原位生成中间相沥青增密C/C复合材料的研究
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摘要
C/C复合材料是由炭纤维增强炭基体组成，由于具有高导热性，低热膨胀系数，优良的摩擦性能及在极端条件下良好的性能表现使其成为一种具有广阔用途的先进复合材料。
中间相沥青具有高炭化收率，高密度和易石墨化等特点，是浸渍法增密C/C复合材料的优质炭基体前躯体。但是由于中间相沥青黏度很高会堵塞浸渍剂进入复合材料内部的通道，使材料内部的浸渍效果于低外部造成密度的不均一性。原位生成中间相沥青增密C/C复合材料是一种高效率，低成本的增密方法，可以有效解决致密化不均一的问题。原位增密的机理为：熔融的液态单体(纯多环芳烃如萘等)和催化剂渗入预制体的纤维束和孔洞中。当孔洞被完全填充后，原位热缩聚反应使单体转变为中间相沥青。经过随后的热缩聚和炭化处理，中间相沥青在预制体内转变为炭基体。
本工作研究了分别使用AlCl_3和ZrCl_4为催化剂催化聚合蒽制备光学各向异性含量高的优质中间沥青。考察了催化剂种类，催化剂添加量，反应温度及保温时间对中间相沥青形成与转化行为的影响。同时考察了AlCl_3和ZrCl_4在中间相沥青形成，炭化和石墨化过程的化学状态和转化行为。在以上研究的基础上确定了原位生成中间相沥青增密C/C复合材料的最佳工艺条件，制备出掺杂不同催化剂的C/C复合材料。对催化剂的残留和转化对C/C复合材料性能的影响进行了研究和分析。
在相同的反应条件下AlCl_3的催化活性优于ZrCl_4，而随着使用量的增加ZrCl_4的催化效果也会增加。使用AlCl_3为催化剂生成的中间相沥青具有更好的光学结构和更高的炭化收率。在一定的反应条件下，使用ZrCl_4为催化剂也可以制备出具有良好性能的中间性沥青。虽然使用ZrCl_4作为催化剂反应速度较使用AlCl_3慢，但是其反应体系内存在的大量的烷基侧链，环烷结构和小分子物质可以大大降低生成沥青的黏度。对比不同的反应温度发现在，350℃下可以得到性能更加优秀的中间相沥青。在经过炭化处理后，由于中间相沥青所含有的轻组分的挥发和逸出使微晶结构受到破坏，其结构参数会发生下降。
AlCl_3在经过沥青热缩聚反应后转变为非晶态的Al(OH)_3，其原因可能是由于AlCl_3与反应原料中的少量水反应。在经过炭化处理后部分Al(OH)_3分解为Al_2O_3，但两者都为非晶态物质无法从XRD谱图中检测到。在以上过程中AlCl_3的转化使其在1000℃热处理后仍然可以保存在沥青中，但是进一步的石墨化处理使含Al物质完全消失。ZrCl_4在经过沥青热缩聚反应后转变为t-ZrO_2。在进一步炭化处理后t-ZrO_2晶体结构进一步完善并有部分t-ZrO_2转变为m-ZrO_2。在石墨化处理后，大部分ZrO_2与碳反应生成ZrC，部分则生成碳氧化锆(ZrCxOy)。由于在炭化和石墨化过程中ZrCl_4转变为相对稳定的ZrO_2，ZrC和碳氧化锆，使催化剂完整地保留在了沥青炭中。在石墨化过程中生成的ZrC能够促进石墨结构的生长。由于AlCl_3和ZrCl_4转变为氧化物与氢氧化物，Cl元素则以不稳定的Cl-状态吸附于催化剂的表面，随着热处理温度的升高Cl元素最终逸出。
在350℃进行三次原位增密后，使用不同催化剂(AlCl_313wt.%，ZrCl_413wt.%，ZrCl_420wt.%)的低密度和高密度C/C复合材料的表观密度由初始编织体的0.625g/cm3和1.715g/cm3分别提升到1.289g/cm3，1.383g/cm3，1.373g/cm3和1.790g/cm3，1.810g/cm3，1.798g/cm3。使用AlCl_3为催化剂的增密效果较使用ZrCl_4低，这是由于AlCl_3的催化活性很高使体系粘度快速上升，从而大大降低了浸渍效率。经过三次原位增后，低密度C/C复合材料的抗弯强度由低于5MPa分别上升至74.1Ma，68.3MPa和55.0MPa。而高密度复合材料的抗弯强度则由101.5MPa上升至200.8MPa，234.5MPa和220.6MPa，虽然高密度C/C复合材料增密效果只有5%左右，但是强度增加量达到100%以上。低密度复合材料的力学性能随ZrCl_4使用量的提高而下降，这是由于在炭化处理过程中ZrO_2晶粒的长大及晶型转化破坏了炭基体的结构所致。由于高密度C/C复合材料中催化剂的含量很低，其力学性能在ZrCl_4含量的上升时保持不变。
含Zr催化剂的残留会对炭基体微晶结构产生破坏，使材料的导电性能下降。在低温下C/C复合材料的抗氧化性能主要由其密度因素决定，具有更高密度的样品其内部缺陷更少，抗氧化性能也相应提高。虽然ZrO_2颗粒的存在会部分降低复合材料的力学性能，但是由于其可以与碳反应生成ZrC进而极大提高C/C复合材料的抗烧蚀性能，因此通过原位增密制备的ZrO_2和ZrC掺杂的C/C复合材料将拥有广阔的前景。
Carbon/carbon (C/C) composites, consisting of carbon matrix reinforcedwith carbon fibers, are advanced materials that have widespread applicationsattributed to their superior mechanical properties, high thermal conductivity,low thermal expansion, excellent friction properties and good performanceunder extreme conditions.
Mesophase pitch, with high carbon yeild, high density and highgraphitizability, can be used as good precursor of carbon matrix in makingC/C composites. But due to its high viscosity, the mesophase pitch blocks theaccess channels to the inner part of the preform. The extent of mesophasepenetration decreases from the outer edge to the center of the composites,resulting in non-uniform filling. The in situ mesophase transformation indensification of C/C composites is a new, efficient, and low-cost process toaddress this issue. The mechanism of the process is that the mixture of moltenmonomer (pure aromatic hydrocarbons such as naphthalene) and catalyst easily penetrate fiber bundles and void space of the preform. When thepreform is completely filled, the in situ poly-condensation leads the monomerto mesophase pitches. After poly-condensation and carbonization, mostmesophase pitches retained in the preform are transformed into carbon matrix.
