SiCp/Al复合材料的SPS烧结及热物理性能研究

采用纯粉末, 通过SPS烧结制备了组织均匀、致密且体积分数高的SiCp/Al电子封装材料. 通过对SPS烧结现象的研究, 认为该复合材料的SPS烧结过程属于反应性烧结, 大部分收缩在极短时间内完成; 另外对SiC体积分数和SiC颗粒尺寸对热导率、热膨胀系数的影响进行了研究, 发现SiC体积分数越高, 复合材料的热导率和热膨胀系数越低; SiC颗粒粒径增大, 复合材料的热导率增高, 而热膨胀系数减小.     

SiC陶瓷基片的烧结工艺与SiC_p/Al复合材料的制备方法

概述了电子封装基片材料的基本性能要求;讨论了SiC陶瓷基片常用的4种烧结工艺,即常压烧结、热压烧结、反应烧结和放电等离子烧结;介绍了SiCp/Al复合材料的制备方法,即搅拌铸造法、无压渗透法、喷射沉积法、粉末冶金法;据此进一步提出了SiC陶瓷基片材料的发展方向。     

微波烧结SiC颗粒增强铝基复合材料

采用微波烧结的方法,在烧结温度分别为680℃,710℃,740℃,770℃,800℃制备了15％的SiCp／Al复合材料。探讨温度对材料的致密度和力学性能的影响。结果表明：致密度和材料硬度及冲击韧性随温度变化呈马鞍形,在770℃样品的密度和硬度及冲击韧性达到最佳值,分别为2．62g／cm3,42．6MPa,40J／cm2。结论：用微波烧结SiCp／Al复合材料可在短时间内使样品达到烧结致密化,缩短烧结时间,节约能源。     

放电等离子快速烧结SiC晶须增强Si3N4BN层状复合材料

采用放电等离子烧结技术（SPS）快速烧结了SiC晶须增强的Si3N4/BN层状复合材料。利用SPS技术，在烧结温度为1650℃，保温15min的条件下，材料的密度可达3．18g/cm^3, 抗弯强度高达600MPa，断裂功达到3500J/m^2。研究表明；特殊的层状结构，SiC晶须的拔出与折断是材料断裂功提高的主要原因。X射线衍射及扫描电子显微镜研究表明：α-Si3N4已经在短短的烧结过程中全部转变成长柱状的β-Si3N4，并且长柱状的β-Si3N4和SiC晶须具有明显的织构。     

放电等离子烧结对TiB_2/AlCoCrFeNi复合材料组织与性能的影响

采用放电等离子烧结方法(SPS),制备体积分数5%TiB_2的等摩尔AlCoCrFeNi高熵合金基复合材料。通过密度测试、X射线衍射、扫描电镜及力学性能测试等方法,研究SPS烧结温度及烧结压力对复合材料的微结构演变与力学性能影响。结果表明:随着SPS烧结温度及烧结压力的增加,复合材料的硬度及抗压强度得到明显提高。在1200℃/30MPa进行SPS烧结后,复合材料的致密度达99.6%,抗压强度达2416MPa,屈服强度达1474MPa,硬度超过470HB。烧结过程中,复合材料的基体高熵合金发生相变,1200℃及30~45MPa烧结时,复合材料由BCC,B_2,FCC,σ及TiB_2相组成。     

TiAl纳米合金的机械活化-放电等离子原位烧结

（Ti-50％（原子分数）AD-10％Al2O3粉体经过球磨的机械活化（MA）后，用放电等离子烧结（SPS）工艺，在烧结的同时进行固化。采用机械活化-放电等离子烧结（MA—SPS）的方法原位烧结制备TiAl—Al2O3块体纳米材料。球磨前后，（Ti-50％（原子分数）AD-10％Al2O3粉体的衍射图（XRD）相似。MA后得到晶粒度〈25nm的纳米粉体，其中Al2O3起到机械活化和细化晶粒的作用，促使粉体快速纳米化。纳米粉体在温度低于800℃、烧结时间〈5min的烧结参数下，烧结成TiAl纳米合金。TiAl纳米合金的微观结构表明，合金有γ-TiAl和α2—Ti3Al双相组织。SPS原位烧结后，得到密度为3．73g／cm^3的（γ＋α2）双相组织，组成相的晶粒度〈130nm。     

