碳化硼固相烧结微观结构演化的同步辐射CT观测

利用同步辐射CT (SR-CT) 技术,在碳化硼陶瓷样品烧结过程中对其进行实时投影成像,并应用滤波反投影算法和数字图像处理技术,得到了样品在整个烧结过程中内部微结构演化的二维和三维重建图像,实现了对陶瓷固相烧结过程实时、无损的观测.通过重建图像清晰观测到了陶瓷样品在烧结三个阶段中颗粒接触、烧结颈形成、晶粒和气孔长大、气孔球化并收缩等烧结现象;统计了样品在不同烧结时刻的孔隙率,得到了孔隙率随烧结时间和烧结时间对数的变化曲线,并根据曲线分析了样品在不同烧结时刻致密化速率的变化,得到了烧结中期孔隙率和时间对数的线性关系.实验结果和现有烧结理论相吻合,并为进一步完善烧结理论以及建立扩散和本构模型提供了有效的实验数据.     

陶瓷烧结过程孔隙演化的二维相场模拟

采用二维相场模型模拟陶瓷烧结过程中颗粒间孔隙的演化过程.选取四方堆积颗粒间气孔作为对象.通过连续的密度场和长程取向场（LRO）描述烧结体的微结构,密度场的演化由Cahn-Hillard（CH）方程控制,而颗粒的取向场演化由时间相关的Ginzburg-Laudau（TDGL）方程控制.上述非线性演化方程利用半隐傅立叶频域法求解.模拟结果反映了颗粒间接触,烧结颈生长和气孔球化的微观过程.量化计算烧结颈生长率以及在不同晶界和表面迁移率比值时的烧结率,较好地符合理论分析的趋势.     

固相烧结后期晶粒和气孔拓扑生长演化的二维相场模拟

本文采用二维相场模型模拟固相陶瓷烧结后期，晶粒和气孔耦合生长演化过程。以连续变化的组分参量和长程序参量（LRO)表征微观烧结体的组分相和晶相扩散拓扑结构，由Cahn-Hillard(CH)方程和Ginzburg-Laudau(TDGL)方程分别控制组分场和取向场时间相关的扩散演化，并且利用半隐傅立叶频域法高效地模拟了烧结后期晶粒和气孔拓扑形貌的扩散演化，并且利用半隐傅立叶频域法高效地模拟了烧结后晶粒和气孔拓扑形貌的演化过程和统计分析生长参数，并通过与完全致密体晶粒生长速率比较，量化分析残余气孔对昌粒生长的影响。     

先进陶瓷材料固相烧结理论研究进展

系统介绍了陶瓷材料固相烧结理论的历史和研究进展,综述了用来描述烧结前期、中期和后期的烧结理论和烧结模型.目前烧结理论大多局限于烧结全程的某一阶段,且只研究某一种扩散机制起主导作用,多数理论烧结模型不能完全反映真实烧结参数,烧结单元模型的定量描述不够完善,缺乏描述烧结全程的烧结模型,且大多研究局限于基础研究,如物质的传输机制、致密化过程、气孔和晶粒生长机制.因此,建立多种扩散机制耦合作用的全期烧结模型,进一步研究烧结动力学,用计算机模拟烧结的真实条件,建立能定量描述的烧结模型,是未来烧结理论研究的方向.     

固相烧结SiC陶瓷

实验采用α-SiC,β-SiC和（1％αSiC＋99％β-SiC作为起始粉末,以B,C为添加剂,热压烧结SiC陶瓷,其烧结过程中尽管发生多型体之转的转变,但其现现形式为α-SiC的6H→4H,和β-SiC的3C→6H两种形式,尽管有大量的长柱颗粒生成,但是由于没有弱的界面结合,不能原位增强。     

颗粒级配对固相烧结碳化硅陶瓷的影响

通过粗细碳化硅粉体的颗粒级配实现了致密固相烧结碳化硅(S-SiC)陶瓷的增强增韧, 系统研究了粗粉(~4.6 µm)加入量对烧结试样的致密化、微结构与力学特性的影响。结果表明: 当粗粉加入量不超过75wt%时, 可制备出相对密度≥98.3%的致密S-SiC陶瓷, 烧结收缩率低至14.5%;引入的粗粉颗粒产生钉扎作用, 显著抑制了S-SiC陶瓷中异常晶粒生长, 形成细小的等轴晶粒, 进而提高了S-SiC陶瓷的抗弯强度。同时, 粗粉颗粒的引入导致S-SiC陶瓷的断裂方式由穿晶断裂转变为穿晶-沿晶复合断裂, 使得S-SiC陶瓷的断裂韧性增强。对于粗粉引入量为65wt%的S-SiC陶瓷, 抗弯强度与断裂韧性分别为(440±35) MPa与(4.92±0.24) MPa•m^1/2, 相比于未添加粗粉的S-SiC陶瓷, 分别提升了14.0%与17.1%。     

