碳热还原协同溶胶-凝胶法合成纳米ZrB2粉末

利用ZrO2-B2O3-C反应体系碳热还原的基本原理,分别使用正丙醇锆（Zr（Oc3H7）4）、硼酸（H3BO3）和蔗糖（C12H22O11）为原料,采用溶胶-凝胶-碳热还原法合成了二硼化锆（ZrB2）纳米粉末。我们首先使用络合剂醋酸（AcOH）修饰Zr（OC3H7）4,以防止Zr（OC3H7）4的快速水解;其次,选用蔗糖作为碳源,是考虑到蔗糖热解时可以完全分解为碳,这样可以准确计算热解过程碳的生成量。此外,研究了凝胶温度对ZrB2纳米粉末形貌的影响。结果表明：当起始原料B／Zr（mol）=2．3、热解温度为1550℃时,通过碳热还原协同溶胶-凝胶法成功合成了单相ZrB2纳米粉末;当凝胶温度分别为65、75和85℃时,ZrB2纳米粉末形貌从球状演变为链状,最后生长为棒状,生长机理为定向吸附。     

凝胶-溶胶协同碳热还原法合成二硼化锆粉体及生长机制探究

以正丙醇锆(C12H28O4Zr)为锆源,硼酸(H3BO3)为硼源,山梨醇(GH14O6)为碳源,乙酸(C2H4O2)为溶剂,采用溶胶-凝胶协同碳热还原法制备了高纯超细硼化锆(ZrB2)粉体.分别研究了碳含量和硼含量对产物的物相和形貌的影响.通过X射线衍射仪、拉曼光谱仪、扫描电镜、透射电镜以及自带的X射线能谱仪对硼化锆...     

溶胶-凝胶法制备PZT纳米晶反应机理

以硝酸氧锆、钛酸四丁酯、醋酸铅为原料，乙二醇为溶剂，用溶胶—凝胶技术制备了钙铁矿型的锆钛酸铅(PZT)纳米晶。实验中发现前驱物间的聚合反应使硝酸氧锆能很好地溶于乙二醇。通过对原料、不同温度下的溶胶、干凝胶、PZT粉末的红外光谱分析，给出了溶胶、凝胶形成的机理，进一步证实溶胶—凝胶过程中通过前驱物的水解、缩聚反应形成金属元素与乙二醇相配位的链状或网状聚合物。原料中所含的NO3^—离子反应后形成的硝酸酯被包裹在溶胶和凝胶的聚合物网络中，CH3COO^—离子反应后生成醋酸酯并通过两个O与聚合物网络中的金属元素配位。     

纳米晶氮化铝粉料的制备

采用溶胶-凝胶工艺结合碳热氮化还原法进行纳米晶AlN粉末的制备和表征.以异丙醇铝((C3H7O)3Al)、蔗糖、尿素((NH2)2CO)为原料,通过控制硝酸和水的加入量,制备出透明的溶胶,经浓缩后得到透明的凝胶,干燥后得到分子水平混合的铝源和碳源的前驱体,经裂解、碳热氮化还原法制备出纳米晶AlN粉末.系统研究了C/Al比、添加尿素、碳热氮化还原反应的温度和时间等因素对合成粉料特性的影响,并进一步优化了制备工艺参数.采用XRD、BET等对合成产物的特性进行了分析和表征.通过原料组成、工艺参数的优化,制备出高纯纳米晶AlN粉末,其晶粒尺寸可达23 nm,除碳后比表面积可达70m2/g.     

溶胶凝胶燃烧法合成YAG纳米粉

以硝酸钇、硝酸铝为原料,采用溶胶-凝胶/燃烧合成结合法合成了钇铝石榴石(Y3Al5O12,YAG)超细微粉.用X射线衍射仪(D/Max-2550V型)及傅立叶红外光谱(FT-IR)确定前驱体和不同温度处理的粉末的相组成;借助于德国NETZSCH STA449C TG-MS热分析仪(升温速率为10℃/min)对前驱体粉末的热分解过程进行了研究,由JEM-200CX型透射电镜观察粉体的形貌.结果表明过多的柠檬酸和羧酸盐在400℃分解形成碳酸盐,在800℃YAG相开始逐渐形成,在900℃形成了结晶完全的YAG相,而没有中间相产生.经1000℃热处理获得了超细、分散良好、粒度为80nm左右的均匀粉体.     

