Synthesis of in situ Al–TiB2 composites using stir cast route

When elemental Ti and B powders were added to molten Al at above 1000°C, fine in situ TiB₂ particulates were formed through Al–Ti–B exothermic reaction. By optimising the nucleation of TiB₂, the tensile and yield strengths of a synthesised Al–15V_f%TiB_s composite were twice that of matrix material. Modification of Al-matrix with 4.5 wt%Cu tripled the tensile and yield strengths at peak-aged condition. Owing to the co-presence of brittle Al₃Ti flakes with TiB₂ particles in the composites synthesised by the Al–Ti–B system, ductility was reduced to 68% and 84% in composites with Al- and Al–Cu matrices, respectively. When the (Ti + B) mixture was incorporated with 3 wt%C, TiB₂ and TiC reinforcing phases were simultaneously produced in the composite with Al–Cu matrix. Such an approach reduced Al₃Ti compound in the composite considerably. Although the presence of Cu in the composite was found to promote the formation of Al₃Ti, its effect on the fluidity caused the melt recovery to increase from 33% to 52%.     

The dispersion mechanism of TiB2 ceramic phase in molten aluminium and its alloys

Titanium diboride (TiB₂) ceramic particulates are dispersed in molten aluminium and its alloys for grain refining and for making cast metal–matrix composites. For producing cast MMC, the dispersion of the ceramic phase via in-situ aluminothermic reduction of K₂TiF₆ and KBF₄ flux mixture with molten aluminium and, via the addition of exogenously formed TiB₂ with the fluoride flux has been studied at 900°C. In this article, the aspects of interfacial energy that govern the dispersion and agglomeration of TiB₂ particulates are examined. The Gibbs-adsorption interface equation is particularly employed to define and to quantify the change in the surface energy as a function of the alloying element concentration and, consequently the effect of interfacial energy on the nucleation rate of TiB₂ formed via metallothermic reduction reaction and the size of the ceramic phase is also explained.     

多粒径TiB2颗粒增强铜基复合材料的制备与载流摩擦磨损性能

采用粉末冶金工艺分别制备了单一粒径TiB₂颗粒和多粒径TiB₂颗粒增强铜基复合材料,对比研究了非载流和载流条件下多粒径（2 μm+50 μm）TiB₂/Cu复合材料的摩擦磨损行为。微观组织观察表明:不同粒径的TiB₂颗粒在Cu基体中分布均匀。与单一粒径TiB₂/Cu复合材料相比,多粒径TiB₂/Cu复合材料具有更高的相对密度、硬度和导电率。摩擦磨损实验结果表明:多粒径TiB₂/Cu复合材料抗摩擦磨损性能明显高于单一粒径TiB₂/Cu复合材料,当2 μm与50 μmTiB₂颗粒配比为1:2时,多粒径TiB₂/Cu复合材料的抗摩擦磨损性能最佳。相对于2 μm单一粒径TiB₂/Cu复合材料,电流为0 A时,（2 μm+50 μm）TiB₂/Cu复合材料的摩擦系数和磨损率分别降低了17.3%和62.5%;电流为25 A时,（2 μm+50 μm）TiB₂/Cu复合材料的摩擦系数和磨损率分别降低了6%和45.8%,同时载流效率和载流稳定性得到明显提高,磨损表面更加平整。磨损机制分析表明:多粒径TiB₂颗粒合理配比有利于提高复合材料载流质量,同时摩擦过程中大粒径的TiB₂颗粒起到支撑作用,小粒径的TiB₂颗粒弥散强化Cu基体,二者的协同作用使TiB₂/Cu复合材料具有更好的抗载流摩擦磨损性能。      

SiC晶须对反应合成多孔TiB_2-TiC复合材料的影响

以Ti、B_4C和SiC晶须(SiC_w)为原料,采用自蔓延高温合成法制备了多孔TiB__2-TiC复合材料。讨论了SiC_w含量对TiB__2-TiC复合材料物相、组织形貌、孔隙率和抗压强度的影响。结果表明:不添加SiC_w时,复合材料中主要物相为贫硼相TiB和Ti_3B_4以及TiC和少量TiB__2;在5Ti+B_4C体系中加入SiC_w后,贫硼相TiB和Ti_3B_4逐渐减少直至消失,而出现富硼相TiB__2和TiC的含量增加。随着SiC_w含量的增加,复合材料的孔隙率逐渐增加,由38.46%增加至5_2.78%。当SiC_w含量小于1.0时,随着SiC_w含量的增加,多孔TiB_2-TiC复合材料的抗压强度明显增加,当SiC_w含量为1.0时,复合材料的抗压强度达到最大值56.04MPa。Ti与SiC_w反应会生成TiC、Ti_3SiC_2和TiSi_2等物相,消耗一定量的Ti,使得与B4C反应的Ti量减少,从而促进富硼相TiB_2形成和TiC的增多。并且在SiC_w表面形成颗粒状TiC或者层片状Ti_3SiC_2,增加SiC_w与TiB_2-TiC基体之间的结合,更有利于发挥SiC_w的强化作用。     

