C／SiC复合材料热性能及抗氧化性能的研究

本文研究了聚碳硅烷化学转化法制备C/SiC复合材料过程中碳纤维(CF)、碳化硅(SiC)基体的热物理性能对C/SiC复合材料性能的影响,并提出了一种可以提高复合材料抗氧化能力的简单有效的方法。     

C/C多孔体对C/C-SiC复合材料微观结构和弯曲性能的影响

以4种纤维含量相同(32%,体积分数,下同),用化学气相渗透(chemical vapor infiltration,CVI)法制备了4种密度的碳纤维增强碳(carbon fiber reinforced carbon,C/C)多孔体,基体炭含量约20%～50%.利用液相渗硅法(liquid silicon infiltration,LSI)制备了C/C-SiC复合材料,研究了C/C多孔体对所制备的C/C-SiC复合材料微观结构和弯曲性能的影响.结果表明:不同密度的C/C多孔体反应渗硅后,复合材料的物相组成均为SiC,C及单质Si;随着C/C多孔体中基体炭含量的增加,C/C-SiC复合材料中SiC含量逐渐减少而热解炭含量逐渐增加.C/C-SiC复合材料弯曲强度随着材料中残留热解炭含量增加而逐渐增加,热解炭含量为约42%的C/C多孔体所制备的C/C-SiC复合材料的弯曲强度最大,达到320 MPa.     

SiC纳米线增强反应烧结碳化硅陶瓷的性能研究

以单晶SiC纳米线作为增强体,碳化硅-碳为陶瓷基体,在1550℃下,采用反应烧结制备碳化硅基陶瓷复合材料(SiCnf/SiC).结合X射线衍射、万能试验机和扫描电镜等检测和分析,研究SiC纳米线对复合材料的微结构和力学性能的影响.研究表明:与未加入SiC纳米线的反应烧结碳化硅陶瓷相比,添加SiC纳米线的复合陶瓷的抗弯强度和断裂韧性都得到显著的提高,抗弯强度提高了52％,达到320 MPa(SiC纳米线含量为12wt％),断裂韧性提高了40.6％,达到4.5 MPa· m1/2(SiC纳米线含量为15wt％);反应后的SiC纳米线仍然可以保持原有的竹节状结构,且随着SiC纳米线的加入,复合陶瓷的断口可以观察到SiC纳米线拔出现象.但由于SiC纳米线“架桥”的现象,添加过量的纳米线会降低复合陶瓷的密度和限制复合陶瓷力学性能的提高.同时还讨论了SiCnf/SiC的增强机理.     

碳含量对反应熔渗法制备SiC晶须增强碳化硅陶瓷性能的影响研究

以SiC晶须作为增强体,通过酚醛树脂高温碳化裂解获得碳包覆的SiC晶须,与纳米碳化硅粉体、炭黑混合均匀形成复合陶瓷乙醇浆料.经过干燥、造粒、成型和排胶后获得SiCw-C-SiC素坯,利用反应熔渗法制备高体积分数的SiC晶须增强SiC陶瓷基复合材料.研究了碳黑含量对复合材料力学性能与显微结构的影响.通过扫描电镜照片显示,碳包覆的SiC晶须经高温反应熔渗后仍保持表面的竹节状形貌,且晶须与碳化硅基体间形成适中的界面结合强度,材料断口处有明显的晶须拔出;当炭黑含量为15wt％时,抗弯强度和断裂韧性达到最高值分别为315 MPa和4.85 MPa·m1/2,比未加晶须的SiC陶瓷抗弯强度提高了25％,断裂韧性提高了15％;当炭黑含量为20wt％时,复合材料中残留部分未反应的炭黑,制约其力学性能的提高.     

