Synthesis and mechanical properties of niobium aluminide-based composites

Niobium aluminide-based composites reinforced with in situ and externally added Al₂O₃ and TiC particulates were fabricated by hot-pressed sintering at 1400 °C. In particular, Nb₂Al–Al₂O₃–TiC in situ composites were successfully obtained from the raw powder mixtures of Nb60Al40 (in at.%)–TiO₂20C8 (in wt.%) by means of this process. The influences of ceramic particulates on the microstructures, flexural strength and fracture toughness were examined. The experimental results indicate that the presence of ceramic particulates yielded a remarkable improvement in both the strength and fracture toughness in comparison with previous results for monolithic niobium aluminide compounds.     

Characterization of A12O3, A12O3 + TiO2 Powder Mixture, and Coatings Prepared by Plasma Spraying

A1₂O₃ and its mixture with 3 wt% Ti0₂ powders were prepared by fusion and crushing methods. Al₂O₃ + 13 wt% TiO₂ and A1₂O₃ + 40 wt% TiO₂ powders were mixtures of fused AI₂O₃ + 3 wt% TiO₂ and 10 wt% and 37 wt% of TiO₂respectively. Chemical analysis of the powders showed that: approximately 1 wt% of impurities were present in each powder. True and tap densities were measured and are discussed for all powders. Powder size study showed narrow range of distribution of particle size in each powder. SEM study showed that the particles were in round and other irregular shapes in all the powders. A1₂O₃ was found to be in alpha phase and TiO₂ in rutile phase. All the powders were coated by plasma spraying at 16 kW. The density of the coatings were measured and are discussed. In the coatings, A1₂O₃ was in both alpha and gamma phases. In A1₂O₃ + 13 wt% TiO₂ and A1₂O₃ + 40 wt% TiO₂ coatings, the oxygen reduction from TiO₂ was observed.     

基于薄膜技术制备超细片状氧化铝的研究

结合薄膜涂布技术,在超声波的作用下,利用溶胶-熔盐复合工艺制备超细片状氧化铝。以硫酸铝钾和氯化钾混合溶液中的KAl (SO₄)₂·12H₂O为铝源,KCl为熔盐,加入Na₂CO₃溶液,经超声处理,制成铝溶胶,并将溶胶涂布在水溶性树脂基底上。洗脱后的片状氢氧化铝经高温煅烧,成为厚度均一、表面光滑的超细片状氧化铝。研究熔盐比例,添加剂种类和含量,超声波处理时间对粉体形貌的影响。扫描电镜及X射线衍射分析结果表明:铝源与熔盐比例为1∶4,添加剂为TiO₂及含量为2%,超声处理时间为30 min,1200℃高温煅烧条件下得到形貌规则,表面光滑,粒径在10μm以下,径厚比10左右的超细六角片状ɑ-氧化铝。     

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.     

Study of the densification of a nanostructured composite powder: Part 1: Effect of compaction pressure and reinforcement addition

Al/Al₂O₃ composite coating was prepared by plasma spraying and characterized by XRD and SEM. Some thermal–mechanical properties of the composite coating including thermal diffusivity, microhardness, fracture toughness and sliding wear rate were measured. The results showed that the Al/Al₂O₃ composite coating, compared with Al₂O₃ coating, exhibits denser structure and developed splat interface. The coexistence of Al metal phase and Al₂O₃ ceramic phase effectively increased the fracture toughness and thermal diffusivity of composite coating, in spite of the slight decrease in microhardness. Furthermore, the wear resistance of Al/Al₂O₃ composite coating is superior to that of Al₂O₃ coating.     