In this work, mesophase pitches were prepared by the aid of AlCl_3andZrCl_4as catalyst. We investigated the effect of catalysts, temperature andholding time on the mesophase formation and transformation behavior. Thechemical state and transformation behavior of catalyst during carbonizationand graphitization were also investigated. On the basis of the above researchwe found the optimum conditions for in situ mesophase transformation indensification of C/C composites. The C/C composites doped with catalystswere prepared and characterized. The effect of retained catalyst andtransformation of catalyst on the properties of C/C composites were alsostudied in detail.
Under the same conditions, the catalytic activity of AlCl_3was superior tothat of ZrCl_4, and with increasing the amount of ZrCl_4, the catalytic effect alsoincreased. AlCl_3could make the mesophase pitches have better opticalstructure and higher carbonization yield. In certain conditions, the mesophasepitches with good optical texture could also be prepared by useing ZrCl_4ascatalyst. Although the poly-condensation reaction rate of samples using ZrCl_4was much slower than that using AlCl_3, the large amount of small moleculesand alkyl groups in the pitches greatly decreased the viscosity of the pitches. After comparing different reaction temperatures, we found that mesophasepitches with best properties were obtained at350℃. The volatilization of lightcomponent in mesophase pitches easily destroyed the microcrystallinestructure of the samples during carbonization.
After poly-condensation, AlCl_3was transformed into amorphous Al(OH)_3,this may be due to the reaction between AlCl_3and a small amount of waterwithin the raw materials. After carbonizing, a part of Al(OH)_3was transformedinto Al_2O_3, but both substances were amorphous, which can not be detectedfrom XRD patterns. In the above process, AlCl_3was transformed into othersubstance, so it was saved after heat treatment at1000℃. After graphitizationall the Al containing substance was completely removed. ZrCl_4wastransformed into t-ZrO_2druing poly-condensation, and the crystal structure oft-ZrO_2was improved and some of t-ZrO_2was transformed into m-ZrO_2aftercarbonization. During graphitization, a majority of ZrO_2was transformed intoZrC, others transformed to zirconium oxycarbide (ZrCxOy). Since ZrCl_4wastransformed into ZrO_2, ZrC and zirconium oxycarbide after carbonization andgraphitization, the Zr containing catalyst perfectly retained in the pitches. TheZrC generated during graphitization promoted the growth of graphite structure.While the AlCl_3and ZrCl_4were converted into the oxides and hydroxides, theCl element was transformed into unstable Cl-ions, which adsorbed at thesurface of catalyst. With increasing the temperature, the Cl elementseventually disappear.
