貌和粒度,采用阿基米德法测量了烧结体的密度.结果表明:温度达到1 000℃时,烧结体的径向收缩率和密度随着温度的升高而显著增加;温度达1 300℃时烧结体的径向收缩率和密度趋于恒定,得到相对密度高于96%、平均粒径约为3.68 μm的SrCe095Y0.05O3-x固体电解质陶瓷体.     

利用Ca（NO3）2-P2O5乙醇溶液体系制备纳米羟基磷灰石

使用Ca（NO3）2-P2O5乙醇溶液体系制备纳米羟基磷灰石，研究了在该体系中水浴温度、煅烧温度、陈化时间等因素对粉体的相成分，粒度和结晶度的影响。结果表明：水浴温度低，合成的粉体粒度小（约20nm），颗粒均匀且具有良好的分散性，但是结晶度较低；陈化后导致粉体粒度变大，结晶度增加；随着煅烧温度的升高，粉体的结晶度增加，600℃时可以得到结晶高的单一的羟基磷灰石粉体。在800℃煅烧时，羟基磷灰石发生部分分解。     

氧化钇稳定立方晶型氧化锆增强钨基合金制备工艺及性能北大核心CSCD

采用共沸蒸馏法结合粉末冶金法制备了氧化钇稳定立方晶型氧化锆增强钨基合金（W-3.0 mass%YSCZ）。利用XRD、SEM、EDS、TEM等检测手段对合金制备过程中不同阶段材料组织、形貌及微观结构进行了分析与表征,测定了复合钨粉的粒度、钨合金的密度、显微硬度、磨损性能及动态压缩性能。结果表明：p H值对前驱体粉体的粒度有显著影响,p H=2的初始溶液制得的前驱体粉体粒径细小,随着初始溶液的p H值增大,复合粉末粒径逐渐增加;p H=2的初始溶液制得的前驱体粉经550℃×4 h煅烧后得到粒径为40～60 nm煅烧粉体,再经750℃×2 h＋900℃×4 h氢气还原后得到尺寸为35～50 nm的钨与ZrO_2-Y2O3构成的近球形纳米级复合粉末;制得的钨合金中的ZrO_2为立方晶型,表明常温下Y2O3对ZrO_2晶型起到了稳定作用;ZrO_2-Y_2O_3颗粒对钨晶粒具有明显的细化作用,获得的钨晶粒粒径为3～6μm;钨基合金相对密度达90.9%,抗压强度达到1009 MPa,耐磨性较纯钨提高了约18.7%。     

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。