不同锆源对聚丙烯酰胺凝胶法制备氧化锆纳米粉体的影响

采用聚丙烯酰胺凝胶法,分别以氧氯化锆、硫酸锆和硝酸氧锆为锆源制备ZrO2纳米粉体,利用热重-差热同步分析仪(TG-DSC)、X射线衍射仪(XRD)和扫描电子显微镜(SEM) 分别对凝胶的热分解过程及氧化锆粉体的物相组成和形貌进行分析和表征,研究了不同锆源对聚丙烯酰胺凝胶法所制备的ZrO2纳米粉体相转变、物相组成及粉体形貌的影响。结果表明,锆盐影响聚丙烯酰胺凝胶的热分解完全温度,以硝酸氧锆为前驱体制得的凝胶热分解完全温度最低,约为530 ℃,以硫酸锆和氧氯化锆为前驱体制得的凝胶热分解完全温度分别为573 ℃和580 ℃。锆盐影响氧化锆的晶化温度,但氧化锆的相转变过程相似,均是由无定型氧化锆转变为四方相氧化锆,并在900 ℃时完全转变为单斜相氧化锆。氧化锆的晶化温度越高,平均粒径越小,团聚程度越高,以上述三种锆源为前驱体均可制备出近似球形的纳米氧化锆粉体,粉体粒径分布在52~97.4 nm范围内。     

溶胶-凝胶法制备HfB2粉体及其氧化行为

以HfCl4、H3BO3、酚醛树脂为原料,通过溶胶-凝胶结合碳热还原法成功制备了HfB2粉体。分别采用XRD和SEM对高温处理后的粉体相组成和微观形貌进行了分析;采用TGA研究了粉体的高温氧化行为。结果表明：处理温度及硼酸浓度的不同会导致产物纯度、颗粒大小的不同,而且高温氧化性能也有所不同。当处理温度为1800 ℃且硼酸含量高于生成硼化铪化学计量比时,产物的纯度较高,颗粒均匀,高温氧化性能较好。对溶胶凝胶结合碳热还原法制备HfB2粉体的反应机制进行了探讨     

Zn2SiO4微波陶溶胶-凝胶法制备及性能研究

以Zn(NO3)2·6H2O和正硅酸乙酯为前驱体,乙醇作为溶剂,采用溶胶-凝胶法制备了ZnzSiO4微波陶瓷粉体,并研究了粉体的烧结特性和微波介电性能.干凝胶在800℃热处理后得到的ZnO和Zn2SiO4纳米级混合粉体.溶胶凝胶法制各的粉体具有更大的比表面积,使作为粉体烧结驱动力的表面能剧增,促使陶瓷在1200～1350℃实现致密烧结,比固相法合成粉体的烧结温度降低近200℃,并具有优异的介电性能:εr=6.14,Qf=67,500 GHz(12 GHz).     

溶胶-凝胶还原氮化合成β-sialon微细粉

以异丙醇铝、氧化硅细粉、活性碳粉等为起始原料，通过溶胶-凝胶、还原氮化工艺制备了β-sialon微细粉。将原料粉末在异丙醇铝水解得到的勃姆石凝胶中充分混合并干燥制备出合成所需的粉体原料，分别添加0．3％（质量分数，下同）的MgO、Y2O3、Fe2O3和CaO粉末并充分混合，混合粉体原料分别在1450℃和1500℃流动氮气下保温8h和4h。研究了添加剂、氮化温度等工艺条件对合成β-sialon粉体的影响。结果表明：添加剂MgO、Y2O3、Fe2O3可以促进β-sialon 的合成，其中MgO的促进作用最明显；1450-1500℃是比较合适的氮化温度；SEM结果表明：合成的β-sialon粉体的粒子尺寸在1gm左右；XRD的结果表明：合成β-sialon粉体的纯度在90％左右，Z值为2．9。     

溶胶-凝胶法制备La2O3纳米粉体

以普通La2O3,硝酸,聚乙二醇为原料,利用溶胶-凝胶法制备了纳米La2O3粉体,利用TG-DTA,XRD,TEM等各种测试方法对干凝胶300℃灼烧所得前驱体粉末的分解过程及最终形成的纳米氧化镧粉体进行了分析和表征,并研究了浓度、搅拌和分散剂聚乙二醇(PEG)添加量等因素的改变对La2O3粉体的粒径、形态的影响.实验结果表明,在适当工艺参数下,可以制得平均粒径小于50 nm的La2O3粉体.     

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。