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基多孔隔热材料表面Al2O3/MoSi2涂层的制备及其性能

采用刷涂法在Al₂O₃基多孔隔热材料表面制备Al₂O₃/MoSi₂涂层,涂层以硅溶胶作为粘结剂,纳米Al₂O₃与Al₂O₃纤维作为耐高温组分,MoSi₂为高发射率组分。通过SEM、XRD对Al₂O₃/MoSi₂涂层微观表面结构、物相组成进行分析。研究纳米Al₂O₃与Al₂O₃纤维的质量比和MoSi₂含量对Al₂O₃/MoSi₂涂层耐温性能的影响,并对Al₂O₃/MoSi₂涂层的抗热震性能、发射率进行表征。结果表明,当纳米Al₂O₃与Al₂O₃纤维的质量比小于1∶1时,热考核后Al₂O₃/MoSi₂涂层表面无裂纹产生;当纳米Al₂O₃与Al₂O₃纤维的质量比在1∶2~1∶4之间时,Al₂O₃/MoSi₂涂层中的纤维网络较完整。MoSi₂的含量为20%时,Al₂O₃/MoSi₂涂层抗热震实验循环25次后表面保持完好,热考核后在2.5~25 μm波段的平均发射率在0.85左右,具有较高的发射率。      

超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料

以1Cr18Ni9Ti、Ti-6Al-4V为金属基底,通过在B4C+Ti体系中引入CrO_3+Al铝热剂,调整反应体系绝热温度依次为3 193、3 282、3 290及3 473K,采用超重力场反应连接制备TiB_2-TiC/1Cr18Ni9Ti和TiB_2-TiC/Ti-6Al-4V梯度复合材料,发现随着反应绝热温度升高,陶瓷/金属界面区厚度不仅因金属熔深增加而增大,并且残存于界面上的Al_2O_3夹杂也随之增多。分别对B4C+Al体系与CrO_3+Al铝热剂进行配制、球磨活化、压制成坯并依次填料入坩埚后,发现残存于界面上的Al_2O_3夹杂完全消除,同时发现在TiB_2-TiC/1Cr18Ni9Ti界面上生成三维网络陶瓷/金属梯度复合结构,而在TiB_2-TiC/Ti-6Al-4V界面上形成跨尺度多层次梯度复合结构。     

Characterization and properties of r.f.-sputtered thin films of the alumina–titania system

Thin films of the aluminum oxide (Al₂O₃)–titanium oxide (TiO₂) system including Al₂O₃, TiO₂, and Al₂O₃/TiO₂ were prepared by radio-frequency (r.f.) magnetron sputtering using ceramic targets of Al₂O₃, TiO₂, and Al₂O₃/TiO₂ composites with different Al₂O₃/TiO₂ ratio. These films were studied at different substrate temperatures, r.f. powers, and annealing temperatures. Composition, microstructure, thermomechanical property of internal stress, and mechanical property of scratch adhesion, were evaluated. A thin film with a dielectric constant of 62 and a loss tangent of 0.012 was obtained at 500 °C from a 10/90 target. This thin film remained the high dielectric constant of TiO₂, but had an improvement in the dielectric loss tangent. Al₂O₃-containing films had a higher resistivity and breakdown field, which was improved further by annealing. Optical properties, such as refractive index and optical transmittance, were also investigated.     

Processing, microstructure and properties of C40 Mo(Si,Al)2/Al2O3 composites

The C40 Mo(Si_0.75Al_0.25)₂/Al₂O₃ composites were prepared by spark plasma sintering (SPS) of mechanically alloyed (MA) powders. The Mo(Si_0.75Al_0.25)₂/0–20 vol.% Al₂O₃ materials, showing micron and submicron composite structure, possess a hardness of 13.9–14.6 GPa but a poor toughness of 1.78–1.80 MPa m^1/2. The addition of 30 vol.% Al₂O₃ leads to the formation of the micron C40 Mo(Si_0.75Al_0.25)₂/Al₂O₃ composite with an intergranular distribution of Al₂O₃, that results in a drop of the hardness to 10.2 GPa and an improvement of the toughness to 3.67 MPa m^1/2. The transition of the cleavage facets to the intergranular fracture with the addition of Al₂O₃ is assumed as the main toughening mechanism.     

