反应浸渗制备连续纤维增强SiC基复合材料及其性能研究
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摘要
连续纤维增强SiC基复合材料（Cf/SiC和SiCf/SiC）具有高强度、高模量、耐高温、耐腐蚀、抗氧化、抗辐照和低活性等优异性能，已成为航空航天和核聚变等领域中较理想的高温结构及功能材料。目前，关于连续纤维增强SiC基复合材料制备工艺的研究主要集中在先驱体浸渍裂解（Polymer Impregnation andPyrolysis，PIP）、化学气相沉积（Chemical Vapor Infiltration，CVI）和纳米浸渍与瞬时共晶（Nano-Infiltrated Transient Eutectoid，NITE）等工艺，而对反应浸渗工艺（Reaction Infiltration，RI）的研究报道则相对较少。本论文开展了RI工艺制备连续纤维增强SiC基复合材料的研究，主要目的是为获得优异性能的连续纤维增强SiC基复合材料探索新的道路。
首先对碳基中间体进行设计与制备。通过对碳基中间体的临界密度和孔隙率的建模计算获得：不论是树脂碳（Resin Carbon, RC）还是热解碳（Pyrolytic Carbon,PyC），SiC纤维和C纤维增强的碳基中间体的临界密度分别为1.68g/cm3和1.36g/cm3；不论是SiC纤维还是C纤维，RC基和PyC基中间体的临界孔隙率分别为19%和26%，该临界密度和孔隙率利于反应浸渗工艺制备连续纤维增强SiC基复合材料。
采用化学气相沉积（Chemical Vapor Deposition, CVD）工艺分别在碳纤维和碳化硅纤维编织体中制备了厚度分别为0.2~0.3μm的PyC/SiC复合涂层，该复合涂层较连续、均匀、致密，同时涂层间分界清晰。PyC的层状结构即改善了纤维的表面状态，又为裂纹在涂层中的扩展提供了途径；SiC涂层的抗氧化性能则起到了保护纤维的作用。
采用浸渍碳化（Infiltration Carbonization, IC）工艺和CVI工艺制备了RC基和PyC基中间体。研究发现利用间苯二酚和甲醛合成的酚醛树脂溶液具有粘度低（25mPa S）、渗透效果好和浸渍/碳化效率高等优点。同时发现PyC较致密，其结构为典型短程有序、长程无序的乱层结构；而RC较疏松，其结构为明显的无序结构。
其次，对反应浸渗工艺进行热力学和动力学分析，结果表明：利用该工艺制备连续纤维增强SiC基复合材料是可行的；同时发现影响反应浸渗效果的主要因素包括硅及硅合金的物理性能（硅蒸气浓度及传质系数、硅合金的粘度、密度和表面张力）、硅合金与碳基中间体的润湿性、以及碳基中间体的孔径尺寸。提高硅蒸气浓度及传质系数、降低硅合金粘度和密度、增强其与中间体的润湿性均有利于增加反应速率、提高反应浸渗效果。
最终利用反应浸渗工艺制备了连续纤维增强SiC基复合材料，研究表明：在碳基中间体的密度和孔隙率接近临界密度和孔隙率的条件下，反应浸渗工艺制备连续纤维增强SiC基复合材料的性能最好。其中在1650℃、保温1h的条件下，SiCf/PyC、SiCf/RC和SiCf/PyC+RC经反应浸渗硅工艺制备的SiCf/SiC复合材料的最高弯曲强度和断裂韧性分别为301.2MPa和17.6MPa m1/2，144MPa和4.53MPa m1/2，342MPa和10.2MPa m1/2；在1550℃、保温0.5h的条件下，经反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金工艺制备SiCf/SiC复合材料的最高弯曲强度和断裂韧性分别为307.1MPa和17.8MPa m1/2，294MPa和18.3MPa m1/2，292.0MPa和18.1MPa m1/2。
当保温时间延长至60min，反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的SiCf/SiC复合材料的密度增大，孔隙率和残余硅含量均减小，弯曲强度和断裂韧性分别下降至188.9MPa和9.2MPa m1/2，178.9MPa和8.8MPa m1/2，184.1MPa和7.0MPa m1/2，其原因是延长保温时间加剧了SiC纤维的高温分解，降低了其性能，从而使SiCf/SiC复合材料的力学性能下降。
在浸渗温度为1450℃时，保温0.5h的条件下，反应浸渗Si-Ti合金制备的SiCf/SiC复合材料中生成TiC相；反应浸渗Si-Zr和Si-Zr-B合金，当温度高于1600℃时，SiCf/SiC复合材料中出现ZrC相。随着温度的升高，反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的SiCf/SiC复合材料中SiC、TiC和ZrC含量逐渐升高，力学性能先升高后降低。当浸渗温度为1650℃时，SiCf/SiC复合材料的力学性能最差，其弯曲强度和断裂韧性分别为61.6MPa和2.8MPa m1/2，38.1MPa和1.6MPa m1/2，38.6MPa和1.8MPa m1/2。这主要是由于反应放热造成了对SiC纤维的高温损伤，导致其性能下降。
