Processing and Characterization of Fiber Reinforced Intermetallic Matrix Composites

A series of intermetallic matrix composites reinforced with Al₂O₃ based fibers were fabricated by pressure casting. The Al₂O₃ based fibers used were DuPont's 20 μm diameter Fiber FP and PRD-166 fiber, Mitsui's 10 μm diameter Almax fiber, and Saphikon's 125 μm diameter single crystal Al₂O₃ fiber. The intermetallic matrices employed were alloys based on Ni₃Al, NiAl, Fe₃Al, Ti₃Al+TiAl, and Nb₂Al+NbAl₃. Optical, scanning and transmission electron microscopy were used to investigate the microstructure of the composites and the fibers. Tensile testing was conducted to determine the Weibull mean strength of the fibers in the as-received and heat treated conditions. The effect of fiber gage length on the Weibull mean strength of the PRD-166 and Fiber FP was evaluated. Indentation tests were performed to determine the effect of alloying additions on the fiber/matrix bond strength in shear in Saphikon fiber reinforced Ni₃Al composites.     

Grain growth mechanisms in a spray-formed Ni3Al/Al2O3 composite in the presence of a liquid phase

Grain growth in the two-phase (liquid + solid) region of Ni₃Al reinforced with 0.8 vol.% Al₂O₃ participates synthesized by a spray atomization and co-injection technique was investigated. The grain growth of the as-sprayed and hot isostatically pressed (HIPed) materials in the two-phase region was found to be consistent with cube law kinetics, i.e., grain growth exponent was approximately 3. The activation energy for grain growth for the as-sprayed material was determined to be 308 ± 19 kJ mol⁻¹ while that of the HIPed material was calculated to be 327 ± 23 kJ mol⁻¹. The activation energy for grain growth was not a function of the amount of liquid phase or the composition of the liquid. Furthermore, the activation energy for grain growth was higher than that for diffusion through the liquid phase, suggesting that the mechanism for grain growth of the as-sprayed and HIPed Ni₃Al composite in the two-phase region was controlled by an interface reaction. The role of the second-phase Al₂O₃ particles on grain growth for the as-sprayed and HIPed Ni₃Al materials was not significant.     

纤维预热温度对连续Al2O3f/Al复合材料力学性能的影响

选用Nextel610型Al₂O₃纤维为增强体、ZL210A连续氧化铝合金为基体,采用真空压力浸渗法制备纤维增强铝基复合材料(Al₂O_3f/Al),纤维的体积分数为40%,预热温度分别为500、530、560和600℃,研究了纤维预热温度对Al₂O_3f/Al复合材料的微观组织、纤维损伤和力学性能的影响。结果表明：随着纤维预热温度的提高复合材料的致密度随之提高,最大达到99.2%,材料的组织缺陷最少,纤维的分布均匀;随着纤维预热温度的提高从复合材料中萃取出来的Al₂O₃纤维的拉伸强度不断降低,纤维预热温度为600℃的复合材料中Al₂O₃纤维的拉伸强度仅为1150 MPa,纤维表面粗糙,有大尺寸附着物。纤维的预热温度对Al₂O_3f/Al复合材料的拉伸强度有显著的影响。预热温度为500、530、560和600℃的复合材料其拉伸强度分别对应于298、465、498和452 MPa。组织缺陷、纤维损伤和界面结合强度,是影响连续Al₂O_3f/Al复合材料强度的主要因素。     

Processing and Heat Treatment Effects on an Al2O3/Ni3Al Composite

Various processing routes may be used to fabricate Ni₃Al matrix composites. In the present study, vacuum hot pressing and hot extrusion were used to fabricate an Al₂O₃ Composite particulate-reinforced Ni3Al composite. Relatively low extrusion temperatures promoted gamma-phase formation as did extended high temperature anneals. The room-temperature bend strength was found to increase as the gamma-phase content increased. Furthermore, the composite creep rate was affected by the. processing parameters and their effect on the amount of gamma/pgamma-prime interface. The matrix and particulates did not exhibit any reaction after normal processing. However, a minor reaction was noted after annealing near 1000°C, while extensive reaction resulting in Ni-Al spinel formation occurred above 1200°C in air     