SXR-CT技术应用研究烧结陶瓷三维微结构拓扑形貌

借助同步辐射硬X射线高强度，强穿透，高分辨和天然准直性的特性，应用卷积反投影重建算法实现CT三维重建技术，简称SXR—CT(Synchrotron X-Ray Computed Tomography),研究了氧化物陶瓷烧结体残余孔隙的三维拓扑微结构。同时量化计算了样品的孔隙率和密度，较好地符合实验测量数据。     

固相剪切碾磨制备铝粉填充聚乙烯基高性能导热复合材料的研究

采用固相剪切碾磨法(S3M)制备铝粉和线性低密度聚乙烯(LLDPE)的复合粉体,再经熔融加工获得高性能LLDPE/Al导热复合材料。借助扫描电镜(SEM)、激光粒度分析仪等表征铝粉在基体中的微观形态和分散状态,同时研究LLDPE/Al复合材料的热导率、力学性能和热稳定性。结果表明:固相剪切碾磨过程中铝粉受磨盘挤压、拉伸、摩擦剪切等复合力场作用,由较小球形颗粒变为较大片状,同时在基体中均匀分散且界面结合得以增强,因此复合材料拥有更高的热导率、更好的力学性能和热稳定性。当铝粉填充质量分数为80%时,经固相剪切碾磨10次制备的复合材料热导率高达8.782W·m~(-1)·K~(-1),拉伸强度和弯曲强度分别为33.00MPa和31.16MPa,初始分解温度比基体提高约13℃。     

固相烧结SiC陶瓷的非线性电学行为研究

固相烧结SiC(SSiC)陶瓷大多数用于结构陶瓷材料, 用于电子和电阻元器件的研究很少。实验以添加不同C含量的致密SSiC陶瓷材料为研究对象, 研究了添加不同C含量SSiC陶瓷的伏安特性、电阻率与电流密度的变化关系及电阻率与温度的变化关系。研究结果表明: SSiC陶瓷表现出明显的非线性电学特性, 其电阻率随着电流的增大而降低; 对于添加3wt% C含量的SSiC陶瓷, 当电场强度超过15.8 V/mm时, 晶界势垒被击穿; 对于添加6wt% C含量的SSiC陶瓷, 当电场强度超过70.7 V/mm时, 晶界势垒被击穿, 它们的电阻率将为晶粒所控制, 电阻率较小; 同时在电场强度1 V/mm条件下, SSiC陶瓷电阻率随着温度的升高而降低, 表现出很好热敏特性, 从常温的10⁶ Ω·cm变化为400℃的5 Ω·cm左右。     

纳米晶钨基重合金粉末的注射成型与固相烧结

采用高能球磨技术制备了９０Ｗ－７Ｎｉ－３Ｆｅ（质量分数,％）纳米晶钨基重合金粉末,研究了该粉末的注射成型和烧结行为,并与传统混合粉末进行了比较,结果表明,机械球磨可以有效地增加粉末喂料的固体粉末含量,改善粉末料的均匀性,并可促进团相烧结的致密化,纳米粉末注射成形坯在 １３００～１４５０℃进行固相烧结后,可得到近全致密（＞９９％）、晶粒细（３～５μｍ）、拉伸强度高（≥１１３０ＭＰａ）和几乎无变形的重合金样品     

铝粉烧结材料等通道转角挤压组织性能演变

对不同路径和不同道次下铝粉烧结材料的等通道转角挤压工艺进行了试验研究,用光学显微镜、扫描电子显微镜和透射电镜分析了粉末烧结材料在不同工艺条件下的晶粒细化规律和致密行为,并测量了挤压后试样的密度和硬度等性能.结果表明,等通道转角挤压工艺对粉末烧结材料具有很强的致密效果和细化效果,可显著提高其力学性能.在单道次变形中,大剪切塑性变形和高静水压力状态是粉末烧结材料获得良好的致密效果的关键;在多道次变形中,变形量的累积和不同的剪切特征不断地改变内部的孔隙形状,使内部基体材料进一步致密.而晶粒的细化效果则取决于变形中的静水压力、变形量和剪切特征等关键因素.     

Microstructural evolution during the supersolidus liquid phase sintering of nickel-based prealloyed powder mixtures

A novel concept for full-density sintering is described. Two prealloyed powders with slight compositional differences are tailored to separate the solidus temperatures into high-melt and low-melt compositions. A mixture of these two powder compositions allows full-density sintering at a temperature between the two solidus temperatures. For these experiments, the two powders were nickel-based alloys, where the low-melt powder contained boron. The mixed powders were sintered at temperatures above the solidus of the low-melt powder to form a transient liquid that promoted rapid densification of the mixture. Microstructure evolution during sintering was assisted using quenching experiments. Variables in this study included the heating rate, peak temperature, hold time, and powder ratio. Interdiffusion between the two powders controls microstructure evolution, with a dominant role associated with boron diffusion and reaction. The transient liquid phase responsible for densification is linked to boron diffusion and subsequent compound precipitation.     