低温多段烧结、真空压力浸渗制备SiCp/Al电子封装材料

选用W7与W63两种SiC粉末,采用高、低温粘结剂配合,模压成型,850℃空气气氛低温多段烧结,制备出体积分数为65.13％的SiC预制件,真空压力浸渗6063A1合金熔液,得到SiCp/A1复合材料.结果表明:复合材料XRD图谱中未出现明显的Al4C3界面相和SiO2杂相;致密度高;100℃时的热膨胀系数为7.592...     

电子封装SiCp/356Al复合材料制备及热膨胀性能

采用无压渗透法制备了SiCp／356Al复合材抖．用SEM和XRD对复合材料组织形貌和物相进行了研究，测定了复合材料在50-400℃温度区间的热膨胀系数。分析了复合材料热膨胀性能的影响因素。结果表明SiCp／356Al复合材料中SiC颗粒分布均匀，无明显新相形成，复合材料的热膨胀系数比基体合金的热膨胀系数显著降低，复合材料热应力引起热膨胀性能的变化随温度的不同而不同。     

Al2O3-ZrO2(3Y)-SiC纳米复合材料的制备及性能

本文研究了非均相沉淀法制备Al2O3－ZrO2（3Y）－SiC复合粉体的工艺过程,认为粉体的理烧温度是至关重要的,热压烧结得到了致密的Al2O3－ZrO2（3Y）－SiC纳米复合材料,ZrO2的加入对烧结温度的影响不大．通过TEM观察,SiC颗粒均匀分散于材料中,大的ZrO2颗粒位于Al2O3晶粒间,小的圆形ZrO2颗粒位于Al2O3晶粒内,一部分Al2O3晶粒呈非等轴状．80Wt％Al2O3－15wt％ZrO2－5Wt％SiC纳米复合材料的抗弯强度可达555MPa,韧性为3.8MPa．m1／2.     

SiCp/Al基复合材料的耐蚀性研究

用电化学方法和腐蚀失重法研究了2024Al和SiCp/2024Al基复合材料在3．5％NaCl水溶液中的耐蚀性,用电化学交流阻抗技术对它们的硫酸阳极氧化膜的耐蚀性进行了研究。结果表明,SiCp/2024Al复合材料在3．5％NaCl水溶液中比相应的基体金属有较大的腐蚀敏感性。SiCp/2024Al的阳极氧化膜耐NaCl溶液腐蚀能力不如2024Al合金的阳极氧化膜,是氧化膜中SiC颗粒的存在破坏了氧化膜的完整性和均匀性。     

Ti3SiC2-SiC复合材料的耐磨擦磨损性能

以商用硅粉、碳粉、钛粉以及少量的铝粉为原料, 利用放电等离子烧结技术原位反应制备了Ti₃SiC₂-SiC复合材料. 利用盘销式摩擦磨损实验机测试了Ti₃SiC₂-SiC复合材料的耐摩擦磨损性能. 结果表明: 随着SiC含量的增加, 材料相对于硬化钢的摩擦系数和磨损系数均呈下降趋势, 这表明SiC的引入提高了复合材料的抗摩擦磨损性能. Ti₃SiC₂单相材料摩擦系数在0.8～1.0之间, 而Ti₃SiC₂-40vol% SiC复合材料在稳态下的摩擦系数达到了0.5, Ti₃SiC₂-40vol% SiC复合材料相对于Ti₃SiC₂单相材料的磨损系数下降了一个数量级. Ti₃SiC₂-SiC复合材料的高抗磨损性归因于磨损类型的改变以及SiC良好的抗氧化性能.     