石墨化处理使反应浸渗工艺制备Cf/SiC复合材料的性能得到了大幅提高。其中经反应浸渗硅工艺制备Cf/SiC复合材料的孔隙率从1.8%降低到0.7%，弯曲强度从170.7MPa提高到250MPa，断裂韧性从10.8MPa m1/2提高到13.3MPa m1/2；且反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的Cf/SiC复合材料的孔隙率分别从6.8%、7.2%和7.0%降低到1.6%、1.8%和1.4%，弯曲强度分别从195MPa、185MPa和190.1MPa提高到294MPa、252MPa和250.4MPa，而断裂韧性则稍有下降，分别从24.5MPa m1/2、22.6MPa m1/2和18.8MPa m1/2下降到20.1MPa m1/2、19.2MPa m1/2和17.7MPa m1/2。对碳纤维增强碳基中间体石墨化处理后，在1550℃、保温0.5h的条件下，反应浸渗Si-Zr和Si-Zr-B合金制备的Cf/SiC复合材料中反应生成了ZrC相。结果表明石墨化处理不仅提高了碳基中间体的孔隙率，增加了孔比表面积，从而提高了复合材料的致密度；同时提高了碳的结构有序性，增加了Si-C、Ti-C和Zr-C反应的反应活性，生成更多的SiC、TiC和ZrC。
利用SEM、TEM、HRTEM、EDX和SAED研究了反应浸渗工艺制备连续纤维增强SiC基复合材料的微观形貌、晶体结构和界面区域成分组成。结果表明：在1550℃浸渗温度下，SiC纤维中只有中间部分晶化，且纤维边缘有一层游离碳；PyC涂层则保持完好，呈现出短程有序结构；SiC涂层则与反应生成的基体结合在一起，且结晶程度较高；同时基体中主要由不同尺寸的大晶粒和纳米晶组成，因此经过1550℃反应浸渗硅合金获得的SiCf/SiC复合材料性能较好。在1650℃浸渗温度下，SiC纤维完全分解且晶化为纳米晶，且纤维边缘的游离碳和PyC涂层均被晶化为以SiC相为主的晶相；同时SiC涂层已完全与基体结合在一起，基体中的晶粒尺寸变大，因此1650℃反应浸渗硅合金获得的SiCf/SiC复合材料性能最差。
反应浸渗工艺的反应过程主要分为四步：首先固态Si及Si合金熔融生成Si蒸气或Si合金熔液，通过扩散渗入碳基中间体的孔隙；然后Si蒸气和Si合金熔液与基体碳接触并反应，生成连续致密的SiC层，直至将Si蒸气或Si合金熔液与基体碳分开；后续SiC、TiC和ZrC的生成主要通过Si、Ti、Zr和C元素在SiC层的扩散实现；最后随着SiC、TiC和ZrC的生长，碳基中间体中的孔隙尺寸不断减小，Si蒸气或Si合金熔液逐渐凝聚并填充碳基中间体中的剩余孔隙。其中Si蒸气或Si合金熔液与碳接触反应生成SiC的时间相对短暂，Si、Ti、Zr和C元素在SiC层的扩散控制着后续SiC、TiC和ZrC的生成。提高反应温度有助于提高这些反应元素的扩散速率，且同时降低Si-Ti、Si-Zr和Si-Zr-B合金中Si-Ti、Si-Zr的结合力，从而提高Si-C、Ti-C和Zr-C的反应程度，获得更多的SiC、TiC和ZrC。
Continuous fiber reinforced silicon carbide matrix composites (Cf/SiC andSiCf/SiC) have been considered as perfect high-temperature structural and functionalmaterials in aerospace and fusion fields due to their high strength, high modulus,excellent thermal stability, good corrosion resistance, oxidation resistance, irradiationresistance and low activity characteristics. Up to date, the studies on the fabricationmethods of continuous fiber reinforced silicon carbide matrix composites are mainlyfocused on the polymer impregnation and pyrolysis (PIP), chemical vapor infiltration(CVI) and nano-infiltrated transient eutectoid (NITE) process, the researches on thereaction infiltration (RI) are rather scarcely reported. In order to seek new fabricationroutes for continuous fiber reinforced silicon carbide matrix composites withoutstanding performance, the investigation for the continuous fiber reinforced siliconcarbide matrix composites fabricated by RI process are developed in this thesis.
