Fabrication of Tia SiC2 modified C/C - SiC composites by liquid silicon infiltration

采用浆料浸渗结合液硅渗透法原位生成高韧性Ti3SiC2基体,制备Ti3SiC2改性C／C—SiC复合材料。研究了TiC颗粒的引入对熔融Si浸渗效果的影响,分析了Ti3SiC2改性C／C-SiC复合材料的微结构和力学性能。实验结果表明：TiC与熔融si反应生成Ti3SiC2是可行的,而且c的存在更有利于生成Ti3SiC2;在含TiC颗粒的C／C预制体孔隙（平均孔径22．3μm）内,熔融si的渗透深度1min内可达10．8cm;Ti3SiC2取代残余Si后提高了C／C-SiC复合材料的力学性能,C／C-SiC-Ti3SiC2复合材料的弯曲强度达203MPa,断裂韧性达到8．8MPa·m^[1/2];对于厚度为20rllm的试样,不同渗透深度处材料均具有相近的相成分、密度和力学性能,无明显微结构梯度存在,表明所采用的浆料浸渗结合液硅渗透工艺适用于制备厚壁Ti3SiC2改性C／C-SiC复合材料构件。     

Ti基复合材料界面反应扩散的微观分析

通过SiC连续纤维增强Ti基复合材料的制备及在不同条件下的热处理试验,利用TEM,SEM,EDS及XRD分析技术研究复合材料的界面反应以及产物相的形成.研究结果表明:SiC /Ti复合材料界面发生了反应扩散,反应元素C,Ti,Si在界面反应层中出现浓度波动;界面反应产物被确认为是Ti3SiC2 ,TiC和 Ti5Si3,在靠近SiC侧出现Ti3SiC2和Ti5Si3单相区,靠近Ti基体侧为Ti5Si3单相区,中间为TiC Ti5Si3双相区;SiC/Ti复合材料界面相序列为SiC┃Ti3SiC2┃Ti5Si3┃TiC Ti5Si3┃Ti5Si3┃Ti.     

SPS原位反应制备TiSi2基复合材料的微观结构和性能研究

以工业用硅粉、碳粉和碳化钛粉为原料,利用放电等离子烧结技术原位反应制备了TiSi2-SiC两相复合材料和TiSi2-SiC-Ti3SiC2三相复合材料.利用XRD、FESEM和TEM对复合材料的相组成和微观结构进行了研究.结果表明,基体相TiSi2的晶粒尺寸在1um以上,反应生成的SiC颗粒尺度在200～300nm,且均匀弥散分布在TiSi2基体中.TiSi2-SiC材料的硬度、断裂韧性和抗弯强度随着SiC含量的增加都有一定程度的提高.Ti3SiC2三元相的引入大大提高了TiSi2-SiC-Ti3SiC2复合材料的力学性能. SiC和Ti2SiC2的引入对TiSi2-SiC复合材料在高温下的电导率和热导率影响较小.     

催化剂及Al对TiAl合金表面Si-Al-Y共渗层组织结构的影响

通过1 050℃下Si-Al-Y扩散共渗4h的方法在TiAl合金表面制备了Y改性Si-Al共渗层,采用SEM、EDS和XRD分析了渗剂中催化剂(AlCl3·6H2O)及Al含量对共渗层组织及相组成的影响。结果表明,催化剂含量为1%(质量分数)时未形成完整的Si-A-Y共渗层;当催化剂含量为3%,5%和8%(质量分数)时所形成的共渗层均具有多层复合结构,共渗层的内层都是由TiAl2和γ-TiAl相组成,互扩散区为富Al的TiAl相;随催化剂含量的增加共渗层外层和中间层的相组成都发生了改变;催化剂含量为3%(质量分数)时所制备的共渗层外层为大量的(Ti,X)5Si4(X表示元素Nb和Cr)和少量的(Ti,X)5Si3相;催化剂含量为5%,8%(质量分数)时所制备的共渗层外层分别为(Ti,X)5Si3和TiSi2相,中间层均为(Ti,X)5Si4及(Ti,X)5Si3相,由于TiSi2外层具有良好的抗高温氧化性能,因此催化剂含量为8%(质量分数)时适合用于Si-Al-Y共渗层的制备。Al含量对共渗层的相组成无显著影响,但改变了共渗层各层厚度。     

熔渗温度对Si/Al复合材料组织及性能的影响

采用无压熔渗法制备Si/Al复合材料,研究了熔渗温度对所制备Si/Al复合材料Si相形貌的影响,对Si相间基体合金的凝固组织进行了分析,测试了Si/Al复合材料热膨胀系数、热导率及抗弯强度。结果表明,在相同熔渗时间下,随着熔渗温度升高,所制备Si/Al复合材料中Si相从颗粒状到形成网络状。Si相间的Al-Si基体合金中不再是典型的初生相和共晶组织,而是出现了类似离异共晶的结晶现象,即初晶Si和共晶Si是在原存的Si相上结晶长大。XRD分析显示在所制备复合材料中只有Si相和Al相。随着熔渗温度升高复合材料热膨胀系数、热导率以及抗弯强度均出现下降。     