Effect of fabrication process on the microstructure and dynamic compressive properties of SiCp/Al composites fabricated by spark plasma sintering

The effect of fabrication process on the microstructure and dynamic properties of SiC_p/Al composites was studied in this paper. Pure Al matrix composites reinforced with 20 vol.% SiC particles were fabricated by spark plasma sintering, and the pre-blended powders were prepared by two different processes. One was to mix the powders in conical flask by using a mechanical stirrer, and the other was the mechanical alloying process by using a planetary ball mill. The sintering temperature was also explored. The conventional split Hopkinson pressure bar was used to test the dynamic properties of these composites. The results show that the sintering temperature significantly affects the consolidation of the composites. The composites, which have not been fully densified, have very loose microstructure and poor mechanical properties. Mechanical alloying process can improve the microstructure and mechanical properties of the composites. These composites are rate dependent, their strengths increase with increasing strain rates.     

热压与放电等离子体烧结两种工艺制备Al2O3/Cu复合材料

由机械合金化法(MA)制得纳米级Al₂O₃颗粒弥散镶嵌于微米级Cu颗粒表面的复合粉末, 利用球形化工艺改善所制得复合粉的形貌及粒度范围, 分别采用热压法(HP)和放电等离子体烧结(SPS)法制备Al₂O₃/Cu复合材料。通过测试密度、 电导率、 抗弯强度及SEM复合粉形貌和烧结体断口分析、 微区成分分析, 对比研究了Al₂O₃质量分数分别为0%、 0.5%、 1.0%、 1.5%时Al₂O₃/Cu复合材料的物理、 力学和电学性能。结果表明: 不同制备工艺下随着Al₂O₃含量增加, 材料的抗弯强度先增后降, 电导率除受杂质影响外, 还受材料缺陷的影响, 故变化规律不明显, 对于Al₂O₃含量相同的Al₂O₃/Cu复合材料, 采用SPS法制备的复合材料的致密度、 抗弯强度及电导率均高于HP法; 在弯曲应力下两种制备方法所得复合材料均发生延性断裂。      

Thermal conductivity of spark plasma sintering consolidated SiCp/Al composites containing pores: Numerical study and experimental validation

A simple model was introduced for describing the effect of porosity on the effective thermal conductivity of spark plasma sintered (SPS) consolidated SiC_p/Al composites in terms of an effective medium approximation (EMA) scheme. Numerical results of the present model were compared to an existing model of two-step Hasselman–Johnson approach and experimental data. Both models yielded very close predictions, which provided a satisfactory agreement to the experimental data, especially for the composites with porosity below 10%. At high levels of porosity the model predictions were slightly higher than the experimental values. These two models were further extended to account for the thermal conduction properties of porous composites with a multimodal size distribution or multiphase reinforced mixtures.     

SPS原位反应制备TiC/Ti2AlC/TixAly系复合材料的微观结构及其导电性能

以Al₄C₃、Ti和石墨混合粉体为原料, 采用放电等离子技术原位反应制备了TiC/Ti₂AlC两相复合材料和TiC/Ti₂AlC/Ti_xAl_y三相复合材料. 利用XRD、SEM、TEM研究了复合材料的相组成和微观结构, HRTEM的观察结果显示复合材料的相界面清洁干净, 无非晶相存在. 同时研究了TiC/Ti₂AlC/Ti_xAl_y三相复合材料的原位反应烧结过程, 并对复合材料的导电行为进行了表征. 在室温时TiC/Ti₂AlC材料的电导率大于TiC/Ti₂AlC/Ti_xAl_y三相复合材料,其中TiC/40vol%Ti₂AlC的电导率最高达到8.83×105S/m. TiC/Ti2AlC两相复合材料和TiC/Ti₂AlC/Ti_xAl_y三相复合材料的电导率均随温度的升高而下降, 呈现电导的金属性特征, 同时电导率随温度变化关系符合Arrhenius理论.     

