裂解工艺对先驱体转化制备Cf/SiC材料结构与性能的影响

以聚碳硅烷(PCS)/二乙烯基苯(DVB)为先驱体,经8个周期的反复真空浸渍-交联-裂解处理制备出三维编织碳纤维增强碳化硅(3D-B C_f/SiC)复合材料,考察了裂解工艺对材料结构与性能的影响。结果表明:提高裂解升温速率可以提高材料密度,形成较理想的界面结合,从而提高材料的力学性能。裂解温度对材料性能也有较大的影响,C_f/SiC复合材料在第6个周期采用1600℃ 裂解可以弱化纤维与基体之间的界面,提高材料致密度,材料的力学性能也得到较大改善。裂解升温速率为15℃/min,第6个周期采用1600℃裂解制备的C_f/SiC材料性能较好,弯曲强度达到556.7 MPa。      

3D Cf/SiC抗高温氧化复合材料的制备及其构件的工程试验

采用低分子量聚碳硅烷(PCS)通过先驱体浸渍裂解(PIP)工艺、化学气相沉积(CVD)和粉末烧结技术相结合制备了3D C_f/SiC抗高温氧化复合材料。运用FTIR、¹H-NMR、凝胶渗透色谱法(GPC)、热失重-差热(TGA-DTA)、X射线衍射仪(XRD)和透射电子显微镜(TEM)等手段研究了低分子量PCS的结构及其无机化过程。结果表明: PCS的主要结构为[—Si(CH₃,H)—CH₂—]n,数均分子量为420,陶瓷化产率为70％左右,在1 200 ℃时基本转化为微晶态的β-SiC;3D C_f/SiC复合材料及其构件具有较好的耐高温氧化性能。     

先驱体浸渍-裂解SiC界面改性涂层对气相渗硅3D-C_f/SiC复合材料力学性能的影响

界面改性涂层对调节复合材料的力学性能起到重要作用。特别是在气相渗硅(GSI)制备C_f/SiC复合材料时,合适的界面改性涂层一方面保护C纤维不受Si反应侵蚀,另一方面调节C纤维和SiC基体的界面结合状况。通过在3D-C纤维预制件中制备先驱体浸渍-裂解(PIP)SiC涂层来进行界面改性,研究了PIP-SiC涂层对GSI C_f/SiC复合材料力学性能的影响。结果表明:无涂层改性的GSI C_f/SiC复合材料力学性能较差,呈现脆性断裂特征,其弯曲强度、弯曲模量和断裂韧性分别为87.6 MPa、56.9GPa和2.1 MPa·m~(1/2)。具有PIP-SiC界面改性涂层的C_f/SiC复合材料力学性能得到改善,PIP-SiC涂层改性后,GSI C_f/SiC复合材料的弯曲强度、弯曲模量和断裂韧性随着PIP-SiC周期数的增加而降低,PIP-SiC为1个周期制备的GSI C_f/SiC复合材料的力学性能最高,其弯曲强度、弯曲模量、断裂韧性分别为185.2 MPa、91.1GPa和5.5 MPa·m~(1/2)。PIP-SiC界面改性涂层的作用机制主要体现在载荷传递和"阻挡"Si的侵蚀2个方面。     

PyC/SiC界面相对PIP法制备3D HTA C/SiC复合材料性能的影响

利用三维编织炭纤维预制件通过先驱体浸渍裂解法制备C／SiC复合材料。研究了热解碳（PyC）／SiC界面相对复合材料的微观结构和力学性能的影响。弯曲性能通过三点弯曲法测试，复合材料的断口和抛光面通过扫描电镜观察。结果表明：通过等温化学气相沉积法在纤维表面沉积PyC／SiC界面相以后，复合材料的三点抗弯强度从46MPa提高到247MPa。沉积界面的复合材料断口有明显的纤维拔出现象，纤维与基体之间的结合强度适当，起到了增韧作用；而未沉积界面相复合材料的断口光滑、平整，几乎没有纤维拔出，纤维在热解过程中受到严重的化学损伤，性能下降严重，材料表现为典型的脆性断裂。     

Study on microstructures and mechanical properties of short-carbon-fiber-reinforced SiC composites prepared by hot-pressing