Firstly, carbon matrix intermediate was designed and fabricated. According tothe modeling and calculating for the critical density and porosity of carbon matrixintermediate, it was found that either resin carbon (RC) or pyrolytic carbon (PyC), thecritical density of SiC and C fiber reinforced carbon matrix intermediate are1.68g/cm3and1.36g/cm3respectively; On the other hand, either SiC fiber or C fiber,the critical porosity of RC and PyC matrix intermediate are19%and26%respectively. The critical density and porosity are favorable for fabricating continuousfiber reinforced silicon carbide matrix composites by RI process.
The PyC/SiC multilayer coating with thickness of0.2~0.3μm were fabricated onthe suiface of C fiber and SiC fiber fabric by chemical vapor deposition (CVD)process. This multilayer coating is very continuous, uniform and compact. Moreover,the interface among the coating is very distinct. The PyC coating not only modifiesthe surface state of fibers, but also provides routes for the spread of micro-crackwithin the coating due to the sandwich of PyC. SiC coating protects the fibers becauseof its high oxidation resistance.
The carbon matrix intermediate was fabricated by infiltration carbonization (IC)and CVI process. It was found that the solution of phenolic resin synthesized byresorcinol and formaldehyde possess low viscosity (25mPa S), good infiltrationproperty and high efficiency of infiltration/carbonization. Moreover, it also indicatesthat the PyC is very compact with a typical turbostratic structure containing short range order and long range disorder. However, the RC is rather loose, and its structureis distinct disordered.
Secondly, the RI process was researched by thermodynamics and dynamicsanalysis. It was found that the fabrication of continuous fiber reinforced siliconcarbide matrix composites by RI process is feasible. The main factors affecting RIprocess comprise physical performance of Si and Si alloy (concentration and masstransfer coefficient of Si vapor, viscosity, density and surface tension of Si alloy),wettability of Si alloy with carbon matrix intermediate, and pore size of carbon matrixintermediate. Increasing the concentration and mass transfer coefficient of Si vapor,decreasing the viscosity, density and surface tension of Si alloy, and improving thewettability of Si alloy are all favorable to enhance reaction velocity and improveeffect of RI process.
Finally, continuous fiber reinforced silicon carbide matrix composites werefabricated by RI process. The results show that the properties of continuous fiberreinforced silicon carbide matrix composites fabricated by RI process are the bestwhen the density and porosity of carbon matrix intermediate are close to the criticaldensity and porosity. The maximal flexure strength and fracture toughness of SiCf/SiCfabricated by reaction infiltration Si process (1650℃,1h) using the intermediate ofSiCf/PyC, SiCf/RC and SiCf/PyC+RC are301.2MPa and17.6MPa m1/2,144MPa and4.53MPa m1/2,342MPa and10.2MPa m1/2, respectively. The maximal flexure strengthand fracture toughness of SiCf/SiC fabricated by reaction infiltration Si-Ti, Si-Zr andSi-Zr-B process (1550℃,0.5h) are307.1MPa and17.8MPa m1/2,294MPa and18.3MPa m1/2,292.0MPa and18.1MPa m1/2, repectively.
