Pressureless sintering of La-Y-Sialon ceramics and grain growth in later period of sintering

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Densification and grain growth kinetics of boron carbide powder during ultrahigh temperature spark plasma sintering

Dense B₄C material was fabricated using spark plasma sintering (SPS), and the densification mechanisms and grain growth kinetics were revealed. The density, hardness, transverse flexure strength and toughness of samples were investigated and the model predictions were confirmed by SEM and TEM experimental observations. Results show that SPSed B₄C exhibits two sintering periods: a densification period (1800–2000 °C) and a grain growth period (2100–2200 °C). Based on steady-state creep model, densification proceeds by grain boundary sliding and then dislocation-climb-controlled mechanism. Grain growth mechanism is controlled by grain boundary diffusion at 2100 °C, and then governed by volume or liquid-phase diffusion at 2200 °C.     

氮化铝陶瓷低温烧结过程中的液相迁移与表层晶粒生长

对YF3-CaF2烧结助剂体系的氮化铝(AlN)低温烧结过程中液相向表面迁移的现象和表层晶粒生长进行了研究, 同时分析讨论了液相迁移的机制. AlN低温烧结过程中液相向表面的迁移, 有利于减少晶界相, 提高其热导率. 然而, 液相向表面过量迁移和富集则导致了表层晶粒的异常生长, 坯体内部由于缺乏液相烧结助剂不能实现致密化, 这一现象也造成陶瓷基板的翘曲. AlN陶瓷坯体在烧结起始阶段的快速收缩和坯体内部AlN晶界两面角大于72.5°都有助于液相向表面迁移. 低温烧结后陶瓷表面的主要物相是AlN和Y2O3, Y2O3的出现并被碳热还原生成可挥发的YN可能是表面呈现蓝紫色的原因. 表面Y2O3的产生与钇铝酸盐(Y3Al5O12, Y4Al2O9)液相迁移至AlN陶瓷表面并与炉中碳气氛发生碳热还原有关.     

Quantitative evaluation of normal and abnormal grain growth of cemented carbides during liquid phase sintering

The liquid-phase sintering (LPS) of cemented carbides prepared from submicronic powders induces a micro-structural evolution generally ascribed to normal and abnormal grain growth. Such phenomena can be prevented by small additions of inhibitors (Cr, V). Presently, the mechanisms controlling either the grain growth or its inhibition are not strictly identified. In the present work, the effects of major parameters on grain growth (initial WC grain size, liquid composition, liquid fraction) are studied by image analysis of specimens sintered at 1450°C up to 8h.The evolution of the mean intercept and intercept distribution of WC grains is analysed in terms of the possible mechanisms involved.     

Microscopic study for the behavior of grain boundary using molecular dynamics

In this study, MD simulations have been performed to observe the behavior of a grain boundary in an a-Fe plate under 2-dimensional loading. In MD simulation, the acceleration of every molecule can be achieved from the potential energy and the force interacting between each molecule, and the integration of the motion equation by using the Verlet method gives the displacement of each molecule. Initially, four α-Fe rectangular plates which have different misorientation angles of grain boundary were modeled by using the Johnson potential and Morse potential. We compared the potential energy of the grain boundary system with that of the perfect structure model, which does not have a grain boundary inside. Also, we could obtain the width of the grain boundary by investigating the local potential energy distribution. The tensile loading for each grain boundary model at room temperature was applied and the behavior of the grain boundary was studied. From this study it was clarified that when the Johnson potential is used, the obvious fracture mechanism occurs along the grain boundary. With the Morse potential, the diffusion of the grain boundary appears instead of the grain boundary fracture.     

Effect of grain boundary energy on surface-energy induced abnormal grain growth in columnar-grained film

In columnar-grained film with anisotropy in the surface energy, abnormal grain growth occurs to minimize the overall energy. We studied the effect of grain boundary energy on the surface-energy driven abnormal grain growth in thin films using the Monte Carlo computer simulation. Our simulation results show that the growth speed of abnormal growth slows down when grain boundary energy increases. It is because the speed of normal growth driven by the grain boundary energy minimization gets faster with increasing grain boundary energy, while that of the abnormal growth induced by the fixed surface energy is consistent. The growth kinetics was monitored based on the growth velocity of the abnormal grains relative to the average growth velocity of all the grains. It was also found that the abnormal growth kinetics was retarded by impingements among abnormally growing grains when there was more than one abnormal grain.     