Al-TiO2-B2O3-C系XD合成铝基复合材料的反应机理及力学性能

研究了Al-TiO2-B2O3-C反应系XD合成铝基复合材料的反应机理.结果表明在Al-TiO2-B2O3-C系中,当B2O3/TiO2摩尔比=0.5,C/TiO2摩尔比=0时,TiO2和B2O3分别与Al结合生成热力学稳定的Al2O3和活性Ti原子、B原子,B原子和Ti原子分别穿过各自反应层结合生成热力学稳定的TiB2,过剩的Ti原子则与Al结合生成棒状物Al3Ti;加入碳粉后,Ti原子将优先与C和C与Al的化合物Al4C3反应生成TiC,Al3Ti逐渐减少,在C/TiO2摩尔比为0.5时,Al3Ti相基本消失,力学性能得到改善,其拉伸强度和延伸率分别从266MPa和3%增加到315MPa和7%.     

ZrO_2增韧Al_2O_3陶瓷的力学性能和增韧机制

对通过热压烧结法制备的3种陶瓷99.5vol%Al2O3(AD995)、ZrO2(15vol%)/Al2O3和ZrO2(25vol%)/Al2O3的力学性能和增韧机制进行了实验和理论研究。基于复合材料细观力学理论并考虑ZrO2的相变特性,建立了描述ZrO2/Al2O3陶瓷力学性能的本构模型。结果表明:ZrO2的加入细化了基体Al2O3晶粒,ZrO2/Al2O3陶瓷的致密性得到提高;3种陶瓷试件的破坏呈现小变形到脆性破坏的特点,压缩加载下试件应力-应变曲线近似为线性关系;AD995陶瓷的断裂韧性为5.65 MPa·m1/2,ZrO2(25vol%)/Al2O3陶瓷的断裂韧性为8.42 MPa·m1/2,提高了近50%;随ZrO2增韧相含量的增加,ZrO2/Al2O3陶瓷的弹性模量降低而断裂韧性增加,这一变化趋势与实验结果有良好的一致性。     

Effects of TiO2/Al ratio on microstructures and mechanical properties of TiAl base composites

Effects of TiO₂/Al ratio on the microstructures and mechanical properties of in situ Al₂O₃/TiAl based composites were investigated. The results indicate that the as-sintered products consist of grains of nearly lamellar α₂ + γ structure with a dispersion of randomly oriented Al₂O₃ particles. A 43.9Ti-38.6Al-17.5TiO₂-nNb₂O₅ system was compared to 57.46Ti-36.78Al-5.76TiO₂-nNb₂O₅ system. The lamellar spacing of the products increases and the α₂ phase volume decreases with decreasing TiO₂/Al ratio. For each system, as the volume of α₂ phase increases, the average lamellar spacing decreases. Strength increases with an increasing TiO₂/Al ratio due to the amount of α₂ phase. Al₂O₃ phase increases with increasing TiO₂/Al ratio. Toughness increases with decreasing TiO₂/Al ratio. When the Nb₂O₅ content is smaller than 6 wt.%, the lamellar spacing plays an important role in toughness than the Al₂O₃ content. When the Nb₂O₅ content is larger than 6 wt.%, the Al₂O₃ content exhibits significantly increases the values of toughness than lamellar spacing.     

高功率激光照明用Al2O3-YAG:Ce复相陶瓷荧光体的组分设计与性能优化

结合蓝色激光二极管和黄色荧光转换器制备的固态激光照明引起了人们极大的关注, 但荧光转换材料的热猝灭效应显著影响了高功率激光照明的实现。通过组分设计和性能优化可以提高荧光转换器的热导率和发光均匀性。本工作采用固相反应烧结技术制备了一系列不同Al₂O₃含量的Al₂O₃-YAG:Ce复相陶瓷荧光体, 研究了Al₂O₃含量对Al₂O₃-YAG:Ce陶瓷荧光体微观结构、相组成、光学性能和热学性能的影响。Al₂O₃-YAG:Ce陶瓷荧光体在800 nm处的总透过率随着Al₂O₃含量的增加(0→90%)而下降(82.6%→23.6%)。Al₂O₃-YAG:Ce陶瓷荧光体的激发和发射强度随Al₂O₃含量的增加先增大后减小。当Al₂O₃/Al₂O₃-YAG:Ce的质量比为70%时, 陶瓷荧光体在室温下的热导率高达25.7 W·m^-1·K^-1, 且表现出最高的发射强度。当采用功率密度为20 W·mm^-2的蓝光二极管泵浦 70% Al₂O₃-YAG:Ce复相陶瓷荧光体时, 可获得3724 lm的高光通量和239.4 lm·W^-1的高流明效率。此外, 当功率密度从1 W·mm^-2增大到20 W·mm^-2时, 流明效率仅下降10.5%, 光通量持续增加且未出现发光饱和。上述结果显示, Al₂O₃-YAG:Ce复相陶瓷荧光体具有良好的发光效率和热稳定性, 将在高功率激光照明中具有广阔的应用前景。     