Improvements in mechanical properties of TiB2 ceramics tool materials by the dispersion of Al2O3 particles

TiB₂–Al₂O₃ composites with Ni–Mo as sintering aid have been fabricated by a hot-press technique at a lower temperature of 1530 °C for 1 h, and the mechanical properties and microstructure were investigated. The microstructure consists of dispersed Al₂O₃ particles in a fine-grained TiB₂ matrix. The addition of Al₂O₃ increases the fracture toughness up to 6.02 MPa m^1/2 at an amount of 40 vol.% Al₂O₃ and the flexural strength up to 913.86 MPa at an amount of 10 vol.% Al₂O₃. The improved flexural strength of the composites is a result of higher density than that of monolithic TiB₂. The increase of fracture toughness is a result of crack bridging by the metal grains on the boundaries, and crack deflection by weak grain boundaries due to the bad wetting characters between Ni–Mo and Al₂O₃.     

The CVD of Ceramic Protective Coatings on SiC Monofilaments for Use in Titanium Based Composites

TiB₂, TiC and TiN protective coatings have been deposited onto SiC monofilament fibers by the CVD technique using a cold-wall reactor at reduced pressure. The effect of deposition conditions on the morphology, microstructure, phase composition and adherence of the coatings were studied. The physical and chemical compatibility of these ceramic coatings with SiC filaments together with titanium-alloy matrices were assessed and compared. Dense and uniform TiB₂ coatings have been deposited successfully onto SiC monofilaments. The coating is stable on the SiC fiber and acts as an effective: barrier against the vigorous SiC/Ti-6Al-4V interfacial reaction. The adhesion of TiC on SiC fibers is comparatively weaker than the TiB₂ coating. There was no significant reaction found at the interface of TiC/Ti except at the interface of TiC/SiC. Examination of the TiN coatings showed severe cracking and spalling, hence TiN could not provide protection in a Ti-alloy matrix.     

C.V.D. Coating of Alumina Reinforcing Particles to Improve the Wear Resistance of H.S.S. Based Composites

C.V.D. coating of the reinforcing ceramic particles used in particulate metal matrix composites allows the control of reactivity at the particle/matrix interface. Wear resistant high speed steel-based composites containing uncoated A1₂0₃, uncoated TiC and C.V.D. coated A1₂0₃ were liquid phase sintered, then characterized using “pin-on-disc” wear testing. TiC or TiN C.V.D. coatings of A1₂0₃ were tested to determine die increase in reactivity of the particles with the liquid phases formed during sintering. This resulted in a porosity decrease at the particle/matrix interface in addition to a better ceramic/metal cohesion due to improved wettability. Reactivity and wettability were studied using differential thermal analysis, electron microprobe analysis, transmission electron microscopy, and image analysis. Results from pin-on-disc wear testing illustrated the role of the C.V.D. coating on the wear behavior of the studied materials. Lower wear rates were obtained with the composites containing TiC or TiN-coated Al₂0₃. These results showed that there is a relation between wettability of ceramic particles by the metallic phases and wear resistance of the composites.     