光悬浮区熔定向凝固Al2O3/Er3Al5O12和Al2O3/Yb3Al5O12共晶陶瓷的制备与性能研究

本研究探索了光悬浮区熔法制备Al₂O₃/Er₃Al₅O₁₂(ErAG)和Al₂O₃/Yb₃Al₅O₁₂(YbAG) 定向凝固共晶陶瓷。在10 mm/h的抽拉速率下成功获得了凝固组织均匀、内部无裂纹或孔洞的高质量共晶陶瓷。通过高分辨三维X射线衍射仪研究了Al₂O₃和RE₃Al₅O₁₂在三维空间的分布与组织结构; 利用电子背散射衍射技术分析了定向凝固末期Al₂O₃和RE₃Al₅O₁₂两相的晶体学择优取向和相界面关系。力学性能表征结果显示, Al₂O₃/ErAG和Al₂O₃/YbAG具有优异的力学性能, 二者的维氏硬度分别为(13.5±0.4)和(12.8±0.1) GPa;断裂韧性分别为(3.0±0.2)和(3.2±0.1) MPa·m^1/2。     

Growth of copper and vanadium on a thin Al2O3-film on Ni3Al(111)

The growth of different metals on thin Al₂O₃-films on Ni₃Al(111) was investigated using scanning tunneling microscopy (STM). These thin alumna films are well ordered showing two superstructures, which appear in the STM images at different bias voltages. These superstructures, with periodicities of 2.6 and 4.5 nm, respectively, are shown here to govern the nucleation of the deposited metals. Copper clusters grow on these nucleation centers only at room temperature. Higher temperatures lead to an increase of the cluster size and the loss of order. In turn, vanadium forms ordered cluster arrays at room and higher temperature. Due to the stronger metal–oxide interaction compared to copper vanadium forms smaller clusters at low and high coverages, which do not show any ripening after annealing. Based on these observations, Al₂O₃-films on Ni₃Al(111) prove to be an interesting template for the fabrication of periodic cluster arrays.     

Effect of volume fraction of carbon fibers on wear behavior of Al/Al2O3/C hybrid metal matrix composites

Wear behavior of Al/Al₂O₃/C hybrid metal matrix composites fabricated by squeeze casting method was characterized. The effects of volume fraction of carbon fiber on wear behavior of hybrid composites was investigated. Wear behavior of Al/Al₂O₃/C composites was characterized by the dry spindle wear test under various sliding speeds.

The wear resistance of Al/Al₂O₃/C composites was remarkably improved over Al/Al₂O₃ composites by adding carbon fibers to Al/Al₂O₃/C composites. Specifically, at the intermediate sliding speed the wear resistance of Al/Al₂O₃/C composites containing 8 vol.% carbon fiber was found to be better than that of the rest of the carbon hybrid composites. From fractographic studies, damaged sections in wear surfaces of hybrid composites at intermediate sliding speed were not observed due to the formation of solid lubrication film. The solid lubrication film which was formed as a result of adding carbon fibers improved the wear resistance of carbon hybrid composites because this film reduced the high friction force between MMCs and counter material.     

Characterization of intermetallic phases and oxides formed in annealed Ni/Al multilayer structures

Two different multilayer structures composed of ten alternating Ni and Al thin films were sputter deposited on Si (111) substrates. These multilayers with individual Ni and Al thin film thicknesses of about 25 nm and 38 nm and of 25 nm and 13 nm, respectively, have the average compositions of Ni_0.50Al_0.50 and Ni_0.75Al_0.25. The samples were heat treated in a differential scanning calorimeter instrument with a constant heating rate of 40 °C min ⁻¹ in Ar from room temperature to 550 °C. The compositions of as-deposited and heat-treated samples were studied with high-resolution Auger electron spectroscopy (AES) rotational depth profiling. X-ray photoelectron spectroscopy (XPS) analyses show an excess of Ni in both annealed samples. X-ray diffraction measurements of annealed multilayers show the formation of Ni₂Al₃ and NiAl₃ phases in the Ni_0.50Al_0.50 sample and the presence of Ni₃Al and Ni A1₃ phases with some excess of Ni in the Ni_0.75Al_0.75 sample. AES and XPS investigations of the reacted layers after 15 min annealing in air at 500 °C disclose considerably different surface oxide thin films: on the Ni_0.50Al_0.50 layer the oxide thin film consists of Al₂O₃ with a small amount of NiO, whereas that on the top of the Ni_0.75Al_0.25 layer is thicker and consists of NiO on top and some Al₂O₃ below.     