As the RI holding time extended to60min, the density of SiCf/SiC fabricated byreaction infiltration Si-Ti, Si-Zr and Si-Zr-B process increased, the porosity andresidual Si decreased. However, the flexure strength and fracture toughness declinedto188.9MPa and9.2MPa m1/2,178.9MPa and8.8MPa m1/2,184.1MPa and7.0MPa m1/2, respectively. It indicates that the decompositon of SiC fiber wasenhanced due to extending the holding time, therefore the SiC fiber was severelydamaged, the property of SiC fiber decreased sharply, accordingly the mechanicalproperties of SiCf/SiC decreased.
The TiC phase was formed in the SiCf/SiC fabricated by reaction infiltrationSi-Ti at the temperature of1450℃for0.5h.The ZrC phase was formed in theSiCf/SiC fabricated by reaction infiltration Si-Zr and Si-Zr-B only as the temperatureexceeding1600℃. The content of SiC, TiC and ZrC in the SiCf/SiC fabricated by reaction infiltration Si-Ti, Si-Zr and Si-Zr-B gradually increased as the temperaturerised, but the mechanical properties first increased, then decreased. The mechanicalproperties are the worst as the temperature is1650℃, the flexure strength and fracturetoughness were61.6MPa and2.8MPa m1/2,38.1MPa and1.6MPa m1/2,38.6MPa and1.8MPa m1/2. The reason is that the SiC fiber was damaged by exothermal reaction,which caused the SiC fiber acutely decomposed.
The properties of Cf/SiC fabricated by reaction infiltration process areremarkably improved after the carbon matrix intermediate being graphitized. Theporosity of Cf/SiC fabricated by reaction infiltration Si decreased from1.8%to0.7%,the flexure strength increased from170.7MPa to250MPa, and the fracture toughnessincreased from10.8MPa m1/2to13.3MPa m1/2. Additionally, the porosity of Cf/SiCfabricated by reaction infiltration Si-Ti, Si-Zr and Si-Zr-B decreased from6.8%,7.2%and7.0%to1.6%,1.8%and1.4%; the flexure strength increased from195MPa,185MPa and190.1MPa to294MPa,252MPa and250.4MPa; the fracture toughnessslightly decreased from24.5MPa m1/2,22.6MPa m1/2and18.8MPa m1/2to20.1MPa m1/2,19.2MPa m1/2and17.7MPa m1/2. It also reveales that after the carbonfiber reinforced carbon matrix intermediate being graphitized, the ZrC phase wasformed in the Cf/SiC fabricated by reaction infiltration Si-Zr and Si-Zr-B at thetemperature of1550℃for0.5h. The results show that the graphitizing not onlyimproved the porosity of the carbon matrix intermediate, increased the pore specificsurface area, thereby increased the density of composites; but also improved thestructural order of carbon, enhanced the reaction activity, sequentially more SiC, TiCand ZrC were formed.
The morphology, crystal structure and interfacial component of the continuousfiber reinforced silicon carbide matrix composites fabricated by RI process wereexamined by SEM, TEM, HRTEM, EDX and SAED. It was found that the interior ofSiC fiber crystalled at the temperature of1550℃, and free carbon layer existed on thesurface of SiC fiber. Moreover, PyC coating remained undamaged, and exhibitedshort range order. However, SiC coating combined with the SiC matrix, which iscomposed of high degree crystallized large-grains with different size-scale andnano-crystal, therefore, the properties of SiCf/SiC fabricated by reaction infiltration Sialloy at the temperature of1550℃are the best. It was also found that SiC fibercompletely decomposed and became nano-crystal at the temperature of1650℃.Furthermore, the free carbon on the surface of SiC fiber and the PyC coating becamecrystal. Additionally, SiC coating also combined with the reaction formed matrix, the grain size of the matrix increased, as a result, the properties of SiCf/SiC fabricated byreaction infiltration Si alloy at the temperature of1650℃are the worst.
The RI process could be divided into four steps: Firstly, solid Si and Si alloy aremelted into Si vapor and liquid Si alloy, which diffuse into the pore of carbon matrixintermediate; Secondly, Si vapor and liquid Si alloy contact and react with carbonmatrix, which form continuous and compact SiC layer until Si vapor and liquid Sialloy are detached to carbon matrix. Thirdly, the fomation of SiC, TiC and ZrC carryout by the diffusion of Si, Ti, Zr and C atom through the SiC layer. Finally, pore sizeof carbon matrix intermediate decrease as the forming of SiC, TiC and ZrC, and theresidual pore is filled through condensing of Si vapor and liquid Si alloy. The time ofSi vapor and liquid Si alloy contact and react with carbon matrix is very short, thediffusion of Si, Ti, Zr and C atom through the SiC layer dominate the formation ofSiC, TiC and ZrC. Improving the reaction temperature is helpful to increase thediffusion velocity and reduce the bonding force of Si-Ti, Si-Zr of Si alloy, whichcould enhance the degree of reaction. Accordingly, the content of SiC, TiC and ZrCwould be increased.