Nb-Ti-Cr-Si基超高温合金有坩埚整体定向凝固组织的演化

分析了Nb-Ti-Cr-Si基超高温合金有坩埚整体定向凝固试样不同区域的组织,结果表明未熔区的组织由初生相Nbss、块状的(Nb,X)5Si3和少量的小块状Cr2Nb组成。在过渡区初生相Nbss依附在未熔区的Nbss优先生长,Nbss/(Nb,X)5Si3共晶组织生长比较混乱,在初生相Nbss枝晶间出现了富Ti的Nbss/Cr2Nb共晶团。稳态区组织中Nbss和(Nb,X)5Si3定向排列,实现了整体定向凝固。固/液界面形态为树枝状,在糊状区出现了Nbss/(Nb,X)5Si3、富Ti的Nbss/(Nb,X)5Si3和Nbss/Cr2Nb三种共晶组织,根据组织分析的结果并总结了其凝固路径,测试了不同区域组织的显微硬度,结果表明稳态区的(Nb,X)5Si3的显微硬度最高。     

近熔态扩散新工艺制备SiC纤维增强Al基复合材料的界面分析

采用近熔态扩散新工艺制备了SiCf /Al(5A02)铝合金基复合材料,采用透射电镜(TEM)和X射线能谱 (EDX)分析了界面产物和反应机理.与采用传统固态扩散法制备的样品相对比,样品界面处没有形成脆性相Al4C3,且Al2O3被MgO取代;而固态扩散工艺制得的样品界面处发现针状或块状的Al4C3在C涂层或附着在C涂层上的Al2O3边缘形成,并向基体中生长,破坏了界面的连续性.采用近熔态扩散法制备的样品由于合金元素Mg在从半液态冷却过程中偏聚到界面附近,并与Al2O3发生反应,生成细小的MgO颗粒,阻碍了C的扩散,并抑制了脆性相Al4C3的形成,有利于对界面有害反应的控制.     

Ti/Si(100)体系界面扩散反应动力学研究

采用移动边界条件下扩散问题的处理方法，综合界面反应和扩散两个过程对界面硅化物形成的影响，建立起Ti／Si（100）界面扩散反应动力学理论模型，并拟合快速热退火处理后试样界面Auger深度分析谱，得到Ti，Si在相应界质中扩散系数和表现反应活化能。研究结果表明，Ti／Si体系界面TiSi2生成经历了一个由反应动力学控制到扩散控制的过渡。Si从其晶格中解离并扩散到Ti／TiSi2界面是制约扩散过程的关键因素。     

温度对TiAl合金表面Si-Al-Y共渗层组织结构的影响

通过在1000,1050,1100℃和1150℃下Si-Al-Y扩散共渗4h的方法,在TiAl合金表面制备了Y改性Si-Al共渗层,采用SEM,EDS和XRD分析了共渗温度对共渗层组织及相组成的影响。结果表明:不同温度所制备的Si-Al-Y共渗层均具有多层复合结构,共渗层的内层都是由TiAl2和γ-TiAl相组成,互扩散区为富Al的TiAl相,随温度的升高,共渗层外层和中间层的组成相都发生改变。经1000℃/4h共渗的最外层主要为TiAl3相;温度为1050℃时,由外向内依次为TiSi2外层,(Ti,X)5Si4及(Ti,X)5Si3(X表示元素Nb和Cr)中间层;1100℃和1150℃/4h条件下共渗层具有相似的结构,在1100℃/4h条件下其外层由(Ti,X)5Si4,(Ti,X)5Si3相组成;在1150℃/4h条件下其外层由(Ti,X)5Si3相组成。在四种温度条件下,1050℃/4h下制备的共渗层较厚,组织致密,适合用于Si-Al-Y共渗层的制备。     

无压烧结制备Ti_3SiC_2-SiC复合材料块体EI北大核心

以钛粉、硅粉和石墨粉为原料,通过无压烧结法制备了Ti3SiC2-SiC块体复合材料。利用X射线衍射仪对制得的样品进行相分析,并运用扫描电镜分析材料的微观结构,用差热分析仪测定反应温度。结果表明,Ti∶Si∶C=0.42∶0.23∶0.35时,可制得纯度较高的Ti3SiC2-SiC复合材料块体,只含有极少量的TiSi2杂质。Ti3SiC2晶粒无特定的生长方向,平均长度在10μm以下,厚度小于5μm。略高的Si含量有利于获得纯度较高的Ti3SiC2-SiC复合材料。     