Short-carbon-fiber-reinforced silicon carbide composites were prepared by hot-pressing with SiC powder, Polycarbosilane as precursor polymer and MgO–Al₂O₃–Y₂O₃ as sintering additives. The phase composition, microstructure and mechanical properties of the composites with different Polycarbosilane content were investigated. The results showed that, dense composites could be prepared at a relatively low temperature of 1800 °C via the liquid-phase-sintering mechanism and the highest mechanical property was obtained for the composites with 20 wt.% PCS and 8 wt.% sintering additives. The amorphous interphase formed during sintering process in the composites not only contributed to the densification of the composites, but also improved the fiber–matrix bonding. The nano-silicon carbide derived from Polycarbosilane, could also play a role of improving the relative density of the composites.     

Effects of microstructure on flexural strength of biomorphic C/SiC composites

Biomorphic C/SiC composites were fabricated from different kinds of wood by liquid silicon infiltration (LSI) following a two-step process. In the first-step, the wood is converted into carbon preforms by pyrolysis in a nitrogen atmosphere. The carbon preforms are then infiltrated by silicon melt at 1,560°C under vacuum to fabricate C/SiC composites. The mechanical properties of the C/SiC composites were characterized by flexural tests at ambient temperature, 1,000, and 1,300°C, and the relationship between mechanical properties and microstructure was analyzed. The flexural strength of the biomorphic composites was strongly dependent on the properties of the carbon preforms and the degree of silicon infiltration. The flexural strength increased with increasing SiC content and bulk density of composite, and with decreasing porosity in the C/SiC composite. An analysis of fractographs of fractured C/SiC composites showed a cleavage type fracture, indicating brittle fracture behavior.     

Cf/SiC复合材料表面沉积铱膜层工艺研究

为了进一步提高Cf/SiC复合材料的高温耐烧蚀性能,采用冷壁MOCVD工艺,对条型和管型Cf/SiC复合材料样品进行了金属铱膜层沉积。结果表明,在该工艺条件下,Cf/SiC复合材料的力学性能没有明显降低,沉积的金属铱膜呈白亮的金属色光泽。针对通氧沉积工艺中涂层氧含量较多的问题,通过对涂层进行后处理,使金属铱层的纯度大大提高,为获得高纯膜提供了新的工艺途径。     

Analysis of mechanical properties and SEM for laminated SiC/W composites

In this letter, it is reported that a laminated SiC/W composite has been developed using the hot pressing method. It is found that a chemical reaction between W and SiC occurs during the preparation process. Making use of SEM, the components within the sandwiched-in metal and the fracturing crack for the laminated SiC/W composite are determined. Testing mechanical properties of the laminated SiC/W composite indicates that fracture toughness increases while bending strength reduces, with an increase of the thickness of the sandwiched-in metal ranging from 10–50-μm thickness.     

RCLD工艺制备Cf/C、Cf/C-SiC复合材料的氧化性和力学性能

以碳毡为增强体，碳氢有机液体为前驱体，采用自行设计的快速化学液相沉积工艺（RCLD）制备了Cf/C、Cf/C-SiC复合材料；研究了不同密度的毡体和不同的沉积时间等因素对复合材料力学性能和氧化性的影响，根据材料结构特征分析了其影响机理．     

不同物相电沉积CNTs对C/SiC复合材料力学性能的影响

采用电沉积法与化学气相渗透(CVI)法将碳纳米管(CNTs)分别引入到碳纤维表面和SiC基体中,制得了不同物相电沉积CNTs的C/SiC复合材料(CNTs-C)/SiC和C/(CNTs-SiC)。研究了CNTs沉积物相对C/SiC复合材料力学性能的影响,分析了不同CNTs沉积物相的C/SiC复合材料的拉伸强度及断裂机制。结果表明:相较于未加CNTs的C/SiC复合材料,CNTs沉积到碳纤维表面的(CNTs-C)/SiC复合材料的拉伸强度提高了67.3%,断裂功提高了107.2%;而将CNTs引入到SiC基体中的C/(CNTs-SiC)复合材料的断裂功有所降低,拉伸强度也仅提高了6.9%,CNTs没有表现出明显的增强增韧效果;C/(CNTs-SiC)复合材料与传统的C/SiC复合材料有相似的断裂形貌特征,断裂拔出机制类似,主要为纤维增强增韧,CNTs的作用不明显。     

