树脂基多孔碳孔结构对Cf/SiC复合材料连接性能的影响

连接技术是实现大尺寸以及复杂构型C_f/SiC复合材料制备及工程化应用的关键技术。本工作使用酚醛树脂作为碳源, 通过反应连接法实现了C_f/SiC复合材料的稳定连接, 研究了多孔碳坯的体积密度和孔径对接头连接性能和微观结构的影响, 讨论了惰性填料含量对接头连接性能和显微组织的影响。研究表明: 树脂基多孔碳素坯的体积密度和孔径分别选定在0.71~0.90 g·cm^-3和200~600 nm比较合适, 随着多孔碳素坯孔径增加, 游离硅尺寸逐渐增大; 当孔径为190 nm时, 连接件强度最大为(125±12) MPa。添加SiC惰性填料可以明显减小多孔碳素坯的体积收缩, 当SiC惰性填料质量分数为50%时, 连接件强度最高达到(216±44) MPa, 基本与基体材料强度相当。总体而言, 本研究为实现C_f/SiC复合材料稳定连接提供了理论指导, 对实现复杂形状或大型C_f/SiC复合材料的制备和工程应用具有重要意义。     

混合酸(HNO3+HF)刻蚀法致霾汽车尾气过滤载体材料的设计与研究

以纺织加工过程中废弃的棉短绒为模板,经过溶胶法浸渍形成棉纤维/氧化硅复合体,再经常温树脂固化、低温真空碳化、高温碳热还原反应及液相渗硅等方式制备出SiC/Si复合材料,最后通过混合酸(HNO3+HF)循环氧化腐蚀制备出过滤汽车尾气陶瓷载体材料。扫描电镜(SEM)结果显示,多孔SiC具有不规则且相互连通的孔道结构,其微观形貌特征遗传于棉短绒和酚醛树脂制备的多孔碳;三点弯曲试验表明SiC/Si陶瓷复合材料的强度高达200MPa,多孔SiC的气孔率可达62%,混合酸腐蚀的多孔SiC的弯曲强度和断裂韧性均小于致密SiC/Si复合体,并提出了混合酸循环氧化-腐蚀机制解释游离态Si的腐蚀过程。     

凝胶注模成型制备纳米复合多孔氮化硅陶瓷

采用凝胶注模成型两步法烧结工艺,利用纳米碳粉增强,成功地制备出了具有高强度、结构比较均匀并有较高气孔率的氮化硅多孔陶瓷。借助X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱(EDS)、Archimedes法和三点弯曲法等方法对多孔氮化硅陶瓷的微观结构和基本力学性能进行了研究。结果表明:在适当工艺条件下可制成平均强度>100 MPa、气孔率>60%的多孔氮化硅陶瓷。SEM照片显示气孔是由长柱状β-Si₃N₄晶搭接而成的,气孔分布均匀。XRD图谱显示有SiC生成。发育良好的柱晶结构、均匀的气孔分布以及反应生成的SiC微晶是获得高性能的主要原因。      

烧结温度对SiC/莫来石复相多孔陶瓷的影响

以高岭土、SiC粉末、Al2O3粉末为主要原料,采用添加造孔剂法制备了SiC/莫来石复相多孔陶瓷,探讨了烧结温度对多孔陶瓷的气孔率、体积密度、抗折强度等的影响。分别采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)表征了样品的物相组成与断面形貌。结果表明,以淀粉为造孔剂,在1350℃下保温2h制备的样品综合性能最佳,其孔隙率为31.40%,抗折强度达到42.50MPa。     

C/C多孔体对C/C-SiC复合材料制备及性能的影响

以准三维针刺碳纤维预制体,经化学气相渗透(CVI)法制备了4种密度的C/C多孔体,利用先驱体浸渍裂解法(PIP)制备了C/C-SiC复合材料,研究了C/C多孔体对C/C-SiC复合材料制备和最终性能的影响。结果表明:C/C多孔体密度越低,最终得到的C/C-SiC复合材料开孔隙率及SiC含量较高。SiC的存在使C/C-SiC材料具有较高的弯曲强度,纤维和基体界面也是影响弯曲强度的关键因素,其中密度为1.35g/cm3的C/C多孔体所制备的C/C-SiC复合材料纤维和基体之间形成较好的结合界面,其弯曲强度最大。同时,SiC含量增加可显著提高C/C-SiC复合材料的抗烧蚀性能。     