Experimental and simulation studies on grain growth in TiC and WC-based cermets during liquid phase sintering

The grain growth behaviors of TiC and WC particles in TiC-Ni, TiC-Mo₂C-Ni, WC-Co and WC-VC-Co alloys during liquid phase sintering were investigated for different Ni or Co contents and compared with the results of Monte Carlo simulations. In the experimental study, TiC-Ni and WC-Co alloys had a maximum grain size at a certain liquid volume fraction, while the grain size in TiC-Mo₂C-Ni and WC-VC-Co alloys increased monotonically with an increasing liquid volume fraction. These results mean that the grain growth of these alloys cannot be explained by the conventional mechanisms for Ostwald ripening, namely diffusion or reaction controlled processes. Monte Carlo simulations with different energy relationships between solidliquid interfaces predicted the effect of the liquid volume fraction on grain size similar to the experimental results. The contiguous boundaries between solid (carbide) particles appear to influence the grain growth behavior in TiC- and WC-based alloys during liquid phase sintering.     

Effect of carbide additions on grain growth in TiC−Ni cermets

The growth of carbide particles in TiC-XC-2 vol.% Ni and TiC-XC-30 vol.% Ni alloys, where X=Zr, Cr, W, Ta and Mo, was fitted to an equation of the form d³-d_o ³=Kt. The grain growth behavior during liquid phase sintering at 1673K decreased markedly with the addition of Mo₂C or WC, changed little for TaC, and increased with the addition of ZrC or Cr₃C₂. The grain contiguity decreased with increasing Ni content in the TiC−Mo₂C−Ni alloy and was greater in the alloys with smaller growth rate constant. Consequently, the effect of carbide addition on the grain growth of 2 vol.% Ni alloys was found to be similar to that of 30 vol.% Ni alloys. The grain growth mechanism could be explained by the effect of contiguous carbide grain boundaries in restricting the overall grain growth, as well as the area of the solid/liquid interfaces in the alloy by the usual solution/reprecipitation model.     

金属纳米晶粉体材料中的不连续晶粒长大

采用高能球磨法制备了Co纳米晶粉体,平均晶粒尺寸为(17±3)nm.设计了一系列宽温度范围的退火实验,考察纯Co纳米晶粉体的晶粒长大行为.实验发现,低温区和高温区的晶粒长大动力学有明显差异,而在中温区出现不连续晶粒长大特征.高分辨透射电镜观测表明:在低温区,纳米晶中存在较大比例的小角度纳米晶界,而在高温区则基本为典型的大角度晶界.结合纳米晶热力学计算和DSC分析,认为纳米晶粒在中温区的突发迅速长大是由残余储存能作为附加驱动力激发的动力学过程,其主导机制是通过相邻小角度位向差的纳米晶粒的转动而实现晶粒快速粗化.     

微波烧结WC-Co硬质合金致密化与晶粒生长

分别采用微波烧结和常规烧结制备WC-8Co硬质合金,通过1 000~1 400℃温度范围烧结以及1 400℃保温0~240 min的微波和常规烧结实验,测量各样品的收缩率、密度和晶粒尺寸,分析其致密化行为和晶粒生长,研究烧结温度和保温时间对合金致密化和晶粒生长的影响。结果表明,与常规烧结比较,微波烧结促进YG8硬质合金的致密化,且获得的合金组织均匀,晶粒细小。另外,保温时间对微波烧结YG8硬质合金的晶粒生长几乎没有影响。     

Sintering process and grain growth of Mn-Zn ferrite nanoparticles

The density, microstructure and magnetic properties of non-doped Mn-Zn ferrite nanoparticles sintered compacts were investigated. The compacts of non-doped Mn-Zn ferrite nanoparticles were sintered by segmented-sintering process at lower sintering temperature. The density of sintered samples was measured by Archimedes method, and the phase composition and microstructure were examined by XRD and SEM. The sintered Mn-Zn ferrite magnetic measurements were carried out with Vibrating Sample. The results show that the density of sintered compacts increases with the rising of sintering temperature, achieving 4.8245 g·cm-3 when sintered at 900 ℃, which is the optimal density of Mn-Zn functional ferrite needed and from the fractured surface of sintered samples, it can be seen that the grain grows well with small grain size and homogeneous distribution.     

最大取向值对晶粒生长元胞自动机模拟结果的影响

为了研究最大取向值Q的大小对晶粒生长的元胞自动机模拟过程及结果的影响,对Q值分别取30、50、70、100、150、200时进行了模拟分析。结果表明,Q值较小时晶粒生长过程中极易发生晶粒碰撞现象导致晶粒异常长大,当Q值大于100时模拟过程平稳且符合晶粒生长理论,当Q值大于150时对模拟过程没有显著影响。不同Q值时晶粒的生长指数相差很小,且与其他研究者给出的生长指数十分接近,说明模拟过程是可信的。     