首先对碳基中间体进行设计与制备。通过对碳基中间体的临界密度和孔隙率的建模计算获得：不论是树脂碳（Resin Carbon, RC）还是热解碳（Pyrolytic Carbon,PyC），SiC纤维和C纤维增强的碳基中间体的临界密度分别为1.68g/cm3和1.36g/cm3；不论是SiC纤维还是C纤维，RC基和PyC基中间体的临界孔隙率分别为19%和26%，该临界密度和孔隙率利于反应浸渗工艺制备连续纤维增强SiC基复合材料。
采用化学气相沉积（Chemical Vapor Deposition, CVD）工艺分别在碳纤维和碳化硅纤维编织体中制备了厚度分别为0.2~0.3μm的PyC/SiC复合涂层，该复合涂层较连续、均匀、致密，同时涂层间分界清晰。PyC的层状结构即改善了纤维的表面状态，又为裂纹在涂层中的扩展提供了途径；SiC涂层的抗氧化性能则起到了保护纤维的作用。
采用浸渍碳化（Infiltration Carbonization, IC）工艺和CVI工艺制备了RC基和PyC基中间体。研究发现利用间苯二酚和甲醛合成的酚醛树脂溶液具有粘度低（25mPa S）、渗透效果好和浸渍/碳化效率高等优点。同时发现PyC较致密，其结构为典型短程有序、长程无序的乱层结构；而RC较疏松，其结构为明显的无序结构。
其次，对反应浸渗工艺进行热力学和动力学分析，结果表明：利用该工艺制备连续纤维增强SiC基复合材料是可行的；同时发现影响反应浸渗效果的主要因素包括硅及硅合金的物理性能（硅蒸气浓度及传质系数、硅合金的粘度、密度和表面张力）、硅合金与碳基中间体的润湿性、以及碳基中间体的孔径尺寸。提高硅蒸气浓度及传质系数、降低硅合金粘度和密度、增强其与中间体的润湿性均有利于增加反应速率、提高反应浸渗效果。
最终利用反应浸渗工艺制备了连续纤维增强SiC基复合材料，研究表明：在碳基中间体的密度和孔隙率接近临界密度和孔隙率的条件下，反应浸渗工艺制备连续纤维增强SiC基复合材料的性能最好。其中在1650℃、保温1h的条件下，SiCf/PyC、SiCf/RC和SiCf/PyC+RC经反应浸渗硅工艺制备的SiCf/SiC复合材料的最高弯曲强度和断裂韧性分别为301.2MPa和17.6MPa m1/2，144MPa和4.53MPa m1/2，342MPa和10.2MPa m1/2；在1550℃、保温0.5h的条件下，经反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金工艺制备SiCf/SiC复合材料的最高弯曲强度和断裂韧性分别为307.1MPa和17.8MPa m1/2，294MPa和18.3MPa m1/2，292.0MPa和18.1MPa m1/2。
当保温时间延长至60min，反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的SiCf/SiC复合材料的密度增大，孔隙率和残余硅含量均减小，弯曲强度和断裂韧性分别下降至188.9MPa和9.2MPa m1/2，178.9MPa和8.8MPa m1/2，184.1MPa和7.0MPa m1/2，其原因是延长保温时间加剧了SiC纤维的高温分解，降低了其性能，从而使SiCf/SiC复合材料的力学性能下降。
在浸渗温度为1450℃时，保温0.5h的条件下，反应浸渗Si-Ti合金制备的SiCf/SiC复合材料中生成TiC相；反应浸渗Si-Zr和Si-Zr-B合金，当温度高于1600℃时，SiCf/SiC复合材料中出现ZrC相。随着温度的升高，反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的SiCf/SiC复合材料中SiC、TiC和ZrC含量逐渐升高，力学性能先升高后降低。当浸渗温度为1650℃时，SiCf/SiC复合材料的力学性能最差，其弯曲强度和断裂韧性分别为61.6MPa和2.8MPa m1/2，38.1MPa和1.6MPa m1/2，38.6MPa和1.8MPa m1/2。这主要是由于反应放热造成了对SiC纤维的高温损伤，导致其性能下降。
石墨化处理使反应浸渗工艺制备Cf/SiC复合材料的性能得到了大幅提高。其中经反应浸渗硅工艺制备Cf/SiC复合材料的孔隙率从1.8%降低到0.7%，弯曲强度从170.7MPa提高到250MPa，断裂韧性从10.8MPa m1/2提高到13.3MPa m1/2；且反应浸渗Si-Ti、Si-Zr和Si-Zr-B合金制备的Cf/SiC复合材料的孔隙率分别从6.8%、7.2%和7.0%降低到1.6%、1.8%和1.4%，弯曲强度分别从195MPa、185MPa和190.1MPa提高到294MPa、252MPa和250.4MPa，而断裂韧性则稍有下降，分别从24.5MPa m1/2、22.6MPa m1/2和18.8MPa m1/2下降到20.1MPa m1/2、19.2MPa m1/2和17.7MPa m1/2。对碳纤维增强碳基中间体石墨化处理后，在1550℃、保温0.5h的条件下，反应浸渗Si-Zr和Si-Zr-B合金制备的Cf/SiC复合材料中反应生成了ZrC相。结果表明石墨化处理不仅提高了碳基中间体的孔隙率，增加了孔比表面积，从而提高了复合材料的致密度；同时提高了碳的结构有序性，增加了Si-C、Ti-C和Zr-C反应的反应活性，生成更多的SiC、TiC和ZrC。