Al2O3/BaZrO3双陶瓷界面微观组织演化及机理

以Al₂O₃为背层(硅溶胶为粘结剂), 电熔BaZrO₃作为面层材料(钇溶胶为粘结剂), 1550℃烧结后制成50 mm×25 mm×5 mm的Al₂O₃/BaZrO₃双陶瓷试样。通过光学显微镜(OM)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)和EDS等手段观察了BaZrO₃层和Al₂O₃/BaZrO₃界面的显微结构, 研究了BaZrO₃与Al₂O₃的界面反应。结果表明, 面层由BaZrO₃基体和分布其上的大小10 μm左右的Y稳定的ZrO₂晶粒组成; Al₂O₃/BaZrO₃界面发生反应形成厚约300 μm的过渡层, 界面反应生成物有BaOAl₂O₃、ZrO₂和BaO·Al₂O₃·2SiO₂。界面从单纯的BaZrO₃/Al₂O₃双陶瓷结构演变为BaZrO₃、ZrO₂、BaO·Al₂O₃、BaO·Al₂O₃·2SiO₂和Al₂O₃等多种物相组成的复杂结构。反应过程中Al元素基本不迁移扩散, BaZrO₃中Ba元素向Al₂O₃所在的位置扩散形成BaO·Al₂O₃, 残留物形成一层条状ZrO₂, 而BaO·Al₂O₃·2SiO₂围绕着EC95(Al₂O₃+5%SiO₂)粉体颗粒周围生成。     

激光铝热还原法制备Al2O3/Ti-Al基复合涂层

利用Al和TiO₂之间的放热化学反应, 采用激光原位合成技术在TC4钛合金基体材料表面制备了Al₂O₃/Ti-Al金属间化合物基复合涂层。对比分析了激光功率、激光束扫描速度和光斑尺寸变化对激光能量密度变化量的影响程度, 借助X射线衍射仪(XRD)、光学显微镜(OM)、能谱仪(EDS)和显微硬度计分别考察了激光束扫描速度对复合涂层表面宏观形貌、截面显微组织结构和显微硬度的影响。结果显示, 扫描速度的变化对激光能量密度变化量的影响程度最大, 光斑尺寸次之, 激光功率的变化影响最弱。随着激光束扫描速度的增大, 复合涂层表面渐趋粗糙, “鱼鳞纹”状形貌特征趋于明显, 复合涂层与基材结合区厚度减小。激光原位复合涂层主要由k-Al₂O₃和α-Al₂O₃增强相与α-Ti和α₂-Ti₃Al基体相组成。随着激光束扫描速度增大, 复合涂层内k-Al₂O₃部分转变为α-Al₂O₃, Al₂O₃增强相有由枝晶状向纤维状转变的趋势; 复合涂层截面显微硬度自基体至涂层表面过度平缓, 且涂层区显微硬度分布均匀, 明显高于基材平均显微硬度。     

Al2O3保护层对高温下Pt/ZnO/Al2O3电极导电稳定性的影响

本工作研究了Al₂O₃保护层的厚度对高温下声表面波器件电极导电稳定性的影响, 采用激光分子束外延方法在Pt/ZnO/Al₂O₃电极上制备了不同厚度的Al₂O₃保护层。通过测量样品高温环境中的实时电阻, 发现Al₂O₃缓冲层的厚度对电极在高温下的导电稳定性的影响非常大。结果表明, 没有Al₂O₃保护层时, Pt/ZnO/Al₂O₃电极的电阻升温至800 ℃时开始急剧地增加。当包覆40 nm的Al₂O₃保护层时, 电极在升温至900 ℃以上才出现电阻值剧烈增加的现象。而随着Al₂O₃保护层厚度的增加, 电极的电阻在高温下的导电性能也更加稳定。SEM测试结果表明, 经过1000 ℃、1 h的高温测试后, Al₂O₃保护层越薄的Pt/ZnO/Al₂O₃电极, 结块形成的Pt颗粒越大与不连续的Pt空洞更多。这些结果为制备高温下稳定工作的声表面波器件提供了一条新的思路。     

Microstructures, densification and mechanical properties of TiC–Al2O3–Al composite by field-activated combustion synthesis

Dense TiC–Al₂O₃–Al composite was prepared with Al, C and TiO₂ powders by means of electric field-activated combustion synthesis and infiltration of the molten metal (here Al) into the synthesized TiC–Al₂O₃ ceramic. An external electric field can effectively improve the adiabatic combustion temperature of the reactive system and overcome the thermodynamic limitation of reaction with x < 10 mol. Thereby, it can induce a self-sustaining combustion synthesis process. During the formation of Al₂O₃–TiC–Al composite, Al is molten first, and reacted with TiO₂ to form Al₂O₃, followed by the formation of TiC through the reaction between the displaced Ti and C. Highly dense TiC–Al₂O₃–Al with relative density of up to 92.5% was directly fabricated with the application of a 14 mol excess Al content and a 25 V cm⁻¹ field strength, in which TiC and Al₂O₃ particles possess fine-structured sizes of 0.2–1.0 μm, with uniform distribution in metal Al. The hardness, bending strength and fracture toughness of the synthesized TiC–Al₂O₃–Al composite are 56.5 GPa, 531 MPa and 10.96 MPa m^1/2, respectively.     