Microstructure evolution in aluminum alloy AA 2014 during multi-layer friction deposition

How microstructures evolve in heat-treatable aluminum alloys during multi-layer friction deposition is an intriguing question. The current work shows that the process invariably leads to overaging of strengthening precipitates in such materials as alloy 2014. The problem can be overcome using a solution treatment, but it can lead to other problems such as abnormal grain growth. Based on these findings, it appears that the benefits of friction deposition cannot be fully realized in heat-treatable aluminum alloys.     

Ni-Al喷涂层反应烧结的组织演变与结合机制

为了改进热喷涂层组织结构和结合性能，在不引起反应的条件下，将Ni-Al混合粉（93%Ni 7?）喷涂于A3钢基材表面，通过中温反应烧结处理，制备了具有良好结合性能的涂层试样，利用SEM和XRD研究了涂层烧结前后显微组织和相结构的变化。结果表明：反应烧结前后涂层显微组织发生了明显变化，烧结后涂层所固有的层状结构消失；烧结时涂层中Al首先与Ni反应生成Ni2Al3，随处理温度增高而转化为NiAl3，基材界面出现冶金结合，并在界面愈合区间发现了Ni-Fe固溶体。     

选择性激光烧结铝/尼龙复合粉末材料

制备了不同铝粉含量的尼龙12覆膜复合粉末,利用扫描电镜(SEM),能谱分析(EDX),差示扫描量热分析(DSC),热失重分析(TG)对粉末材料的形貌以及热性能进行了表征。对复合粉末进行激光烧结成形,并研究了不同铝粉含量对烧结件尺寸精度以及力学性能的影响。结果表明:尼龙与铝粉表面粘结良好,烧结过程中尼龙熔融,铝粉均匀分布在尼龙基体中;随着铝粉含量的增多,烧结件的弯曲强度和模量显著提高,冲击强度逐渐降低;铝粉质量分数为50 wt%时,烧结试样的弯曲强度和模量与纯尼龙烧结试样相比分别提高了62. 1%和122.3%;铝粉含量的增多能够有效抑制尼龙基体的收缩,提高烧结件的精度。      

Microstructural evolution of injection molded gas- and water-atomized 316L stainless steel powder during sintering

The present study investigates the microstructural evolution and densification behavior of water- and gas-atomized 316L stainless steel powder. Dilatometry and quenching studies were conducted to determine the extent of densification and corresponding microstructural changes. Results indicate that water-atomized powder could be sintered to 97% of theoretical density, while gas-atomized powders could be sintered to near-full density. The difference in the densification behavior is examined in terms of the particle morphology, initial green density and the particle chemistry.     

Effect of the powder precursor characteristics in the reaction sintering of aluminum titanate

Aluminum titanate precursor powders, containing 2.5 wt.% MgO additive, were prepared by two powder processing methods, the hydrolysis of alkoxides and coprecipitation of inorganic salts. The hydrolysis-derived precursor powder showed a higher chemical homogeneity than the coprecipitated-derived precursor powder. Dilatometric analysis, accomplished with XRD and microscopy, was a very good method to study both phase transformation and sintering processes. Different phase transformation paths of TiO₂ and Al₂O₃ were observed in the two powders. The formation of aluminum titanate solid solution began at ∼1220°C in both, but in the hydrolysis-derived powder compact the aluminum titanate grains grew faster, leading to incomplete reaction and a non-uniform microstructure of large grains with small residual inclusions.     

Implementation of a phase field model for simulating evolution of two powder particles representing microstructural changes during sintering

In this work, we present a multiphysics phase field model for capturing microstructural evolution during solid-state sintering processes. The model incorporates modifications of phase field equations to include rigid-body motion, elastic deformation, and heat conduction. The model correctly predicts consolidation of powder particles during sintering because of two competing mechanisms—neck formation and grain growth. The simulations show that the material undergoes three distinctive stages during the sintering process—stage I where neck or grain boundary between two particles is formed, stage II in which neck length stabilizes and growth or shrinkage of individual particles initiates, and finally stage III with rapid grain growth leading to disappearance of one of the grains. The driving forces corresponding to different mechanisms are found to be dependent on the radius of the particles, curvature at the neck location, surface energy, and grain boundary energy. In addition, variation in temperature is found to significantly influence the microstructure evolution by affecting the diffusivity and grain boundary mobility of the sintered material. The model is also used to compare sintering simulation results in 2D and 3D. It is observed that due to higher curvature in 3D, model predicts faster microstructural evolution in 3D when compared to 2D simulations under identical boundary conditions.     

冷轧多晶铜与多晶铝形变显微组织演变的研究

采用ＴＥＭ对冷轧多晶铜与多晶铝的形变显微组织演谱进行了对比研究,多晶铜及多晶铝形变显微组织中均含有三类典型的位错结构类型,其中的两种结构特征在两种材料中是相似的,这两种类型结构存在于非立方取向晶粒,可通过晶粒中位错边界的晶体学取向加以区别,另一类型结构存在于立方取向晶粒;晶粒的晶体学取向决定了其形变显微组织类型,但其它冶金学因素对显微组织也有影响。