不同TiB2颗粒粒径的TiB2/Cu复合材料耐电弧侵蚀行为

采用放电等离子烧结法（SPS）制备了不同TiB₂颗粒粒径的3wt% TiB₂/Cu复合材料,研究了3wt% TiB₂/Cu复合材料致密度、导电率、硬度和耐电弧侵蚀性能随TiB₂颗粒粒径的变化规律,重点分析了不同TiB₂颗粒粒径的3wt% TiB₂/Cu复合材料耐电弧侵蚀行为。结果表明:3wt% TiB₂/Cu复合材料致密度和硬度随TiB₂颗粒粒径的增大而略有降低;TiB₂颗粒粒径越小,TiB₂/Cu复合材料的综合性能越好。随着TiB₂颗粒粒径的增大,3wt% TiB₂/Cu复合材料耐蚀稳定性降低,3wt% TiB₂/Cu阴极材料的损耗量明显增加;当TiB₂颗粒粒径为10 μm时,3wt% TiB₂/Cu复合材料的耐电弧侵蚀性能最佳。电弧蚀形貌观察表明:不同TiB₂颗粒粒径的3wt% TiB₂/Cu复合材料经电弧侵蚀后,3wt% TiB₂/Cu复合材料均由阴极向阳极发生转移;随着TiB₂颗粒粒径的增大,阴极质量损耗逐渐增加,触头表面电弧侵蚀面积增加;而在Cu基体中引入较小的TiB₂颗粒,有利于减弱电接触实验过程中TiB₂/Cu复合材料的喷溅现象。      

多粒径TiB2/Cu复合材料耐电弧侵蚀行为

采用粉末冶金工艺制备了不同配比的多粒径(2 μm+10 μm+50 μm) TiB₂/Cu复合材料。通过JF04C触点材料测试系统对多粒径TiB₂/Cu复合材料进行耐电弧侵蚀性能试验,研究(2 μm+10 μm+50 μm) TiB₂颗粒质量比分别为1∶1∶1、1∶1∶3、1∶3∶1、3∶1∶1时,TiB₂/Cu复合材料的耐电弧侵蚀性能及电弧侵蚀形貌变化规律,探究多粒径配比对TiB₂/Cu复合材料表层耐电弧侵蚀行为的影响。结果表明:当(2 μm+10 μm+50 μm) TiB₂颗粒质量比为1∶1∶1时,TiB₂/Cu复合材料相对密度和导电率最高,分别为99.1%和87.1%IACS。当(2 μm+10 μm+50 μm) TiB₂颗粒质量比为1∶1∶1和1∶3∶1时,TiB₂/Cu复合材料的组织均匀性较好,电弧侵蚀后材料损失相同,材料转移量最少。其中,质量比为1∶3∶1时,TiB₂/Cu复合材料平均燃弧能量最低,且燃弧时间和燃弧能量最稳定。研究表明,这与复合材料的综合物理性能密切相关。在颗粒增强Cu基复合材料设计过程中,引入合适配比的多粒径TiB₂颗粒有助于提高TiB₂/Cu复合材料的密度、导电率等综合物理性能。电弧侵蚀过程中,不同粒径的TiB₂颗粒相互协同作用,有助于提高TiB₂/Cu复合材料的耐电弧侵蚀性能和服役稳定性。      

不同粒径TiB2/Cu复合材料热传导模拟与实验

采用ANSYS对不同粒径TiB₂/Cu复合材料热传导过程进行模拟。采用粉末冶金法制备了不同粒径TiB₂增强的Cu复合材料,采用LINSEIS LFA1600激光导热仪测试了室温至280℃下的TiB₂/Cu复合材料热传导性能变化,并与模拟结果进行对比。结果表明:热导率模拟结果与实验结果吻合较好。在50~200℃之间,复合材料热导率变化不大,在6%~9%范围内波动。200℃之后,模拟值与实验值均呈现出随温度升高而增大的趋势,且吻合度较高。这是由于温度低于200℃时,在模拟过程中未考虑材料界面处两相不同热膨胀系数的影响,导致模拟值与实验值有较大的差异。当温度高于200℃时,模拟值和实验值吻合程度趋于稳定。在200℃时,由于两相热膨胀系数的影响,复合材料内部界面处等效应力大于Cu基体屈服强度,使其发生塑性变形,从而引起热导率发生较大幅度变化。此外,热导率随着TiB₂粒径的增大呈现出先提高后降低的趋势,在10 μm时达到最大。这是由于当颗粒直径小于临界平均直径时,颗粒直径的增大会减少界面数量,从而降低界面热阻。当颗粒直径大于临界平均直径时,平均自由程l的急剧增加导致热导率降低。      