温度和环境对2维C/(SiC–B_xC)_n断裂韧性的影响

采用单边切口梁法研究了二维碳纤维增强碳化硼–碳化硅复合材料(2D C/(SiC–BxC)n)在空气和真空两种环境下断裂韧性与温度的关系,用扫描电镜观察断口微观形貌。结果表明:真空中2D C/(SiC–BxC)n复合材料的断裂韧性随温度升高而降低,室温下界面结合弱,残余热应力大,易发生纤维桥接裂纹,断裂韧性高;高温下相反。在空气中随温度升高断裂韧性增加,700℃达到最大值,尔后随温度升高而降低,这与生成的B2O3和SiO2.B2O3固溶体会封填裂纹以及碳相的氧化有关。     

先驱体浸渗裂解法制备C/C-SiC复合材料的烧蚀性能

用先驱体浸渗裂解法制备了碳纤维增强碳(carbon fiber reinforced carbon,C/C)-SiC复合材料,用H2-D2火焰法检测其烧蚀性能.结果表明:C/C-SiC复合材料的烧蚀率随复合材料中的Si含量的增加而呈下降趋势;经过5次浸渍,C/C-SiC复合材料的密度从1.46 g/cm3增加到1.75 g/cm3,Si含量从5.06%增加到13.8%,线烧蚀率和质量烧蚀率分别下降474%和34.5%.密度为1.75g/cm3的C/C-SiC复合材料,其线烧蚀率和质量烧蚀率分别为2.22 μm/s和1.289 mg/s,其线烧蚀率和质量烧蚀率分别为密度1.78 g/cm3的C/C复合材料的21.7%和78.6%.基体中SiC的引入明显提高了C/C复合材料的抗氧化烧蚀性能.     

温度和环境对2维C/(SiC-BxC) n断裂韧性的影响

采用单边切口梁法研究了二维碳纤维增强碳化硼–碳化硅复合材料(2D C/(SiC–BxC)n)在空气和真空两种环境下断裂韧性与温度的关系,用扫描电镜观察断口微观形貌。结果表明:真空中2D C/(SiC–BxC)n复合材料的断裂韧性随温度升高而降低,室温下界面结合弱,残余热应力大,易发生纤维桥接裂纹,断裂韧性高;高温下相反。在空气中随温度升高断裂韧性增加,700℃达到最大值,尔后随温度升高而降低,这与生成的B2O3和SiO2.B2O3固溶体会封填裂纹以及碳相的氧化有关。     

Cf/SiC复合材料的原料高效改性及其3D打印制备研究进展

选用3D打印制备的碳纤维增强碳化硅陶瓷基（Cf/SiC）复合材料被广泛应用在航空航天、国防军事等重大领域。碳纤维（Cf）作为陶瓷基复合材料的主要候选增强体之一,由于表面惰性的存在,为了提高其与碳化硅（SiC）陶瓷基体的粘附性,对原料Cf的表面改性工作是十分必要的。粉末原料的高效改性制备是3D打印成型陶瓷的重要途径。本文综述了近年来国内外针对Cf改性的各种方法及特点,对Cf/SiC复合材料的3D打印成型及其高效制备方法进行归纳总结。     

纤维氧化处理对SiCsf/SiC复合材料力学性能的影响

以Y2O3、Al2O3为烧结助剂,采用无压烧结法制备短碳化硅纤维(2～4mm)增强碳化硅(ShortSiCfiberreinforcedSiCcomposite,SiCsf/SiC)复合材料,研究了纤维氧化处理对SiCsf/SiC复合材料结构及力学性能的影响。采用X射线衍射(XRD)、扫描电镜(SEM)以及力学性能试验机对材料进行结构表征和力学性能测试。结果表明:纤维氧化处理后,复合材料的弯曲强度和断裂韧性均有大幅提高。当纤维含量达到5wt%时,复合材料断裂韧性为5.41MPa.m1/2,与原始纤维增强SiC样品相比,提高了6.5%;与无纤维增强SiC样品相比,提高了27%。扫描电镜显示纤维氧化处理后,纤维与基体结合紧密。     

二维C/(BCχ-SiC)n复合材料的高温层间剪切性能

采用双槽口剪切法(double-notchcd shear,DNS)研究了二维(twodimensional,2D)碳乡纤维增强碳化硼-碳化硅[2DC/(BCx-SiC)]复合材料的高温层间剪切性能,用扫描电子显微镜观察断口彤貌.结果表明:在25～1200℃范围内.温度对2DC/(BCx-SiC)n复合材料的层间剪切强度有明显影响,在900℃时材料的层间剪切强度最高可达40.0MPa,分别比25℃和1200℃的商约13%和8%,略高于700℃的.此外,C/(BCx-SiC)n的层间剪切强度始终高于C/SiC的强度,且2种材料的层间剪切强度随温度变化规律相似.断口分析表明:层间剪切失效发生在基体内部或基体/纤维界面上,而纤维并没有受到损伤.     