Casting particulate and fibrous metal-matrix composites by vacuum infiltration of a liquid metal under an inert gas pressure

A new method of making metal-matrix composites is reported. This method combines the essentials of three liquid-phase fabrication methods: (i) vacuum infiltration, (ii) infiltration under an inert gas pressure, and (iii) squeeze casting. In this method, the particulate or fibrous preform is placed in a mould and the matrix alloy is placed above the preform. The matrix alloy is heated to the liquidus temperature together with the mould and the preform under vacuum. Then an inert gas like argon is compressed on to the top surface of the matrix-alloy melt, forcing the melt to infiltrate the preform. The pressure is 1000 to 2500 psi. As the melt is just at liquidus temperature, it is much lower than that used in squeeze casting. Moreover, the pressure is an order of magnitude lower than that used in squeeze casting. The low temperature lessens the interfacial reaction between the matrix and the filler, while the low pressure essentially eliminates preform compression. This method has been successfully used to fabricate aluminium-matrix composites reinforced by short ceramic fibres, continuous ceramic fibres, SiC particles, Al₂O₃ particles, graphite flakes and SiC whiskers.     

Effect of re-melting on particle distribution and interface formation in SiC reinforced 2124Al matrix composite

The interface between metal matrix and ceramic reinforcement particles plays an important role in improving properties of the metal matrix composites. Hence, it is important to find out the interface structure of composite after re-melting. In the present investigation, the 2124Al matrix with 10 wt.% SiC particle reinforced composite was re-melted at 800 °C and 900 °C for 10 min followed by pouring into a permanent mould. The microstructures reveal that the SiC particles are distributed throughout the Al-matrix. The volume fraction of SiC particles varies from top to bottom of the composite plate and the difference increases with the decrease of re-melting temperature. The interfacial structure of re-melted 2124Al–10 wt.%SiC composite was investigated using scanning electron microscopy, an electron probe micro-analyzer, a scanning transmission electron detector fitted with scanning electron microscopy and an X-ray energy dispersive spectrometer. It is found that a thick layer of reaction product is formed at the interface of composite after re-melting. The experimental results show that the reaction products at the interface are associated with high concentration of Cu, Mg, Si and C. At re-melting temperature, liquid Al reacts with SiC to form Al₄C₃ and Al–Si eutectic phase or elemental Si at the interface. High concentration of Si at the interface indicates that SiC is dissociated during re-melting. The X-ray energy dispersive spectrometer analyses confirm that Mg- and Cu-enrich phases are formed at the interface region. The Mg is segregated at the interface region and formed MgAl₂O₄ in the presence of oxygen. The several elements identified at the interface region indicate that different types of interfaces are formed in between Al matrix and SiC particles. The Al–Si eutectic phase is formed around SiC particles during re-melting which restricts the SiC dissolution.     

Synthesis of SiC/Al Co-Continuous Composite by Spontaneous Melt Infiltration

1. IntroductionBecause of the adVantages such as ease of fabrication, low cost and near net shape forming capability,liquid metal infiltration has become a popular technique to fabricate metal matriX composites(MMCs)with high contellt reinforcements. In the process ofmelt infiltration, liquid metal penetrates into the continuous porosity of a packed ceramic filler or preform either by aPPlied positive or negative pressuresuch as in vacuum infiltration[1], pressurized liquldmetal infiltration…     

无压浸渗制备的SiC/Al复合材料的微观组织研究

利用SRD,OM,SEM,TEM等微观结构分析手段,对无压浸渗制备的SiCp/Al复合材料的微观结构进行了研究。结果表明,SiCp/Al复合材料中存在SiC,Al,MgAl2O4,Si和Mgi2Si诸相。在组织中没有粗大的铝硅共晶体针条,铝基体被众多SiC颗粒分割,成为细小的连续的空间网络。在铝基体中分布着Si相及Mg2Si相。透射电子显微镜高分辨像表明,在SiC与铝合金的界面上存在镁铝尖晶石（MgAl2O4）相,没有出现Al4C3相。     

SiCp/Al Composites Fabricated by Modified Squeeze Casting Technique

A cost effective method was introduced to fabricate pure aluminum matrix composites reinforced with 20% volume fraction of 3.5 μm SiC particles by squeeze casting followed by hot extrusion. In order to lower volume fraction of the composites, a mixed preform containing pure aluminum powder and the SiC particles was used. The suitable processing parameters for the infiltration of pure aluminum melt into the mixed preform are： melt temperature 800℃, preform temperature 500℃, infiltration pressure 5 MPa, and solidification pressure 50 MPa. Microstructure and properties of the composites in both as-cast and hot extruded states were investigated. The results indicate that hot extrusion can obviously improve the mechanical properties of the composite.     