Ni2O3对C3S形成过程的影响及其固溶效应

C3S是水泥熟料中最重要的矿物,杂质离子固溶进入C3S晶格并促进其单斜型或三方型稳定存在,研究离子在C3S中的固溶作用机理,能更深入了解阿利特的微结构及性质。利用化学分析、XRD、DTA及相图分析,研究Ni2O3对C3S形成过程的影响及其固化效应。结果表明:Ni2O3主要以+2价的形式在CaO-Si O2二元体系中存在,因其优先与Si O2反应形成固溶体,f-CaO随Ni2O3掺量递增而增大;当Ni2O3掺量大于其CaO-Si O2二元体系固溶极限时,f-CaO变化趋势呈相反趋势,且促进C3S形成效应明显。通过最小二乘法及Ni2O3固溶度的精确界定,可推导出Ni2O3在C3S中的固溶反应分子式为:(Ca3-0.53xNi0.53x)(Si1-0.47xNi0.47x)O5(x=0.0442)。     

纳米Al_2O_3/聚酰亚胺复合薄膜的介电与力学性能

采用原位聚合与热亚胺化的方法,成功制备了一系列不同纳米Al_2O_3粒子质量分数的纳米Al_2O_3/聚酰亚胺(PI)复合薄膜。通过SEM、TEM、XRD、FTIR、LCR数字电桥、高压电源及电子万能材料试验机对纳米Al_2O_3/PI复合薄膜的微观结构、介电性能及力学性能进行了表征和测试。结果表明:纳米Al_2O_3粒子在均匀地分散在PI基体中;当纳米Al_2O_3粒子质量分数为8%时,纳米Al_2O_3/PI复合薄膜的击穿强度和拉伸强度均达到了最大值;纳米Al_2O_3/PI复合薄膜的介电常数随纳米Al_2O_3质量分数的增加而增加。     

热处理对Ni-P-A12O3化学复合镀层摩擦磨损性能的影响

热处理可显著提高镀层的硬度和耐磨性能。采用化学镀的方法在45钢表面制备了Ni-P-纳米A12O3复合镀层,并以不同温度对其热处理,研究了镀层热处理前后的物相、硬度和耐磨性能。结果表明：400℃热处理后,Ni-P-A12O3复合镀层达到稳态,稳定相是Ni＋Ni3P＋NiO＋A12O3;镀层的显微硬度随热处理温度的升高而先...     

纳米Al_2O_3分布对Al_2O_3/PE-EVA复合材料导热性能与力学性能的影响

旨在将纳米Al2O3分散在聚乙烯(PE)和乙烯醋酸乙烯共聚物(EVA)的共混物中,构建具有选择性分布结构的局域高粒子浓度导热复合材料。采用纳米Al2O3为导热填料,以PE和EVA为基体树脂,使用熔融共混法制备了Al2O3/PE-EVA导热复合材料。利用选择性溶液萃取方法和SEM研究了PE-EVA共混物的相结构及纳米Al2O3在共混物中的分布,评价了Al2O3/PE-EVA复合材料的导热性能与力学性能。结果表明:在PE与EVA质量比为1∶1时可获得具有两相共连续结构的共混物;在两相共连续PE-EVA共混物中引入纳米Al2O3后,发现纳米Al2O3主要分布在PE相中;纳米Al2O3的分布行为及共连续结构的形成有助于提高复合材料的导热性能,在纳米Al2O3质量分数为50%时,与Al2O3/PE复合材料相比,具有选择分布和相连续结构的Al2O3/PEEVA复合材料的热导率提高了21.2%;随着纳米Al2O3质量分数的增加,Al2O3/PE-EVA复合材料的拉伸强度与Al2O3/PE复合材料的拉伸强度相近,同时由于EVA相的增韧作用,其断裂伸长率优于Al2O3/PE复合材料。     