Effect of high-temperature heat treatment on the microstructure and mechanical behavior of PIP-based C/C-SiC composites with SiC filler

C/C-SiC composites were fabricated by a combined process of chemical vapor deposition (CVD), slurry infiltration(SI), and precursor infiltration and pyrolysis (PIP). The microstructure and mechanical behavior were investigated for the dense C/C-SiC composites before and after high-temperature heat treatment. The results indicated that the sintering of the SiC matrix and the migration of the SiC matrix/fiber bundles weak interface occurred after high-temperature heat treatment at 1900 ℃. The SiC sintering resulted in an increase in the flexural strength of the C/C-SiC composites from 298.9 ± 35.0 MPa to 411.1 ± 57.3 MPa. The migration of the weak interface changed the direction of crack propagation, making the fracture toughness of the C/C-SiC composites decrease from 13.3 ± 1.7 MPa⋅m ^1/2 to 9.02 ± 1.5 MPa⋅m ^1/2.     

C/C-SiC梯度基复合材料氧化行为研究

研究比较了Ｃ／Ｃ－ＳｉＣ梯度基复合材料和Ｃ／Ｃ复合材料的氧化行为．实验结果表明：ＳｉＣ通过占据表面活性点提高了共沉积基体的氧化起始温度;由于减少了碳与氧的接触面积,阻挡氧化凹坑的扩展,降低了材料的氧化质量损失速率．利用ＳＥＭ观察了梯度基复合材料微观氧化过程     

Formation mechanism of Si-Y-C ceramic matrix by reactive melt infiltration using Si-Y alloy and properties of C/Si-Y-C composites

Herein, Si-Y eutectic alloy were introduced into porous C/C preform by reactive melt infiltration (RMI) to prepare C/Si-Y-C composite. Phase compositions and their distributions in the as-prepared composites were investigated. Result indicated that four main regions were found in the typical zone in Si-Y-C matrix, i.e., amorphous carbon, polycrystalline SiC doped with YSi2, amorphous SiC and single crystal YSi2. Based on the reaction between Si-Y alloy and C/C preform and microstructural observations, a model regarding to microstructure formation mechanism was proposed to reveal reaction process. Moreover, improved flexural strength, fracture toughness, thermal diffusivity and thermal conductivity of C/Si-Y-C composite were achieved compared to C/C-SiC.     

Preparation of SiC/SiC composites with high toughness by reaction of the SiCP+C double-cladding layer with liquid silicon

SiC/SiC composites prepared by liquid silicon infiltration (LSI) have the advantages of high densification, matrix cracking stress and ultimate tensile strength, but the toughness is usually insufficient. Relieving the residual microstress in fiber and interphase, dissipating crack propagation energy, and improving the crystallization degree of interphase can effectively increase the toughness of the composites. In this work, a special SiC particles and C (SiC_P +C) double-cladding layer is designed and prepared via the infiltration of SiC_P slurry and chemical vapor infiltration (CVI) of C in the porous SiC/SiC composites prepared by CVI. After LSI, the SiC generated by the reaction of C with molten Si combines with the SiC_P to form a layered structure matrix, which can effectually relieve residual microstress in fiber and interphase and dissipate crack propagation energy. The crystallization degree of BN interphase is increased under the effects of C-Si reaction exotherm. The as-received SiC/SiC composites possess a density of 2.64 g/cm³ and a porosity of 6.1%. The flexural strength of the SiC/SiC composites with layered structure matrix and highly crystalline BN interphase is 577 MPa, and the fracture toughness reaches up to 37 MPa·m^1/2. The microstructure and properties of four groups of SiC/SiC composites prepared by different processes are also investigated and compared to demonstrate the effectiveness of the SiC_P +C double-cladding layer design, which offers a strategy for developing the SiC/SiC composites with high performance.     