利用SEM、TEM、HRTEM、EDX和SAED研究了反应浸渗工艺制备连续纤维增强SiC基复合材料的微观形貌、晶体结构和界面区域成分组成。结果表明：在1550℃浸渗温度下，SiC纤维中只有中间部分晶化，且纤维边缘有一层游离碳；PyC涂层则保持完好，呈现出短程有序结构；SiC涂层则与反应生成的基体结合在一起，且结晶程度较高；同时基体中主要由不同尺寸的大晶粒和纳米晶组成，因此经过1550℃反应浸渗硅合金获得的SiCf/SiC复合材料性能较好。在1650℃浸渗温度下，SiC纤维完全分解且晶化为纳米晶，且纤维边缘的游离碳和PyC涂层均被晶化为以SiC相为主的晶相；同时SiC涂层已完全与基体结合在一起，基体中的晶粒尺寸变大，因此1650℃反应浸渗硅合金获得的SiCf/SiC复合材料性能最差。
反应浸渗工艺的反应过程主要分为四步：首先固态Si及Si合金熔融生成Si蒸气或Si合金熔液，通过扩散渗入碳基中间体的孔隙；然后Si蒸气和Si合金熔液与基体碳接触并反应，生成连续致密的SiC层，直至将Si蒸气或Si合金熔液与基体碳分开；后续SiC、TiC和ZrC的生成主要通过Si、Ti、Zr和C元素在SiC层的扩散实现；最后随着SiC、TiC和ZrC的生长，碳基中间体中的孔隙尺寸不断减小，Si蒸气或Si合金熔液逐渐凝聚并填充碳基中间体中的剩余孔隙。其中Si蒸气或Si合金熔液与碳接触反应生成SiC的时间相对短暂，Si、Ti、Zr和C元素在SiC层的扩散控制着后续SiC、TiC和ZrC的生成。提高反应温度有助于提高这些反应元素的扩散速率，且同时降低Si-Ti、Si-Zr和Si-Zr-B合金中Si-Ti、Si-Zr的结合力，从而提高Si-C、Ti-C和Zr-C的反应程度，获得更多的SiC、TiC和ZrC。
Continuous fiber reinforced silicon carbide matrix composites (Cf/SiC andSiCf/SiC) have been considered as perfect high-temperature structural and functionalmaterials in aerospace and fusion fields due to their high strength, high modulus,excellent thermal stability, good corrosion resistance, oxidation resistance, irradiationresistance and low activity characteristics. Up to date, the studies on the fabricationmethods of continuous fiber reinforced silicon carbide matrix composites are mainlyfocused on the polymer impregnation and pyrolysis (PIP), chemical vapor infiltration(CVI) and nano-infiltrated transient eutectoid (NITE) process, the researches on thereaction infiltration (RI) are rather scarcely reported. In order to seek new fabricationroutes for continuous fiber reinforced silicon carbide matrix composites withoutstanding performance, the investigation for the continuous fiber reinforced siliconcarbide matrix composites fabricated by RI process are developed in this thesis.