二维碳/碳化硅复合材料与铌合金的连接

实现了二维C/SiC与Nb合金NbHf10-1M的可靠连接. 连接时将Ti-Cu核心中间层与Cu辅助中间层构成的叠层结构置于C/SiC与Nb合金之间, 并采用了固相扩散连接与瞬间液相扩散连接(Transient liquid phase-diffusion bonding, TLP-DB)相结合的连接方法. 结果表明: 辅助中间层厚度>0.72mm时, 可以有效缓解接头热应力. 核心中间层在TLP-DB过程中形成的液相对C/SiC具有良好浸润性, 可渗入C/SiC基体, 并包裹位于核心中间层与C/SiC界面区域的C纤维. 接头剪切强度最高为14.1MPa.     

SiC陶瓷与316L不锈钢真空活性钎焊北大核心CSCD

采用Ag-Cu-Ti活性钎料,通过真空钎焊方法进行了SiC陶瓷与316L不锈钢的连接,研究了接头的界面组织、特征点成分和物相,并探讨了钎焊温度(800～930℃)、保温时间(0～30 min)对接头界面组织和连接强度的影响。结果表明,SiC陶瓷与316L不锈钢钎焊抗剪断口均发生在SiC陶瓷与钎料连接界面处,由于活性元素Ti的作用,在陶瓷与钎料的界面处形成了连续的反应层,反应生成了Ti C和Ti5Si3;在316L不锈钢与钎料的界面处,生成了Fe-Ti化合物和Cu-Ti化合物。随着钎焊温度升高及保温时间延长,接头强度均呈现出一个峰值,在温度为900℃,保温20 min的工艺条件下可获得最大接头抗剪强度。     

Ti-Si共晶钎料的制备及其对SiC陶瓷可焊性

采用海绵钛和单晶硅为原料,通过非自耗电弧熔融技术制备91.5Ti-8.5Si(wt%)和22Ti-78Si(wt%)共晶钎料.在真空中1400℃×10min条件下,研究了共晶钎料对SiC陶瓷的润湿性能和界面反应.结果表明:两种共晶钎料对SiC陶瓷均具有良好的润湿性能,润湿角分别约为10°和25°.在润湿实验后,91.5Ti-8.5Si(wt%)钎料和SiC陶瓷分离,22Ti-78Si (wt%)钎料和SiC陶瓷之间结合紧密.在润湿实验的温度制度下,用22Ti-78Si (wt%)钎料(厚度为0.2mm)对SiC陶瓷进行了初步连接,接头的抗弯强度为72MPa.采用SEM、EDS、XRD等检测手段对钎料的形貌和物相组成、钎料和SiC陶瓷的界面结合情况进行了表征,揭示了钎料对SiC陶瓷润湿性和界面反应的机理.     

用Ti50Cu＋W钎料连接Si／SiC复相陶瓷与殷钢的研究

采用真空钎焊方法,以Ti50Cu W钎料连接Si/SiC复相陶瓷与殷钢.观察分析了获得接头显微组织结构,测定了接头的力学性能,研究了工艺参数和增强相W含量对接头组织结构和力学性能的影响.研究结果表明:采用Ti50Cu W钎料连接Si/SiC复相陶瓷与殷钢,可获得连接良好、组织致密的接头,W含量30%(体积分数),钎焊温度970℃,保温时间5rain时,接头室温剪切强度达到最大值106MPa.     