Experimental investigations on grinding characteristics and removal mechanisms of 2D–Cf/C-SiC composites based on reinforced fiber orientations

The effects of fiber orientations on the grinding force and ground surface roughness in grinding 2D–C_f/C–SiC composites were investigated in this work. The characteristics of surface microstructure and the mechanism of the grinding phenomena are also discussed. The results show that the prominent removal mechanism for grinding the 2D-C_f/C-SiC composites is the brittle fracture, and the destruction of the composites is mainly via breaking of interfacial bonds, fiber fracture, and matrix cracking. The grinding force of different grinding surfaces follows the order: Surface B > Surface A > Surface C, and the surface roughness follows: Surface C > Surface A > Surface B. Grinding parameters, such as feeding speed, depth of cut, and wheel speed, have a great influence on the grinding force and surface roughness. This result suggests that this body of work offers a useful guideline for improving the design and processing of 2D–C_f/C–SiC composites.     

Fabrication of C/C-SiC composites using high-char-yield resin

Carbon fiber reinforced ceramic matrix composites (C/C-SiC composites) were fabricated using a type of high-char-yield phenolic resin with the char yield of 81.17 wt.%. Firstly, the fabric prepreg was prepared by spreading the phenolic resin solution onto the two dimensional carbon fiber plain weave fabric and dried consequently. Afterward, the resin was cured and then the carbon fiber reinforced polymer (CFRP) was pyrolyzed to get amorphous carbon. Finally, C/C-SiC composites were obtained through liquid silicon infiltration (LSI) process. SEM micrographs showed that the Si/SiC area was homogeneously dispersed in the matrix, and during the siliconization process, a layer of SiC was formed along the surface of carbon fibers or carbon matrix. The fiber volume of CFRP was about 40 vol.%, which was much lower than other studies. XRD result indicated that only β-SiC type was formed. The result of X-ray computed tomography clearly showed the structure changes before and after the melt infiltration process. Mechanical property test showed that the composites had fracture strength of 186 ± 23 MPa, and a flexural modulus of 106 ± 8 GPa.     

界面相对碳纤维增韧碳化硅复合材料性能的影响

利用减压ＣＶＩ技术制备了三维碳纤维增韧碳化硅复合材料,研究了热解碳界面相对复合材料性能的影响。结果表明：适当选择界面相厚度,可获得弯曲强度和断裂韧性较高的碳纤维增韧碳化硅复合材料。     

裂解碳包覆对SiC纳米纤维增强SiC陶瓷基复合材料性能的影响

以SiC纳米纤维(SiC_nf)为增强体,通过化学气相沉积在SiC纳米纤维表面沉积裂解碳(PyC)包覆层,并与SiC粉体、Al₂O₃-Y₂O₃烧结助剂共混制备陶瓷素坯,采用热压烧结工艺制备质量分数为10%的SiC纳米纤维增强SiC陶瓷基(SiC_nf/SiC)复合材料。研究了PyC包覆层沉积时间对SiC_nf/SiC陶瓷基复合材料的致密度、断裂面微观形貌和力学性能的影响。结果表明:在1 100 ℃下沉积60 min制备的PyC包覆层厚度为10 nm,且为结晶度较好的层状石墨结构;相比于纤维表面无包覆层的复合材料,复合材料的断裂韧性提高了35%,达到最大值(19.35±1.17) MPa·m^1/2,抗弯强度为(375.5±8.5) MPa,致密度为96.68%。复合材料的断裂截面可见部分纳米纤维拔出现象,但SiC_nf/SiC陶瓷基复合材料界面结合仍较强,纳米纤维拔出短,表现为脆性断裂。     

Microstructure and properties of B4C-SiC composites prepared by polycarbosilane-coating/B4C powder route

B₄C-SiC composites with fine grains were fabricated with hot-pressing pyrolyzed mixtures of polycarbosilane-coated B₄C powder without or with the addition of Si at 1950 °C for 1 h under the pressure of 30 MPa. SiC derived from PCS promoted the densification of B₄C effectively and enhanced the fracture toughness of the composites. The sinterability and mechanical properties of the composites could be further improved by the addition of Si due to the formation of liquid Si and the elimination of free carbon during sintering. The relative density, Vickers hardness and fracture toughness of the composites prepared with PCS and 8 wt% Si reached 99.1%, 33.5 GPa, and 5.57 MPa m^1/2, respectively. A number of layered structures and dislocations were observed in the B₄C-SiC composites. The complicated microstructure and crack bridging by homogeneously dispersed SiC grains as well as crack deflection by SiC nanoparticles may be responsible for the improvement in toughness.