放电等离子烧结Ni/TiB2-TiC复合材料微观组织及磨损性能

采用放电等离子烧结技术,以Ni、Ti、B₄C混合粉末为原料制备Ni/TiB₂-TiC复合材料,分析了Ni含量对复合材料的物相组成、组织结构、硬度和耐磨性的影响。结果表明：Ni/TiB₂-TiC复合材料主要物相为γ-Ni、TiB₂和TiC,其中TiB₂呈矩形条状和多边形状,TiC则呈现不规则块状;随着原始粉末中Ni含量的增加,TiB₂和TiC陶瓷相尺寸减小,其在Ni粘结相中的分布呈现出均匀化的趋势,复合材料更加致密。Ni含量显著影响Ni/TiB₂-TiC复合材料的耐磨性和磨损机制,Ni含量较低时（20wt%和30wt%）,复合材料摩擦系数（COF）较大且存在明显的波动,出现严重的疲劳磨损;随着Ni量的增加（40wt%）,材料的COF降低且趋于平稳,表现为微切削磨损;当Ni含量持续增加时（50wt%）,由于局部Ni的聚集导致粘着磨损产生,COF有所上升,耐磨性反而下降。     

Assessment of tensile behaviour of an Al–Mg alloy composite reinforced with NiAl and oxidized NiAl powder particles helped by nanoindentation

AA5056 matrix composites have been reinforced with as-received and oxidized NiAl particles and their nanohardness investigated as a function of distance to reinforcement. Results indicate that a non-heat treatable aluminium matrix, as is the present case, does not require that the intermetallic particles are surrounding by a protective Al₂O₃ layer to avoid reactions at matrix-reinforcement interfaces. On the other hand, the quality of the matrix-reinforcement bonding has been quantified by the reinforcement influence distance, defined as the distance from the particle at which the nanohardness of the matrix drops to its asymptotic value.     

等离子加热反应合成TiB2-TiC-Fe2Ti复合材料

以Ti、B₄C和Fe粉为原料,采用等离子束加热反应合成TiB₂-TiC-Fe₂Ti复合材料,分析了其物相、组织结构、显微硬度和断口形貌等。结果表明：反应生成物中物相主要有TiB₂、TiC和Fe₂Ti,同时含有少量的Fe₃C。各物相以不同的形态均匀分布,TiB₂呈现六边形和长条形,TiC近似球形,Fe₂Ti作为粘结相存在于TiB₂和TiC相之间,促进了各相之间的结合。等离子束加热具有高加热及冷却速率,降低了晶粒生长时间,有利于获得细小的组织。随着电流增加,单位时间内输入坯体热量增多,TiB₂和TiC充分长大,各相之间结合更加紧密。     

TiB2/Cu复合材料的电弧侵蚀行为

采用放电等离子烧结法（SPS）制备TiB₂质量分数为1wt%~5wt%的TiB₂/Cu复合材料,测试其导电率和硬度。当TiB₂质量分数由0增至5wt%时,复合材料的导电率由96.9%（International Annealed Copper Standard,IACS）降至65.1%（IACS）,布氏硬度由42.8增至65.2。对所制备的不同TiB₂质量分数的TiB₂/Cu复合材料在直流24 V、不同电流条件下进行电接触实验,探究TiB₂添加量和电流对TiB₂/Cu复合材料耐电弧侵蚀性能的影响。结果表明,TiB₂/Cu复合材料的平均燃弧时间、平均燃弧能量和材料损耗量随着电流的增加而增加,TiB₂/Cu复合材料的阴极损耗量高于阳极,整体上TiB₂/Cu复合材料由阴极向阳极转移。在24 V和25 A条件下,不同TiB₂质量分数的TiB₂/Cu复合材料的燃弧时间和燃弧能量随操作次数增加不断波动,整体上呈逐渐增加的趋势,3wt% TiB₂/Cu复合材料的稳定性最高,平均燃弧时间和燃弧能量最低。随着TiB₂质量分数的增加,TiB₂/Cu复合材料损耗量降低,表面蚀坑变浅。     

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.     

Mg对原位自生TiB2/Al-4.5Cu复合材料微观组织及力学性能的影响

采用Al-K₂TiF₆-KBF₄混合盐原位自生反应法,制备了不同Mg质量分数的3wt% TiB₂/Al-4.5Cu复合材料。采用SEM、TEM、HM硬度测试和室温拉伸等方法研究了Mg含量和多级热处理对3wt% TiB₂/Al-4.5Cu复合材料微观组织和力学性能的影响。微观组织观察发现:Mg质量分数为3wt%时,经过多级热处理后,TiB₂颗粒的团聚现象明显改善,反应生成的TiB₂颗粒平均尺寸约为130 nm,基体内伴随有大量弥散分布的纳米级颗粒,且α-Al的晶粒尺寸也明显减小。力学测试结果表明:多级热处理后,3wt% TiB₂/Al-4.5Cu复合材料的硬度和抗拉强度随Mg含量的增加而提高,但过量的Mg (≥4wt%)会造成TiB₂颗粒细化效果下降。分析表明:Mg的加入能够降低TiB₂/α-Al界面能,减少脆性相Al₃Ti、Al₂B的生成,并通过反应生成的MgAl₂O₄使界面结构变成TiB₂/MgAl₂O₄/α-Al,从而有效抑制了TiB₂的团聚,改善了TiB₂颗粒与Al液界面的润湿性,提高了形核率,进一步细化了α-Al晶粒尺寸。      

