碳纤维表面BAPPO改性及其复合材料界面耐原子氧性能研究
发布时间：2018-10-10 14:24
【摘要】：碳纤维/环氧树脂复合材料因其具有各项优异的性能被广泛的应用在各种航天器当中,但当航天器运行到近地太空轨道时会受到原子氧的侵蚀,所以原子氧的防护成为制约航天器存活时间的一项课题,近年来通过含芳香类苯磷氧结构(PPO)分子的引入对聚合物的耐原子氧性能有很大的提高。本文采用三种方法对碳纤维表面进行改性,并研究碳纤维与环氧树脂之间的界面耐原子氧性能:通过双(3-氨基苯基)苯基氧化膦(BAPPO)与环氧树脂复配的碳纤维表面上浆涂覆法,碳纤维表面化学接枝BAPPO法,碳纤维表面二元接枝POSS法。研究上浆涂覆法改性碳纤维复合材料界面性能,首先采用红外光谱,核磁共振谱对双(3-氨基苯基)苯基氧化膦(BAPPO)进行表征,通过SEM,IFSS以及单丝拉伸方法确定最佳上浆剂的浓度,得出当质量分数为1%时上浆剂对纤维的整体性能最好,其集束性,表面形貌最佳,界面剪切强度以及单丝拉伸强度最高,分别达到88.63MPa,3.31GPa比抽提的纤维分别提高了19.67%以及3.54%,表面能达到55.02m N/m,比抽提的纤维提高43.35%。研究化学接枝改性碳纤维复合材料界面性能,通过XPS,SEM等测试手段确定通过碳纤维接枝BAPPO的最佳反应质量分数,当BAPPO质量分数为3%时,P含量的达到3.23%,接枝效率最高,界面剪切强度提高了17.73%,单丝拉伸强度下降了5.79%,表面能提高了17.14%。研究碳纤维二元接枝POSS的最佳接枝时间,当POSS的质量分数为1%,反应时间为24h,接枝反应的Si含量最大,达到11.37%,Si/C比最大,界面剪切强度提高了15.84%,单丝拉伸下降了2.60%,表面能提高了21.76%。经过模拟空间原子氧暴露试验8h后,微复合材料界面性能经过比较可以发现,抽提后的碳纤维IFSS下降了16.65%,原丝的IFSS下降了13.33%。经过上浆后的IFSS下降了5.22%,经过BAPPO改性后的IFSS下降了1.63%,经过二元接枝POSS后,IFSS下降了3.95%。经过抽提后的IFSS下降比例最大,其次为T300原丝,然后为经过1%上浆涂覆后的碳纤维,二元接枝POSS后的碳纤维,BAPPO改性后的碳纤维,拉伸强度经过比较可以发现,原丝碳纤维,抽提碳纤维,上浆碳纤维下降比例依次变小,接枝BAPPO与接枝POSS的纤维拉伸强度基本没有发生改变。通过SEM,AFM,XPS分峰表征三种方法改性的碳纤维经过原子氧暴露的防护机理,通过SEM,AFM观察其表面形貌,发现经过上浆,接枝BAPPO以及二元接枝POSS的方法均在其表面形成不规则的厚度不均匀的膜,通过XPS分析得出,接枝BAPPO以及上浆的纤维经过AO暴露后表面均形成P-O类似于磷酯结构的膜作为防护层,二元接枝POSS的纤维经过AO暴露后,推测形成类似硅的氧化物以及磷的氧化物用于保护纤维界面层。
[Abstract]:Carbon fiber / epoxy composites have been widely used in various spacecraft because of their excellent properties. However, when the spacecraft is in low Earth orbit, it will be eroded by atomic oxygen. Therefore, the protection of atomic oxygen has become a problem that restricts the survival time of spacecraft. In recent years, the atomic oxygen resistance of polymers has been greatly improved through the introduction of aromatic phenophosphate oxygen (PPO) molecules. In this paper, the surface of carbon fiber was modified by three methods, and the interfacial atomic oxygen resistance between carbon fiber and epoxy resin was studied. The surface of carbon fiber was chemically grafted with BAPPO and the surface of carbon fiber was grafted with POSS. The interfacial properties of carbon fiber composites modified by sizing coating method were studied. Firstly, the Bis (3-aminophenyl) phenyl phosphine oxide (BAPPO) was characterized by IR and NMR spectra. The optimum sizing agent concentration was determined by SEM,IFSS and monofilament stretching method. The results show that when the mass fraction is 1, the sizing agent has the best overall properties, such as the best concentration, the best surface morphology, the highest interfacial shear strength and the highest tensile strength of monofilament. Compared with the extracted fiber, the fiber reached 88.63 MPA ~ 3.31 GPA and increased by 19.67% and 3.54, respectively, and the surface energy reached 55.02m N / m, and 43.35% higher than that of the extracted fiber. The interfacial properties of chemical grafted carbon fiber composites were studied. The optimum reaction mass fraction of BAPPO grafted with carbon fiber was determined by means of XPS,SEM. When the mass fraction of BAPPO was 3, the P content reached 3.23 and the grafting efficiency was the highest. The interfacial shear strength was increased by 17.73, the tensile strength of monofilament decreased by 5.79 and the surface energy increased by 17.14. When the mass fraction of POSS is 1 and the reaction time is 24 h, the content of Si is the largest, reaching 11.37 Si / C ratio, the interfacial shear strength is increased 15.84 and the tensile strength of monofilament decreases by 2.60 and the surface energy increases by 21.76. After 8 hours of simulated space atomic oxygen exposure test, the interfacial properties of the microcomposites were compared. It was found that the IFSS of the extracted carbon fiber decreased 16.65% and the IFSS of the precursor decreased 13.33%. After sizing, the IFSS decreased 5.22%, the IFSS modified by BAPPO decreased 1.63%, and the IFSS decreased 3.95% after binary