液相对ZnO陶瓷放电等离子体烧结过程的影响

本文采用放电等离子体烧结技术制备了ZnO陶瓷,主要研究了液相(醋酸溶液)的添加对烧结过程的影响。结果表明,通过对初始粉料添加微量的2 mol/L的醋酸溶液,在等离子体烧结过程中,ZnO陶瓷试样在52 _^oC开始收缩,115 _^oC开始致密化,160 _^oC致密度可达95%以上,200 _^oC度即可完成致密化。在250 ℃烧结5 min后,晶粒尺寸从初始粉体的200 nm增长到600 nm。X衍射结果表明,在液相辅助等离子烧结过程中,ZnO陶瓷中未出现明显杂相,并且晶粒生长表现出沿外施压力垂直的方向取向生长。通过计算发现液相辅助等离子体烧结ZnO陶瓷,其晶粒生长活化能仅为78.8 kJ/mol,约为传统高温烧结的三分之一。ZnO陶瓷试样的室温阻抗结果表明,晶界阻抗随烧结温度的升高而下降,从120 _^oC烧结试样的9.82×10_⁶ W下降到250 _^oC烧结试样的2.75×10_³ W。     

Control of {111| twin formation and abnormal grain growth in BaTiO3

To investigate the experimental conditions for {111| twin formation and abnormal grain growth in BaTiO₃, various powder compacts with and without excess TiO₂ were sintered either in an oxidizing atmosphere (air) or in a reducing atmosphere (95N₂-5H₂). In all the samples sintered in 95N₂-5H₂, no twins formed and no abnormal grain growth occurred. On the other hand, when the samples with excess TiO₂ were sintered in air, abnormal grain growth occurred and all the abnormal grains contained {111| twins. X-ray diffraction analysis showed that, during sintering, the excess TiO₂ formed a Ba₆Ti₁₇O₄₀ phase with the space group A2/ a in air and a Ba₆Ti₁₇O_40-x phase with the space group C in 95N₂-5H₂. These results show that the {111| twins form and the abnormal grain growth occurs only when the powder compact contains excess TiO₂ to form a Ba₆ Ti₁₇O₄₀ phase and is sintered in an oxidizing atmosphere. The results may also suggest that the Ba₆Ti₁₇O₄₀ phase acts as the nucleation site of {111| twins. The suggestion has been further confirmed via a TEM observation.     

激光烧结纳米Al2O3陶瓷的研究

纳米陶瓷材料具有许多优异的功能和特性,但在烧结过程中纳米颗粒容易长大,从而失去纳米特性.对激光烧结纳米陶瓷进行的理论和试验分析证明:利用激光烧结的方法,可使烧结陶瓷的晶粒保持在纳米尺度,从而为纳米材料在功能部件和结构部件等方面的应用提供了基础.     

MC方法模拟晶粒长大的改进算法和晶粒数统计的研究

基于材料等温下所有晶粒长大的同步性,认为单元进行再取向尝试时采用随机提取更符合物理模型,且所有单元全部提取并完成一次再取向尝试记为一个MCS,弥补了以往模拟中采用逐一提取单元的不足.晶粒长大模拟结果符合大晶粒不断变大且有相似性,小晶粒的无规则随机变小的规律.采用了对晶粒个数、面积的精确统计算法,得出晶粒长大指数达到0.48～0.51.     

V-Nb-(Ti)微合金化钢奥氏体晶粒长大的动力学

采用金相分析方法研究了V-Nb和V-Nb-Ti微合金化钢在不同加热温度下原始奥氏体晶粒长大的规律,并在此基础上,对其奥氏体晶粒生长动力学方程进行了数学回归分析.结果表明:随奥氏体化温度的升高,两种微合金化钢的奥氏体晶粒尺寸均呈现增加的趋势,其不均匀因子则呈现出先增大后减小的趋势.但V-Nb-Ti微合金化钢的奥氏体晶粒尺寸和不均匀因子的变化趋势均比V-Nb微合金化钢的平缓.V-Nb和V-Nb-Ti微合金化钢的奥氏体晶粒长大动力学方程均符合Beck方程.后者的奥氏体晶粒长大激活能20 kJ/mol稍大于前者19 kJ/mol.     

加热工艺参数对12%Cr钢晶粒长大行为的影响

研究了不同加热工艺参数下(加热温度1050～1300℃,保温时间0.25～24 h) 12%Cr超超临界转子钢的奥氏体晶粒长大行为,并通过光学显微镜(OM)观察晶粒尺寸的变化规律,建立晶粒长大数学模型。结果表明:随着加热温度增加,晶粒尺寸逐渐增加,加热温度低于1150℃时,晶粒尺寸增加明显,而温度高于1150℃后,晶粒尺寸逐渐趋于稳定;随着保温时间的增加,晶粒尺寸逐渐增加,保温时间增加到3 h后,晶粒尺寸增加趋势放缓。采用非线性回归方法和Arrhenius晶粒长大模型,建立了该钢的晶粒长大数学模型。