After three in situ desification at350℃using different catalysts (AlCl_313wt%, ZrCl_413wt%, ZrCl_420wt.%), the bulk density of low and high densityC/C composites increased from0.625g/cm3and1.715g/cm3to1.289g/cm3,1.383g/cm3,1.373g/cm3and1.790g/cm3,1.810g/cm3,1.798g/cm3, respectively.Due to the higher catalytic activity of AlCl_3, the high viscosity greatly reducedthe efficiency of the impregnation process, which made the densificationefficiency using AlCl_3was much lower than that using ZrCl_4. After three insitu densification, the flexural strength of low density composites rose fromlower than5MPa to74.1Ma,68.3MPa and55.0MPa, while the flexuralstrength of high density composites increased from101.5MPa to200.8MPa,234.5MPa and220.6MPa, respectively. Although the densification efficiencyof high density C/C composites was only about5%, the flexural strengthincreased more than100%. The mechanical properties of low densitycomposites decreased when increasing ZrCl_4content. This is because thegrowth of ZrO_2grain and phase transformation of ZrO_2during carbonizationdestroyed the carbon matrix structure, which decreased the mechanicalproperties of the composites. Attributed to the very low content of catalyst incomposites, the mechanical properties of high density composites did notchange when the content of ZrCl_4increased.
Due to the retained Zr-containing catalysts brought damage to themicrocrystalline structure of the carbon matrix, the electrical conductivity ofthe composites decreased. The oxidation properties of the C/C composites at low temperatures were mainly determined by their density, the higher densityand fewer defects increased the oxidation resistance. Although the ZrO_2particles partly reduced the mechanical properties of the composite, it couldreact with carbon into ZrC, which would greatly reduce the ablation rates ofC/C composites. The ZrO_2and ZrC doped C/C composites fabricated throughin situ mesophase transformation will have broad applications.
中间相沥青具有高炭化收率，高密度和易石墨化等特点，是浸渍法增密C/C复合材料的优质炭基体前躯体。但是由于中间相沥青黏度很高会堵塞浸渍剂进入复合材料内部的通道，使材料内部的浸渍效果于低外部造成密度的不均一性。原位生成中间相沥青增密C/C复合材料是一种高效率，低成本的增密方法，可以有效解决致密化不均一的问题。原位增密的机理为：熔融的液态单体(纯多环芳烃如萘等)和催化剂渗入预制体的纤维束和孔洞中。当孔洞被完全填充后，原位热缩聚反应使单体转变为中间相沥青。经过随后的热缩聚和炭化处理，中间相沥青在预制体内转变为炭基体。
本工作研究了分别使用AlCl_3和ZrCl_4为催化剂催化聚合蒽制备光学各向异性含量高的优质中间沥青。考察了催化剂种类，催化剂添加量，反应温度及保温时间对中间相沥青形成与转化行为的影响。同时考察了AlCl_3和ZrCl_4在中间相沥青形成，炭化和石墨化过程的化学状态和转化行为。在以上研究的基础上确定了原位生成中间相沥青增密C/C复合材料的最佳工艺条件，制备出掺杂不同催化剂的C/C复合材料。对催化剂的残留和转化对C/C复合材料性能的影响进行了研究和分析。