Firstly, carbon matrix intermediate was designed and fabricated. According tothe modeling and calculating for the critical density and porosity of carbon matrixintermediate, it was found that either resin carbon (RC) or pyrolytic carbon (PyC), thecritical density of SiC and C fiber reinforced carbon matrix intermediate are1.68g/cm3and1.36g/cm3respectively; On the other hand, either SiC fiber or C fiber,the critical porosity of RC and PyC matrix intermediate are19%and26%respectively. The critical density and porosity are favorable for fabricating continuousfiber reinforced silicon carbide matrix composites by RI process.
The PyC/SiC multilayer coating with thickness of0.2~0.3μm were fabricated onthe suiface of C fiber and SiC fiber fabric by chemical vapor deposition (CVD)process. This multilayer coating is very continuous, uniform and compact. Moreover,the interface among the coating is very distinct. The PyC coating not only modifiesthe surface state of fibers, but also provides routes for the spread of micro-crackwithin the coating due to the sandwich of PyC. SiC coating protects the fibers becauseof its high oxidation resistance.
The carbon matrix intermediate was fabricated by infiltration carbonization (IC)and CVI process. It was found that the solution of phenolic resin synthesized byresorcinol and formaldehyde possess low viscosity (25mPa S), good infiltrationproperty and high efficiency of infiltration/carbonization. Moreover, it also indicatesthat the PyC is very compact with a typical turbostratic structure containing short range order and long range disorder. However, the RC is rather loose, and its structureis distinct disordered.
Secondly, the RI process was researched by thermodynamics and dynamicsanalysis. It was found that the fabrication of continuous fiber reinforced siliconcarbide matrix composites by RI process is feasible. The main factors affecting RIprocess comprise physical performance of Si and Si alloy (concentration and masstransfer coefficient of Si vapor, viscosity, density and surface tension of Si alloy),wettability of Si alloy with carbon matrix intermediate, and pore size of carbon matrixintermediate. Increasing the concentration and mass transfer coefficient of Si vapor,decreasing the viscosity, density and surface tension of Si alloy, and improving thewettability of Si alloy are all favorable to enhance reaction velocity and improveeffect of RI process.
Finally, continuous fiber reinforced silicon carbide matrix composites werefabricated by RI process. The results show that the properties of continuous fiberreinforced silicon carbide matrix composites fabricated by RI process are the bestwhen the density and porosity of carbon matrix intermediate are close to the criticaldensity and porosity. The maximal flexure strength and fracture toughness of SiCf/SiCfabricated by reaction infiltration Si process (1650℃,1h) using the intermediate ofSiCf/PyC, SiCf/RC and SiCf/PyC+RC are301.2MPa and17.6MPa m1/2,144MPa and4.53MPa m1/2,342MPa and10.2MPa m1/2, respectively. The maximal flexure strengthand fracture toughness of SiCf/SiC fabricated by reaction infiltration Si-Ti, Si-Zr andSi-Zr-B process (1550℃,0.5h) are307.1MPa and17.8MPa m1/2,294MPa and18.3MPa m1/2,292.0MPa and18.1MPa m1/2, repectively.
As the RI holding time extended to60min, the density of SiCf/SiC fabricated byreaction infiltration Si-Ti, Si-Zr and Si-Zr-B process increased, the porosity andresidual Si decreased. However, the flexure strength and fracture toughness declinedto188.9MPa and9.2MPa m1/2,178.9MPa and8.8MPa m1/2,184.1MPa and7.0MPa m1/2, respectively. It indicates that the decompositon of SiC fiber wasenhanced due to extending the holding time, therefore the SiC fiber was severelydamaged, the property of SiC fiber decreased sharply, accordingly the mechanicalproperties of SiCf/SiC decreased.