二维C/SiC复合材料准静态和动态拉伸力学性能

采用分离式Hopkinson拉杆装置和电子万能试验机研究了二维C/SiC复合材料在4种应变率（0.001、0.010、90.000和350.000 s-1）下的拉伸力学性能,计算并验证了动态试验中的应力平衡状态;采用SEM分析了复合材料在不同应变率下的破坏断口和失效机制;建立了复合材料包含损伤和应变率相关的本构方程。结果表明:二维C/SiC复合材料的应力-应变曲线都表现出非线性的特征。随着应变率的增加,二维C/SiC复合材料的拉伸强度从204 MPa增加到270 MPa,增加了33%,这表明复合材料的拉伸强度具有较强的应变率敏感性。复合材料在准静态和动态加载下表现出不同的破坏模式是由材料内部界面行为的应变率效应造成的。      

平纹编织SiC/SiC复合材料多尺度建模及强度预测

连续SiC纤维增强SiC基体复合材料（SiC/SiC）具有优异的高温力学性能、辐照稳定性及较低的氚渗透率,在核工程结构领域具有良好的应用前景,掌握其承载状态下的损伤演化和强度性能,对SiC/SiC复合材料的应用具有重要指导意义。本文基于平纹编织SiC/SiC复合材料的制备过程和组分材料分布的多尺度特性,考虑复合材料微观结构的局部近似周期性,建立了纤维丝尺度和纤维束尺度单胞模型。使用有限元分析软件对纤维丝尺度模型的弹性性能和强度性能进行预测,将这些性能参数代入纤维束尺度模型,引入Tsai-Wu失效准则,根据材料的不同失效模式并对失效单元进行方向性刚度折减,模拟了平纹编织SiC/SiC复合材料在单轴拉伸载荷下的渐进损伤过程。数值模拟曲线与试验曲线吻合较好,实现了对平纹编织SiC/SiC复合材料强度的有效预测。      

C/C坯体密度对2D C_f/SiC复合材料结构和性能的影响

通过理论计算,探究C_f/SiC复合材料密度与C/C坯体密度的相关性;而后采用碳纤维布叠层制作2D C/C坯体,经先驱体浸渍裂解工艺增密,制得密度分别为0.98、1.06、1.12g/cm~3的C/C坯体,通过液相渗硅法反应合成2DC_f/SiC复合材料,探究C/C坯体密度对其结构和性能的影响。与理论计算结果来对比。研究结果表明:试验结果与理论数学计算结果基本一致。随着C/C坯体密度的增加,C_f/SiC复合材料的密度出现先上升后下降的趋势,当C/C坯体密度大于0.98g/cm~3后,复合材料的弯曲强度随着C/C坯体密度的增加而降低,C/C坯体密度为0.98g/cm~3时,2DC_f/SiC复合材料结构和性能较优。     

不同应力水平下SiCf/SiC复合材料的损伤行为和机制研究

为提高对SiC_f/SiC复合材料在服役中失效机制的理解以及更合理地设计该类材料,通过声发射探测结合两种力学加载实验对该材料的损伤过程进行了评估与分析,并利用光学显微镜和扫描电子显微镜等手段对其损伤状态的演变进行了详细的表征和总结。实验结果表明,声发射技术可有效评估SiC_f/SiC复合材料的损伤程度,并用以分析特定加载应力水平下的损伤发展。研究表明:裂纹在较低的加载应力下(80 MPa)易在材料的原生缺陷附近或多种组分的边界处萌生,但对材料自身强度影响较小;较高的加载应力(≥100 MPa)则会使材料产生大尺度开裂,并与纤维发生相互作用进而降低材料的稳定性。SiC_f/SiC复合材料在递增的加载应力下会产生5种开裂形式以及纤维的断裂拔出和界面的脱粘等损伤行为。     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

3D C/SiC复合材料的热辐射性能

利用稳态量热计法和傅里叶红外光谱仪分别测定了3D C/SiC复合材料在90℃时的半球向总发射率和室温法向光谱反射率,研究了表面形貌、涂层厚度及高温氧化对3D C/SiC热辐射性能的影响。结果表明:3D C/SiC具有优异的热辐射性能,其总发射率可达0.83;随着SiC涂层厚度的增加,3D C/SiC总发射率先降低后上升;高温氧化后,3D C/SiC的热辐射性能有所提高。      