烧结应力的缓冲及Al2O3/不锈钢微滤膜的制备

以多孔不锈钢片为基体、以氧化铝粉体(平均粒径0.5 μm)为膜材料, 用三种工艺制备了Al₂O₃/不锈钢微滤膜。采用扫描电子显微镜和金相显微镜分别对样品表面和断面形貌进行了表征, 用毛细流动法测定了Al₂O₃/不锈钢膜的孔径分布, 并通过超声震荡法考察了膜的附着力。研究表明, 在基体与氧化铝涂层间预洗引入一层不锈钢细粉作为过渡层再进行共烧结,有效地解决了Al₂O₃膜层易于剥落的问题, 并成功制备了Al₂O₃/不锈钢复合微滤膜, 膜厚为40~50 μm。该不锈钢粉末过渡层不仅可以修饰基体表面, 还能够缓冲Al₂O₃层在热处理过程中产生的热膨胀和烧结收缩应力, 并对Al₂O₃层和不锈钢基体产生粘结作用, 提高了膜的附着力。本工作所采用的共烧结法既简化了制备工艺, 又节约了能源。共烧结温度是影响膜附着力与孔径分布的关键因素, 经1100、1150、1200和1250℃共烧结, 所制备的Al₂O₃/不锈钢膜平均孔径为0.2、0.3、0.5和3.9 μm, 其纯水通量分别为3.8、4.1、6.9和20.5 m³/(m²·h·bar)。     

Ti添加对WC-Ni3Al硬质合金微观组织与力学性能的影响

为提高WC-Ni₃Al硬质合金的力学性能，采用放电等离子烧结制备Ti掺杂的WC-Ni₃Al硬质合金，并研究不同Ti添加量对WC-Ni₃Al硬质合金微观组织和力学性能的影响。结果表明: Ti的添加减小WC-Ni₃Al块体样品中反应生成的少量Al₂O₃的尺寸，并且使Al₂O₃的分布更加均匀。一方面，小尺寸的Al₂O₃与原位生成的(Ti, W)C协同提高WC-Ni₃Al块体样品的硬度；另一方面，适量Ti的添加还提高WC-Ni₃Al硬质合金的断裂韧度，这是由于原位生成的(Ti, W)C与WC有较好的界面结合，增加对裂纹扩展的桥接与偏转作用。当添加3%(质量分数)的Ti时，WC-Ni₃Al硬质合金获得了优异的力学性能，硬度和断裂韧度分别为(19.29±0.18) GPa和(13.14±0.24) MPa·m^1/2。     

Nickel Enriched Diffusion Layers on a NiAl Alloy

The intermetallic phase NiAl is a perspective material for high-temperature and shape memory effect applications. Formation of Ni₅Al₃, Ni₂Al, Ni₃Al phases which influence the extent of martensitic transformation in NiAl have been studied up to now with controversial results. We have investigated (using SEM and local elemental analyses) the microstructure of nickel enriched surface layers on a Al-79 wt.% Ni alloy. The layers were prepared by diffusion annealing and subsequently given two different heat treatments: at 930°C outside the Ni₅Al₃ region and at 500°C within the Ni₅Al₃ region of the phase diagram. In the specimen which was only diffusion annealed separate islands of Ni₅Al₃ phase elongated in the direction of the concentration gradient could be recognized within the nickel enriched surface layer. In the samples additionally annealed at 500°C, a well defined continuous layer of the Ni₅Al₃ phase situated 0.4 mm below the specimen surface was found. In the samples annealed at 930°C, isolated Ni₃Al precipitates were observed. Their number and size gradually increased with increasing nickel content.     

低温燃烧法制备(W,Mo)C/Al2O3/La2O3复合粉末及性能

为了开发出一种无黏结相硬质合金来减少传统硬质合金中钴元素的应用,采用化学法制备(W,Mo)C/Al₂O₃/La₂O₃。以偏钨酸铵、钼酸铵、硝酸铝、硝酸镧、尿素和葡萄糖为原料,通过低温燃烧法探究硝酸盐和尿素、葡萄糖的不同配比,得出最优配比后还原炭化制备(W,Mo)C/Al₂O₃/La₂O₃粉末。在1500~1800℃经离子烧结制备(W,Mo)C/Al₂O₃/La₂O₃无黏结相材料,研究其力学性能并分析强韧化机制。结果表明:硝酸盐和尿素的最佳摩尔配比为1∶2,硝酸盐和葡萄糖的最佳摩尔配比为1∶0.5,加入葡萄糖后颗粒尺寸减小了0.28μm,比表面积提高了75.64%。致密度、维氏硬度和抗弯强度在1600℃时达到最大值分别为:98.45%,2202HV和1203 MPa,断裂韧度在1500℃时达到最大值为7.52 MPa·m^1/2。由于晶粒的细化及第二相颗粒的增韧的影响,(W,Mo)C/Al₂O₃/La₂O₃在1500~1600℃时以沿晶断裂和穿晶断裂为主;晶粒长大以及孔隙的出现导致(W,Mo)C/Al₂O₃/La₂O₃在1700~1800℃时以沿晶断裂为主。