Co对Ti45Al-8Nb-0.3Y合金组织结构和高温抗氧化性能的影响EI北大核心CSCD

采用真空电弧非自耗熔炼方法制备Ti45Al-8Nb-0.3Y-m Co(m=0,0.5,1,2,原子分数/%,下同)合金,研究合金的组织和高温抗氧化性能。结果表明:Co能够明显细化TiAl-Nb合金组织,但对合金中α_(2)+γ片层组织的形成具有较强烈的抑制作用,并且会促进富Co的B_(2)相析出。Ti45Al-8Nb-0.3Y-mCo合金在1000℃空气中氧化100 h后形成的氧化膜均主要由较为疏松的TiO_(2)和Al_(2)O_(3)混合组成,且TiAl-Nb-0.3Y合金的氧化增重随Co含量增加而增大,但氧化膜的抗剥落能力随Co含量增加而明显提高;添加Co能够在一定程度上降低氧化膜的内应力,对提高其抗剥落性能有益,但引起的粗大B_(2)相析出削弱了合金的高温抗氧化性能。     

Formation of MgAl2O4 in Al2O3-(Al-4wt.%Mg) composites

The Al₂O₃ particles are introduced into the Al-4wt.%Mg melt by the “vortex” method. After being cast, Al₂O₃-(Al-4wt.%Mg) composites are remelted at 700, 750, 800 and 850°C for different residence times to investigate the formation of MgAl₂O₄ (spinel).

The results show that MgAl₂O₄ is the unique interface of the Al₂O₃-(Al---Mg) composites held at 700–850°C. Fine MgAl₂O₄ crystals grow on the surface of the Al₂O₃ particle but, as the holding temperature and the residence time increase, some spinels will form themselves into pyramidal shape. The MgAl₂O₄ grows not only at the matrix-particle interface but also on the surface of the composite specimens. The formation reactions of interfacial MgAl₂O₄ are as follows: Mg(1) + 2Al(1) + 2O₂(g) = MgAl₂O₄(s)3Mg(1) + 4Al₂O₃(s) = 3MgAl₂O₄(s) + 2Al(1) Both of them are equally important.     

Ionic Conductivity and Mechanical Properties of Post-HIPed Cubic Zirconia/Alumina Composites

8 mol.% yttria-doped cubic zirconia (8Y-CSZ)/AI₂O₃ composites containing 0-30 vol.% Al₂O₃ particles were fabricated by sintering, followed by hot isostatic pressing (post-HIPing). All composites were densified to at least 99·5% of the theoretical density by post-HIPing. The bending strength of composites sintered at 1500°C in air was independent of A1₂O₃ content, but a significant improvement in the bending strength was achieved by the post-HIPing technique. The bending strength and the fracture toughness of the HIPed composites increased with increasing A1₂O₃ content. Ionic conductivity of the composites was evaluated and the total, lattice, and grain boundary conductivities slightly decreased with increasing A1₂O₃ content. The HIPed composites containing up to 20 vol.% A1₂0₃ appear to be suitable candidate materials as electrolyte for solid oxygen fuel cell.     