The TiC phase was formed in the SiCf/SiC fabricated by reaction infiltrationSi-Ti at the temperature of1450℃for0.5h.The ZrC phase was formed in theSiCf/SiC fabricated by reaction infiltration Si-Zr and Si-Zr-B only as the temperatureexceeding1600℃. The content of SiC, TiC and ZrC in the SiCf/SiC fabricated by reaction infiltration Si-Ti, Si-Zr and Si-Zr-B gradually increased as the temperaturerised, but the mechanical properties first increased, then decreased. The mechanicalproperties are the worst as the temperature is1650℃, the flexure strength and fracturetoughness were61.6MPa and2.8MPa m1/2,38.1MPa and1.6MPa m1/2,38.6MPa and1.8MPa m1/2. The reason is that the SiC fiber was damaged by exothermal reaction,which caused the SiC fiber acutely decomposed.
The properties of Cf/SiC fabricated by reaction infiltration process areremarkably improved after the carbon matrix intermediate being graphitized. Theporosity of Cf/SiC fabricated by reaction infiltration Si decreased from1.8%to0.7%,the flexure strength increased from170.7MPa to250MPa, and the fracture toughnessincreased from10.8MPa m1/2to13.3MPa m1/2. Additionally, the porosity of Cf/SiCfabricated by reaction infiltration Si-Ti, Si-Zr and Si-Zr-B decreased from6.8%,7.2%and7.0%to1.6%,1.8%and1.4%; the flexure strength increased from195MPa,185MPa and190.1MPa to294MPa,252MPa and250.4MPa; the fracture toughnessslightly decreased from24.5MPa m1/2,22.6MPa m1/2and18.8MPa m1/2to20.1MPa m1/2,19.2MPa m1/2and17.7MPa m1/2. It also reveales that after the carbonfiber reinforced carbon matrix intermediate being graphitized, the ZrC phase wasformed in the Cf/SiC fabricated by reaction infiltration Si-Zr and Si-Zr-B at thetemperature of1550℃for0.5h. The results show that the graphitizing not onlyimproved the porosity of the carbon matrix intermediate, increased the pore specificsurface area, thereby increased the density of composites; but also improved thestructural order of carbon, enhanced the reaction activity, sequentially more SiC, TiCand ZrC were formed.
The morphology, crystal structure and interfacial component of the continuousfiber reinforced silicon carbide matrix composites fabricated by RI process wereexamined by SEM, TEM, HRTEM, EDX and SAED. It was found that the interior ofSiC fiber crystalled at the temperature of1550℃, and free carbon layer existed on thesurface of SiC fiber. Moreover, PyC coating remained undamaged, and exhibitedshort range order. However, SiC coating combined with the SiC matrix, which iscomposed of high degree crystallized large-grains with different size-scale andnano-crystal, therefore, the properties of SiCf/SiC fabricated by reaction infiltration Sialloy at the temperature of1550℃are the best. It was also found that SiC fibercompletely decomposed and became nano-crystal at the temperature of1650℃.Furthermore, the free carbon on the surface of SiC fiber and the PyC coating becamecrystal. Additionally, SiC coating also combined with the reaction formed matrix, the grain size of the matrix increased, as a result, the properties of SiCf/SiC fabricated byreaction infiltration Si alloy at the temperature of1650℃are the worst.
The RI process could be divided into four steps: Firstly, solid Si and Si alloy aremelted into Si vapor and liquid Si alloy, which diffuse into the pore of carbon matrixintermediate; Secondly, Si vapor and liquid Si alloy contact and react with carbonmatrix, which form continuous and compact SiC layer until Si vapor and liquid Sialloy are detached to carbon matrix. Thirdly, the fomation of SiC, TiC and ZrC carryout by the diffusion of Si, Ti, Zr and C atom through the SiC layer. Finally, pore sizeof carbon matrix intermediate decrease as the forming of SiC, TiC and ZrC, and theresidual pore is filled through condensing of Si vapor and liquid Si alloy. The time ofSi vapor and liquid Si alloy contact and react with carbon matrix is very short, thediffusion of Si, Ti, Zr and C atom through the SiC layer dominate the formation ofSiC, TiC and ZrC. Improving the reaction temperature is helpful to increase thediffusion velocity and reduce the bonding force of Si-Ti, Si-Zr of Si alloy, whichcould enhance the degree of reaction. Accordingly, the content of SiC, TiC and ZrCwould be increased.
引文
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