在相同的反应条件下AlCl_3的催化活性优于ZrCl_4，而随着使用量的增加ZrCl_4的催化效果也会增加。使用AlCl_3为催化剂生成的中间相沥青具有更好的光学结构和更高的炭化收率。在一定的反应条件下，使用ZrCl_4为催化剂也可以制备出具有良好性能的中间性沥青。虽然使用ZrCl_4作为催化剂反应速度较使用AlCl_3慢，但是其反应体系内存在的大量的烷基侧链，环烷结构和小分子物质可以大大降低生成沥青的黏度。对比不同的反应温度发现在，350℃下可以得到性能更加优秀的中间相沥青。在经过炭化处理后，由于中间相沥青所含有的轻组分的挥发和逸出使微晶结构受到破坏，其结构参数会发生下降。
AlCl_3在经过沥青热缩聚反应后转变为非晶态的Al(OH)_3，其原因可能是由于AlCl_3与反应原料中的少量水反应。在经过炭化处理后部分Al(OH)_3分解为Al_2O_3，但两者都为非晶态物质无法从XRD谱图中检测到。在以上过程中AlCl_3的转化使其在1000℃热处理后仍然可以保存在沥青中，但是进一步的石墨化处理使含Al物质完全消失。ZrCl_4在经过沥青热缩聚反应后转变为t-ZrO_2。在进一步炭化处理后t-ZrO_2晶体结构进一步完善并有部分t-ZrO_2转变为m-ZrO_2。在石墨化处理后，大部分ZrO_2与碳反应生成ZrC，部分则生成碳氧化锆(ZrCxOy)。由于在炭化和石墨化过程中ZrCl_4转变为相对稳定的ZrO_2，ZrC和碳氧化锆，使催化剂完整地保留在了沥青炭中。在石墨化过程中生成的ZrC能够促进石墨结构的生长。由于AlCl_3和ZrCl_4转变为氧化物与氢氧化物，Cl元素则以不稳定的Cl-状态吸附于催化剂的表面，随着热处理温度的升高Cl元素最终逸出。
在350℃进行三次原位增密后，使用不同催化剂(AlCl_313wt.%，ZrCl_413wt.%，ZrCl_420wt.%)的低密度和高密度C/C复合材料的表观密度由初始编织体的0.625g/cm3和1.715g/cm3分别提升到1.289g/cm3，1.383g/cm3，1.373g/cm3和1.790g/cm3，1.810g/cm3，1.798g/cm3。使用AlCl_3为催化剂的增密效果较使用ZrCl_4低，这是由于AlCl_3的催化活性很高使体系粘度快速上升，从而大大降低了浸渍效率。经过三次原位增后，低密度C/C复合材料的抗弯强度由低于5MPa分别上升至74.1Ma，68.3MPa和55.0MPa。而高密度复合材料的抗弯强度则由101.5MPa上升至200.8MPa，234.5MPa和220.6MPa，虽然高密度C/C复合材料增密效果只有5%左右，但是强度增加量达到100%以上。低密度复合材料的力学性能随ZrCl_4使用量的提高而下降，这是由于在炭化处理过程中ZrO_2晶粒的长大及晶型转化破坏了炭基体的结构所致。由于高密度C/C复合材料中催化剂的含量很低，其力学性能在ZrCl_4含量的上升时保持不变。
含Zr催化剂的残留会对炭基体微晶结构产生破坏，使材料的导电性能下降。在低温下C/C复合材料的抗氧化性能主要由其密度因素决定，具有更高密度的样品其内部缺陷更少，抗氧化性能也相应提高。虽然ZrO_2颗粒的存在会部分降低复合材料的力学性能，但是由于其可以与碳反应生成ZrC进而极大提高C/C复合材料的抗烧蚀性能，因此通过原位增密制备的ZrO_2和ZrC掺杂的C/C复合材料将拥有广阔的前景。
Carbon/carbon (C/C) composites, consisting of carbon matrix reinforcedwith carbon fibers, are advanced materials that have widespread applicationsattributed to their superior mechanical properties, high thermal conductivity,low thermal expansion, excellent friction properties and good performanceunder extreme conditions.
Mesophase pitch, with high carbon yeild, high density and highgraphitizability, can be used as good precursor of carbon matrix in makingC/C composites. But due to its high viscosity, the mesophase pitch blocks theaccess channels to the inner part of the preform. The extent of mesophasepenetration decreases from the outer edge to the center of the composites,resulting in non-uniform filling. The in situ mesophase transformation indensification of C/C composites is a new, efficient, and low-cost process toaddress this issue. The mechanism of the process is that the mixture of moltenmonomer (pure aromatic hydrocarbons such as naphthalene) and catalyst easily penetrate fiber bundles and void space of the preform. When thepreform is completely filled, the in situ poly-condensation leads the monomerto mesophase pitches. After poly-condensation and carbonization, mostmesophase pitches retained in the preform are transformed into carbon matrix.