Effect of Al2O3 particles on mechanical properties of directionally solidified intermetallic Ti–46Al–2W–0.5Si alloy

The effect of Al₂O₃ particles on microhardness and room-temperature compression properties of directionally solidified (DS) intermetallic Ti–46Al–2W–0.5Si (at.%) alloy was studied. The ingots with various volume fractions of Al₂O₃ particles and mean ₂–₂ interlamellar spacings were prepared by directional solidification at constant growth rates ranging from 2.78×10⁻⁶ to 1.18×10⁻⁴ ms⁻¹ in alumina moulds. The ingots with constant volume fraction of Al₂O₃ particles and various mean interlamellar spacings were prepared by directional solidification at a growth rate of 1.18×10⁻⁴ ms⁻¹ and subsequent solution annealing followed by cooling at constant rates varying between 0.078 and 1.889 K s⁻¹. The mean ₂–₂ interlamellar spacing λ for both DS and heat-treated (HT) ingots decreased with increasing cooling rate according to the relationship λ∝ ^−0.46. In DS ingots, microhardness, ultimate compression strength, yield strength and plastic deformation to fracture increased with increasing cooling rate. In HT ingots, microhardness and yield strength increased and ultimate compression strength and plastic deformation to fracture decreased with increasing cooling rate. The yield stress increased with decreasing interlamellar spacing and increasing volume fraction of Al₂O₃ particles. A linear relationship between the Vickers microhardness and yield stress was found for both DS and HT ingots. A simple model including the effect of interlamellar spacing and increasing volume fraction of Al₂O₃ particles was proposed for the prediction of the yield stress.     

SiCW对反应烧结多孔Al2TiO5-SiCW 复合材料的影响

以γ-AlOOH、TiO₂和SiC_w为原料,通过反应烧结制备了多孔Al₂TiO₅-SiC_w复合材料,研究了SiC_w对Al₂TiO₅-SiC_w复合材料物相、微观组织结构、孔隙率和抗压强度的影响。结果表明: 反应产物中主要物相有Al₂TiO₅、Al₆Si₂O₁₃、TiC和SiO₂。由于晶须分解速度快,SiC_w可全部与TiO₂反应生成TiC和SiO₂。添加SiC_w,一方面显著细化了Al₂TiO₅基复合材料的微观组织,生成的细小规则的TiC晶粒和存在于Al₂TiO₅晶界处的Al₆Si₂O₁₃有利于抑制Al₂TiO₅晶粒长大,提高其抗压强度。另一方面,因为SiC_w改变了原料中颗粒之间的堆积方式,使孔径增大、孔隙率显著提高。生成的一定量的SiO₂对晶粒产生黏结,使得Al₂TiO₅基复合材料的孔洞骨架密实,提高了抗压强度,但当SiC_w加入量多时,由于出现较多的玻璃相,会降低抗压强度。     

SiC对反应烧结多孔Al2TiO5的物相及组织性能影响

本研究以γ-AlOOH、TiO₂和SiC为原料, 通过无压反应烧结制备了Al₂TiO₅多孔材料, 分析比较了SiC粒度和含量对合成产物的物相组成、显微组织、抗压强度、孔隙率和孔径分布的影响。结果表明: 反应产物的物相组成为Al₂TiO₅、Al₆Si2O₁₃、TiC、SiO₂和Al₂O₃, 还有少量未反应的TiO₂。SiC与TiO₂反应生成TiC和SiO₂, TiC颗粒弥散分布于多孔材料壁面或者骨架中, 而SiO₂进一步与γ-AlOOH分解出的Al2O3反应生成Al₆Si₂O₁₃晶须, 晶须交错分布于Al₂TiO₅颗粒之间或者孔洞中, 与TiC颗粒一起提高复合材料的抗压强度, 特别是采用小粒径SiC时, 对抗压强度的改善效果更加显著; 添加大粒径SiC后, 改变原有颗粒堆积状态, 可提高复合材料的孔隙率。但当SiC含量超过5wt%时, 因为生成较多低熔点的SiO₂, 部分填充于多孔材料的孔隙中, 部分则分布于Al₂TiO₅晶粒之间, 既减小孔隙率, 又降低晶粒间结合强度和试样的抗压强度。