22Ti-78Si高温共晶钎料对SiC陶瓷的钎焊连接

利用非自耗电弧熔融技术制备的22Ti-78Si (wt%)高温共晶钎料实现SiC陶瓷连接. 采用SEM、材料试验机研究了工艺参数对钎焊接头的组织结构、强度和断口形貌的影响规律. 结果表明: 在钎焊温度1380~1420℃、保温时间5~20min、钎料厚度50~200 μm条件下, 均能实现SiC陶瓷连接, 在1400℃、保温时间10min和钎料厚度100μm的条件下, SiC/22Ti-78Si/SiC接头剪切强度最大值可达125MPa.     

Vitreous joining of SiC-coated carbon/carbon composites

This paper investigated the feasibility of joining of carbon/carbon (C/C) composites by using a silicate as interlayer. A SiC coating was pre-prepared on C/C substrate by pack-cementation technique to improve the wettability of glass on C/C composites, then the joints were prepared by a one-shot and low cost way. Microstructure and morphologies of the as-received joints were characterized by XRD, SEM and EDS. The results indicated that the SiC coating not only had a strong bonding with C/C composites, but also had a good physical and chemical compatibility with silicate glass. The room-temperature shear strength of the joints gives encouraging results, which can be up to 26 MPa. The fracture mode and the fracture behavior were discussed also.     

Joining of SiC ceramic-based materials with ternary carbide Ti3SiC2

The joining of two pieces of SiC-based ceramic materials (SiC or C_f/SiC composite) was conducted using Ti₃SiC₂ as filler in vacuum in the joining temperatures range from 1200 °C to 1600 °C. The similar chemical reactions took place at the interface between Ti₃SiC₂ and SiC or C_f/SiC, and became more complete with joining temperature increases, and with the consequent increased joining strengths of the SiC and C_f/SiC joints. Based on the XRD and SEM analyses, it turns out that two reasons are most important for the high joining strengths of the SiC and C_f/SiC joints. One is the development of layered Ti₃SiC₂ ceramic, which has plasticity in nature and can contribute to thermal stress relaxation of the joints; the other is the chemical reactions between Ti₃SiC₂ and the base materials which result in good interface bonding.     

C/C复合材料与LAS陶瓷连接的显微结构与性能

采用Y2O3-Al2O3-SiO2-TiO2(YAST)玻璃作为中间层,对SiC-MoSi2表面改性的C/C复合材料与Li2CO3-Al2O3-SiO2(LAS)陶瓷进行热压连接,所施压力为20MPa,保温时间为30min,连接温度分别为1150℃,1200℃,1250℃,1300℃。利用SEM,EDS和BEI(背散射电子像)对SiC-MoSi2涂层,连接界面的形貌和断口进行了分析,研究结果表明,SiC-MoSi2涂层与基体结合紧密,Si、C元素在界面处呈梯度状分布,形成厚度约为15μm的过渡层。YAST玻璃与基体润湿良好,接头的剪切强度可达26.21MPa。     

Joining of carbon/carbon composites for nuclear applications

Using hot pressing, carbon/carbon composites were joined using a Ti₃SiC₂/SiC interlayer which was in situ synthesized by the reaction of TiC and Si. Phase composition of the interlayer was characterized by X-ray diffraction. Morphologies of the joints before and after shear test were determined by scanning electron microscope and energy dispersive spectroscopy. The mechanical strength of the joints was assessed by shear strength test. Phase analysis reveals that the interlayer was mainly composed of ternary Ti₃SiC₂, SiC, and little TiC. The microstructure observation results show that the dense and uniform interlayer adheres firmly to the C/C composites. A composition gradient reaction layer was formed at the joining interface between C/C substrates and interlayer. The room temperature average shear strength of the joints is about 38.9 ± 3.6 MPa. The joining mechanism and failure behavior of the joints were also discussed.     