The dynamic properties of SiCp/Al composites fabricated by spark plasma sintering with powders prepared by mechanical alloying process

The dynamic compressive properties of SiC particle reinforced pure Al matrix composites, fabricated by spark plasma sintering technique with mixture powders prepared by mechanical alloying process, were tested in this paper. Two different average SiC particle sizes of 12 μm and 45 μm were adopted, and the compressive tests of these composites at strain rates ranging from 800/s to 5200/s were conducted by split Hopkinson pressure bar. The damage mechanism of the SiC_p/Al composites was analyzed through the microstructural observations and high-precision density measurements. Results show that the dynamic properties and damage accumulation of these composites are significantly affected by the particle distribution, size, particle cracking, particle/matrix interface debonding and adiabatic heat softening. The composites containing smaller SiC particles exhibit higher flow stress, lower strain rate sensitivity, and less damage at high strain rate deformation.     

放电等离子烧结制备Diamond/Al复合材料

采用放电等离子烧结法（SPS）制备了Diamond/Al复合材料,研究了金刚石粒径、成分配比、工艺参数等对复合材料的导热性能的影响。结果表明,SPS可以得到导热性能较好的Diamond/Al复合材料,致密度是影响该材料导热性能的最重要因素。在实验确定的金刚石体积分数50%,金刚石粒径70 μm,温度550℃、压力30 MPa的工艺条件下,所制备的材料致密度较高,热导率为182 W/(m·K),比相同条件下纯铝粉烧结体的热导率提高了34.8%,表明金刚石的添加对烧结铝基材料导热性能有明显的改善作用。      

放电等离子烧结制备高导热SiC_P/Al电子封装材料

为了满足电子封装材料越来越高的性能要求,采用放电等离子烧结(SPS)工艺制备了SiCP/Al复合材料。研究了烧结温度和保温时间等工艺条件对SiCP/Al复合材料组织形貌和性能的影响。结果表明:采用SPS烧结,温度为700℃、保温时间为5 min时,所制备的70 vol%SiCP/Al复合材料热导率达到195.5 W(m.K)-1,与传统15%W-Cu合金相当,是Kovar合金的10倍,但密度小,仅为3.0 g.cm-3;其热膨胀系数为6.8×10-6K-1,与基板材料热膨胀系数接近;抗弯强度为410 MPa,抗拉强度为190 MPa,达到了电子封装材料对热学性能和力学性能的要求。     

On CTE of SPS consolidated SiCp/Al composites with various particle size distributions

Abstract

The coefficient of thermal expansion (CTE) of spark plasma sintering consolidated SiC_p/Al composites with various size distributions was investigated with the combination of experimental measurements and modelling analyses. The CTE of the composites decreased with increasing particle volume fraction, and large particles played a major role in the decline of CTE. The measured CTE lay between the predictions of Kerner model and Schapery lower bound, but the possible formation of percolating particle network and the influence of matrix plasticisation led to the slight deviation of the experimental values from model predictions. A CTE peak appeared for all the composites with increasing temperature to about 250–300°C due to the action of matrix plasticisation filling the microvoids in the composites. The composites with mixed particles of substantially different sizes were prone to concentrate thermal stresses on large particles, which induced an early appearance of matrix plastic deformation that can result in a comparably low CTE peak temperature.     

机械合金化-放电等离子烧结Al2Cu颗粒增强Al基复合材料的制备

以Al粉和Cu粉为原料,采用机械合金化(MA)和放电等离子烧结(SPS)工艺,原位合成了致密的Al₂Cu/Al块体复合材料,着重研究了MA过程中粉末的形貌、尺寸和物相结构的变化以及SPS后复合材料的微观组织和力学性能。结果表明: 在MA过程中,随着MA时间延长,部分Cu原子逐渐固溶于Al原子晶格中,形成均匀过饱和的固溶体Al(Cu);在SPS过程中,Cu从过饱和固溶体中析出并与Al反应形成Al₂Cu颗粒,且弥散分布于Al基体中,形成Al₂Cu/Al复合材料;Al₂Cu/Al复合材料的致密度高达98.7%,室温下的压缩断裂强度为611.3 MPa,延伸率为9.6%,具有良好的力学性能。