The microstructures of aluminium alloy metal-matrix composites manufactured by squeeze casting

Squeeze-cast metal-matrix composite ingots have been manufactured by recasting A356/10% SiC_p and by melt infiltrating A357/Al₂O_3f. The resulting microstructures have been examined by optical and transmission electron microscopy. The primary aluminium in squeeze-cast A356/10% SiC_p exhibits a dendritic structure with eutectic silicon particles and SiC particulate distributed throughout the interdendritic regions. Unlike squeeze-cast monolithic A357, the primary aluminium dendrite arm spacing and eutectic-silicon particle size in squeeze-cast A356/10% SiC_p are not strongly affected by an increased cooling rate at high applied pressure. With low die and preform temperature, a high applied pressure is essential to obtain complete melt infiltration in A357/Al₂O_3f. During melt infiltration, the ceramic preform acts as a filter, preferentially allowing silicon rich liquid to pass through.     

SiCf/SiC复合材料耐高温氟熔盐腐蚀性能研究

实验研究了熔渗(MI)工艺、浸渍-裂解(PIP)工艺和化学气相渗透(CVI)工艺制备SiC_f/SiC复合材料在800℃的氟熔盐(46.5mol% LiF-11.5mol% NaF-42.0mol% KF)中的腐蚀行为, 通过X射线衍射仪、扫描电镜以及能谱仪等表征手段, 对腐蚀前后样品的物相组成和微观结构进行了分析。实验结果表明, 不同工艺获得的SiC基体与高温氟熔盐的相容性与基体组成有关; MI-SiC中的游离Si相以及PIP-SiC和CVI-SiC中的富氧相是SiC基体中的两种腐蚀弱区, 易被熔盐选择性腐蚀; MI-SiC_f/SiC复合材料以纤维束间游离Si基体腐蚀为主, PIP-SiC_f/SiC复合材料基体腐蚀损伤集中在网络状富氧带, CVI-SiC_f/SiC复合材料的腐蚀损伤主要是沉积层间的含氧边界以及由此造成的基体层状剥离。与MI和PIP样品相比, CVI基体纯度高, 结晶度好, 表观腐蚀速率仅为0.0445 μg/(mm²·h), 具有更好的耐氟熔盐腐蚀性能。     

碳化硅颗粒增强铝基复合材料的无压浸透反应机理探讨

为探讨SiCp/Al基复合材料无压浸渗反应机理,利用XPS鉴定了SiC预制体浸渗前沿界面上的反应产物结构.采用HRTEM研究了SiCp/Al基复合材料的界面结构.结果表明,浸渗与未浸渗部分之间的界面上存在MgO.Al2O3和ZnO诸化合物,没有发现氮的化合物.在SiC相与铝相的界面上仅存在MgAl2O4相,MgAl2O4相几乎连续地包敷在SiC颗粒上.这表明,高温下SiC与熔Al合金接触后,SiC颗粒表面上的SiO2与Al,Mg,Zn诸元素发生了放热反应,从而降低了表面张力,提高了湿润性.促进了自发浸渗.     

碳化硅颗粒增强铝基复合材料的无压浸渗反应机理探讨

为探讨SiCp/Al复合材料无压浸渗反应机理,利用XPS鉴定了SiC预制体浸渗前沿界面上的反应产物结构,采用HRTEM研究了SiCp/Al基复合材料的界面结构。结果表明,浸渗与未浸渗部分之间的界面上存在MgO,Al2O3和ZnO诸化合物,没有发现氮的化合物,在SiC相与铝相的界面上仅存在MgAl2O4相,MgAl2O4相几乎连续地包敷在SiC颗粒上,这表明,高温下SiC与熔Al合金接触后,SiC颗粒表面上的SiO2与Al,Mg,Zn诸元素发生了放热反应,从而降低了表面张力,提高了湿润性,促进了自发浸渗。     

微孔碳陶瓷化反应机理的研究

研究了微孔碳制备SiC陶瓷的反应过程及反应机理.SiC陶瓷的最终组织受C/Si质量比及渗硅时间的影响.较低C/Si质量比时试样中心未被硅化,较高C/Si质量比时制得由SiC、Si及极少量未反应C组成的复相陶瓷.随渗硅时间延长,复相陶瓷中SiC颗粒的形状由长条状向无规则状转变,颗粒分布则由局部有序向无序转变.反应过程为：液硅因毛细作用自发的渗入微孔碳孔道,同时与溶解的碳壁发生反应生成SiC.因孔道及碳壁尺寸的不同造成液硅渗入深度和碳壁被溶解厚度的差异,结果出现被SiC包裹的小颗粒碳.随后被包裹的碳通过SiC层扩散到液硅中,沉积在先形成的SiC上促使大量先形成SiC的合并以及部分硅被SiC包裹,进而改变SiC陶瓷的显微组织.