中间层厚度对LAS玻璃陶瓷与C/C复合材料连接强度的影响

采用不同厚度的MgO-Al2O3-SiO2(MAS)玻璃作为中间层,对表面改性炭/炭(C/C)复合材料与Li2CO3-Al2O3-SiO2(LAS)玻璃陶瓷进行热压连接,重点研究了中间层厚度对接头强度的影响,并利用扫描电子显微镜(SEM)对连接界面及剪切断口的微观组织和形貌进行了分析.结果表明:没有添加中间层时,接头强度仅为10MPa;采用MAS玻璃作为中间层时,接头室温剪切强度随着中间层厚度的增加先增大后减小,当中间层厚度为80μm时,获得的接头剪切强度最大,为26.61MPa.     

SiC/SiC and SiC/Kovar joining by Ni–Si and Mo interlayers

A composite joining technique, using a Ni–56Si filler alloy and Mo as interlayers, was used to join SiC to SiC and to Kovar. The wetting of the Ni–Si alloy on SiC ceramic was studied in a vacuum at 1,350 °C by the sessile drop technique as a function of time; the non-reactive wetting characteristics in the Ni–Si/SiC system were confirmed, with an equilibrium contact angle of about 23°. SiC/SiC joints were fabricated by two processes using a Ni–Si/Mo/Ni–Si structure as the interlayer. SiC/Kovar joints were produced by means of a multilayer structure: molybdenum, which is used as the interlayer, was joined to Kovar on one side by means of transient liquid phase bonding and to SiC on the other side, using a Ni–Si coating as a filler alloy. The resulting joints were analyzed and discussed in terms of joint morphology and microstructure, joint strength, and fracture behavior. Two interfacial layers form at the Kovar/Mo and the Mo/Ni–Si interfaces due to dissolution and interdiffusion phenomena between the metallic elements, without there being any observable reactions with the SiC component. The type of joining process and the experimental conditions used play a key role in determining the joint microstructure and composition, the joint strength and its fracture behavior.     

Investigation on diffusion bonding characteristics of SiC particulate reinforced aluminium metal matrix composites (Al/SiCp-MMC)

Joining characteristics of SiC particulate reinforced aluminium metal matrix composites (Al/SiC_p-MMC) were investigated by vacuum diffusion bonding process. The joining performances of the similar and dissimilar composites were studied, and the influences of SiC_p volume percentage and the insert alloy layer on bonding quality and properties of the bonded joints were also estimated. The experimental results indicate that the strength of vacuum diffusion bonded joints decreases with increasing SiC_p volume percentage, and obtaining satisfactory bonding quality in the diffusion bonded joints of the dissimilar Al/SiC_p-MMC is much more difficult than that of the similar Al/SiC_p-MMC. Moreover, the results still manifest that the diffusion bonding either for the similar or for the dissimilar Al/SiC_p-MMC, the suitable insert alloy layer can improve evidently the joining quality of joints, and the strength of diffusion bonded joints corresponding to using the insert alloy layer is apparently higher than that of no insert layer.     

高体积比SiCp/6063Al复合材料的铝基钎料制备及钎焊工艺研究

采用快速甩带技术制备了(Al-10Si-20Cu-0.05Ce)-1Ti(质量分数/％)急冷箔状钎料,并对60％体积分数的SiCp/6063Al复合材料进行真空钎焊实验,然后对钎料及接头的显微组织与性能进行测定和分析.结果表明,急冷钎料的微观组织细小、成分均匀,厚80～90μm,主要包含Al、CuAl2、Si和Al2Ti等相.当升高钎焊温度(T/℃)或延长保温时间(t/min),SiCp/钎料界面的润湿性改善,6063Al基体/钎料间互扩散和溶解作用增强,接头连接质量逐渐提高.当T=590℃、t=30 min时,接头抗剪强度达到112.6MPa;当T=590℃、t=50 min时,少量小尺寸SiCp因液态钎料排挤而分散于钎缝,因加工硬化而使接头强度递增7.3％.然而,当T≥595℃、t≥60 min时,SiCp偏聚于钎缝,导致接头组织恶化,且剪切断裂以脆性断裂为主.综合考虑钎焊成本与接头强度使用要求,确定最佳钎焊工艺为590℃、30 min.