炭纤维增强C/SiC双基体复合材料的制备及性能(英文)

以针刺炭纤维整体毡为预制体,联用化学气相沉积法与熔融渗硅法制得炭纤维增强C/SiC双基体(C/C-SiC)复合材料;研究了C/C-Si材料的显微结构、力学性能和不同制动速度下的摩擦磨损性能及机理。结果表明:C/C-SiC材料具有适中的纤维/基体界面结合强度,弯曲强度和压缩强度分别达240MPa和210MPa,具有摩擦系数高(0.41～0.54),磨损小(0.02cm3/MJ),摩擦性能稳定等特点.随着制动速度提高,C/C-Si材料的摩擦磨损机制也随之变化:在低速制动条件下主要表现为磨粒磨损;中速时以黏着磨损为主;高速时以疲劳磨损和氧化磨损为主。     

高温热曝露对3D-C/SiC复合材料弯曲性能的影响

3D-C/SiC复合材料试样在空气介质中600℃、900℃和1300℃热曝露不同时间后,采用三点弯曲法测试了以室温弯曲弹性模量表征的损伤变化规律,并进行了SEM和EDS分析.结果表明:3D-C/SiC在热曝露15 h后,损伤变化可分为急剧上升(阶段Ⅰ)和平稳上升(阶段Ⅱ)两个阶段.阶段Ⅰ归因于炭纤维和炭层界面在空气中的直接氧化,阶段Ⅱ由复合材料内部氧的扩散所致.在复合材料制备过程的冷却阶段,因基体和炭纤维热膨胀系数不同所产生的基体微裂纹提供了氧化反应的表面与氧扩散的途径.在同一热曝露时间下,损伤随温度的上升而减少的原由可能是由于高温下裂纹收缩导致氧化表面减少,并降低氧向复合材料内扩散所致.     

Crack-healing and mechanical behaviour of Al2O3/SiC composites at elevated temperature

Alumina/silicon carbide (Al₂O₃/SiC) composite ceramics with large self‐crack‐healing ability, high strength and high heat‐resistance limit temperature for strength were developed and subjected to three‐point bending. A semicircular surface crack 100 μm in diameter was made on each sample. Crack‐healing behaviour was systematically studied, as functions of crack‐healing temperature and healing time, and the fatigue strengths of the crack‐healed sample at room temperature and 1373 K were investigated. Four main conclusions were drawn from the present study. (1) Al₂O₃/SiC composite ceramics have the ability to heal after cracking from 1273to 1673 K in air. (2) The heat‐resistance limit temperature for strength of the crack‐healed sample is ?1573 K, and ?68% of the samples fractured from outside the crack‐healed zone in the testing‐temperature range 873–1573 K. (3) The crack‐healed sample exhibited very high fatigue limit at room temperature and also 1373 K. (4) The large self‐crack‐healing ability is a desirable technique for the high structural integrity of ceramic component.     

Selective growth of SiC nanowires in interlaminar matrix for improving in-plane strengths of laminated Carbon/Carbon composites

β-SiC nanowires(SiCNWs) were selectively grown in the interlaminar matrix with a volume fraction of0.65% by applying a pyrocarbon coating on carbon fibers, which realizes the proper reinforcement of C/C composites. The thickness of the pyrocarbon is optimized to 0.5 μm based on the analysis of in-situ fiber strengths with the fracture mirror method. The pyrocarbon coating increased the in-situ fiber strength by~7% and prevent brittle fracture of the composites. Compared with C/C, the interlaminar shear and flexural strength of SiCNW-C/C(10.06 MPa and 162.44 MPa) increase by 158% and 57%. Incorporating SiCNWs changes the crystallite orientations and refines the crystallite size of pyrocarbon matrix. The functions of SiCNWs vary with their loading density. When SiCNWs are sufficient in the matrix, they help reinforcing and improving the critical failure stress of the matrix. When their density decreases to a certain degree, SiCNWs help changing the crystallite orientations of pyrocarbon and toughening the matrix.