In this work, mesophase pitches were prepared by the aid of AlCl_3andZrCl_4as catalyst. We investigated the effect of catalysts, temperature andholding time on the mesophase formation and transformation behavior. Thechemical state and transformation behavior of catalyst during carbonizationand graphitization were also investigated. On the basis of the above researchwe found the optimum conditions for in situ mesophase transformation indensification of C/C composites. The C/C composites doped with catalystswere prepared and characterized. The effect of retained catalyst andtransformation of catalyst on the properties of C/C composites were alsostudied in detail.
Under the same conditions, the catalytic activity of AlCl_3was superior tothat of ZrCl_4, and with increasing the amount of ZrCl_4, the catalytic effect alsoincreased. AlCl_3could make the mesophase pitches have better opticalstructure and higher carbonization yield. In certain conditions, the mesophasepitches with good optical texture could also be prepared by useing ZrCl_4ascatalyst. Although the poly-condensation reaction rate of samples using ZrCl_4was much slower than that using AlCl_3, the large amount of small moleculesand alkyl groups in the pitches greatly decreased the viscosity of the pitches. After comparing different reaction temperatures, we found that mesophasepitches with best properties were obtained at350℃. The volatilization of lightcomponent in mesophase pitches easily destroyed the microcrystallinestructure of the samples during carbonization.
After poly-condensation, AlCl_3was transformed into amorphous Al(OH)_3,this may be due to the reaction between AlCl_3and a small amount of waterwithin the raw materials. After carbonizing, a part of Al(OH)_3was transformedinto Al_2O_3, but both substances were amorphous, which can not be detectedfrom XRD patterns. In the above process, AlCl_3was transformed into othersubstance, so it was saved after heat treatment at1000℃. After graphitizationall the Al containing substance was completely removed. ZrCl_4wastransformed into t-ZrO_2druing poly-condensation, and the crystal structure oft-ZrO_2was improved and some of t-ZrO_2was transformed into m-ZrO_2aftercarbonization. During graphitization, a majority of ZrO_2was transformed intoZrC, others transformed to zirconium oxycarbide (ZrCxOy). Since ZrCl_4wastransformed into ZrO_2, ZrC and zirconium oxycarbide after carbonization andgraphitization, the Zr containing catalyst perfectly retained in the pitches. TheZrC generated during graphitization promoted the growth of graphite structure.While the AlCl_3and ZrCl_4were converted into the oxides and hydroxides, theCl element was transformed into unstable Cl-ions, which adsorbed at thesurface of catalyst. With increasing the temperature, the Cl elementseventually disappear.
After three in situ desification at350℃using different catalysts (AlCl_313wt%, ZrCl_413wt%, ZrCl_420wt.%), the bulk density of low and high densityC/C composites increased from0.625g/cm3and1.715g/cm3to1.289g/cm3,1.383g/cm3,1.373g/cm3and1.790g/cm3,1.810g/cm3,1.798g/cm3, respectively.Due to the higher catalytic activity of AlCl_3, the high viscosity greatly reducedthe efficiency of the impregnation process, which made the densificationefficiency using AlCl_3was much lower than that using ZrCl_4. After three insitu densification, the flexural strength of low density composites rose fromlower than5MPa to74.1Ma,68.3MPa and55.0MPa, while the flexuralstrength of high density composites increased from101.5MPa to200.8MPa,234.5MPa and220.6MPa, respectively. Although the densification efficiencyof high density C/C composites was only about5%, the flexural strengthincreased more than100%. The mechanical properties of low densitycomposites decreased when increasing ZrCl_4content. This is because thegrowth of ZrO_2grain and phase transformation of ZrO_2during carbonizationdestroyed the carbon matrix structure, which decreased the mechanicalproperties of the composites. Attributed to the very low content of catalyst incomposites, the mechanical properties of high density composites did notchange when the content of ZrCl_4increased.
Due to the retained Zr-containing catalysts brought damage to themicrocrystalline structure of the carbon matrix, the electrical conductivity ofthe composites decreased. The oxidation properties of the C/C composites at low temperatures were mainly determined by their density, the higher densityand fewer defects increased the oxidation resistance. Although the ZrO_2particles partly reduced the mechanical properties of the composite, it couldreact with carbon into ZrC, which would greatly reduce the ablation rates ofC/C composites. The ZrO_2and ZrC doped C/C composites fabricated throughin situ mesophase transformation will have broad applications.
引文
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