原位合成TiB2/Fe复合材料的高温氧化行为

采用微波烧结技术原位生成TiB₂/Fe复合材料,研究其在500℃、600℃与700℃空气中的恒温氧化行为,并对氧化膜的表面、截面形貌及相组成进行了分析。结果表明:TiB₂/Fe复合材料由TiB₂、Fe₂B和α-Fe三种物相组成。随着氧化温度的升高,TiB₂/Fe复合材料的氧化增重明显增大,均呈现抛物线型规律,在500℃时,其氧化产物主要为Fe₂O₃和Fe₃O₄,而700℃时,其氧化物为Fe₂O₃、TiO₂、Fe₉TiO₁₅及少量Fe₃BO₆组成。相同温度下,随着TiB₂含量增加,TiB₂/Fe复合材料氧化物粒径、氧化增重和氧化层厚度均减小,氧化激活能增大,其抗氧化性能也越好。      

CHEMICAL VAPOR DEPOSITION OF TiB2 FOR TiN-TiB2 LAMINAR COMPOSITES

TiB₂ is a material with very interesting properties with respect to erosion and corrosion resistance. Deposition on metallic substrates using TiCI₄, BBr₃ or BCI₃ and H₂ at temperatures around 900° C results in coronation of the substrate, which is most severe when using BBr₃. Therefore, a TiN diffusion barrier is applied. Here we discuss the deposition of TiB₂ using BCI₃ on molybdenum and TiN and compare the results with those of the thermodynamically more favorable reaction with BBr₃. Smooth TiB₂ layers are formed when using BCI₃, with faceting occurring above 900° C. The morphology seems to be independent of the BCI₃/TiCl₄ ratio in the gas phase for values between 0·5 and 4. With an excess of boron in the gas phase - BCI₃/TiCl₄ = 8, depletion occurs already at 800° C. An apparent activation energy of 210 KJ/mol has been determined for a stoichiometric gas phase with BCl₃/TiCI₄ = 2. When the supply of boron is limiting - BCl₃/TiCl₄ = 0·5, the activation energy is 120 KJ/mol.     

Processing and interfacial bonding strength of 2014 Al matrix composites reinforced with oxidized SiC particles

The SiC powder with a SiO₂ protective layer is used as the reinforcements for 2014 Al/SiC_p composites to suppress the reaction between the Al matrix and the SiC particle. 2014 Al/SiC_p composites were fabricated by vacuum hot pressing (VHP) and subsequent extrusion using 2014 Al powders and the SiC particles covered with a SiO₂ layer. The interfacial product was found to be Mg spinel (MgAl₂O₄) formed mainly by the chemical reactions of the SiO₂ layer covered on SiC particles with the Mg, Al in the 2014 Al alloy matrix. Also the interfacial bonding strength of the composites was investigated using push-out tests of SiC rods with the SiO₂ oxidation layer, which were processed within 2014 Al alloy.     

In-Situ Manufacturing of NiAl-TiC Composites with Three Dimensional (3D) Discrete Particular Network and Bi-Continuous Microstructures

NiAl-TiC intermetallic-ceramic composite system is a candidate for structural applications. Thus, in this research, near fully dense NiAl–xTiC composites [x?=?0, 28 and 48?vol fraction percent (vol.%)] were produced through in-situ manufacturing process using exothermic synthesis reactions of Al, Ni, Ti and C precursors and their consolidation via hot press apparatus. NiAl-28?vol.% TiC composite showed a simple three dimensional (3D) discrete networks of TiC particular fillers in the continuous polycrystalline monolithic NiAl intermetallic matrix as a thermal management strategy for elevated temperature applications while NiAl-48?vol.% TiC composite indicated interconnectivity of TiC particles in certain regions of NiAl matrix known as bi-continuous microstructure. Reasons for the higher mechanical properties of NiAl-28?vol.% TiC in comparison monolithic NiAl were also discussed.