grafting of POSS. After extraction, the IFSS decreased the most, followed by the T300 filament, then the carbon fiber coated with 1% sizing, the carbon fiber after binary grafted POSS, the carbon fiber modified by BAPPO, and the tensile strength of the precursor fiber was found by comparison. When the carbon fiber was extracted, the decreasing proportion of the sizing carbon fibers decreased in turn, while the tensile strength of the grafted BAPPO and POSS fibers remained unchanged. The protective mechanism of carbon fiber modified by SEM,AFM,XPS was characterized by atomic oxygen exposure. The surface morphology of carbon fiber modified by three methods was observed by SEM,AFM. The methods of grafted BAPPO and binary grafted POSS formed irregular and uneven films on their surfaces. The results of XPS analysis showed that the surface of grafted BAPPO and sizing fibers were exposed to AO to form P-O membrane similar to phosphate ester structure as a protective layer. After AO exposure to binary grafted POSS fibers, it is assumed that silicon-like oxides and phosphorous oxides are used to protect the interfacial layers of the fibers.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB332
本文编号：2262122
[Abstract]:Carbon fiber / epoxy composites have been widely used in various spacecraft because of their excellent properties. However, when the spacecraft is in low Earth orbit, it will be eroded by atomic oxygen. Therefore, the protection of atomic oxygen has become a problem that restricts the survival time of spacecraft. In recent years, the atomic oxygen resistance of polymers has been greatly improved through the introduction of aromatic phenophosphate oxygen (PPO) molecules. In this paper, the surface of carbon fiber was modified by three methods, and the interfacial atomic oxygen resistance between carbon fiber and epoxy resin was studied. The surface of carbon fiber was chemically grafted with BAPPO and the surface of carbon fiber was grafted with POSS. The interfacial properties of carbon fiber composites modified by sizing coating method were studied. Firstly, the Bis (3-aminophenyl) phenyl phosphine oxide (BAPPO) was characterized by IR and NMR spectra. The optimum sizing agent concentration was determined by SEM,IFSS and monofilament stretching method. The results show that when the mass fraction is 1, the sizing agent has the best overall properties, such as the best concentration, the best surface morphology, the highest interfacial shear strength and the highest tensile strength of monofilament. Compared with the extracted fiber, the fiber reached 88.63 MPA ~ 3.31 GPA and increased by 19.67% and 3.54, respectively, and the surface energy reached 55.02m N / m, and 43.35% higher than that of the extracted fiber. The interfacial properties of chemical grafted carbon fiber composites were studied. The optimum reaction mass fraction of BAPPO grafted with carbon fiber was determined by means of XPS,SEM. When the mass fraction of BAPPO was 3, the P content reached 3.23 and the grafting efficiency was the highest. The interfacial shear strength was increased by 17.73, the tensile strength of monofilament decreased by 5.79 and the surface energy increased by 17.14. When the mass fraction of POSS is 1 and the reaction time is 24 h, the content of Si is the largest, reaching 11.37 Si / C ratio, the interfacial shear strength is increased 15.84 and the tensile strength of monofilament decreases by 2.60 and the surface energy increases by 21.76. After 8 hours of simulated space atomic oxygen exposure test, the interfacial properties of the microcomposites were compared. It was found that the IFSS of the extracted carbon fiber decreased 16.65% and the IFSS of the precursor decreased 13.33%. After sizing, the IFSS decreased 5.22%, the IFSS modified by BAPPO decreased 1.63%, and the IFSS decreased 3.95% after binary grafting of POSS. After extraction, the IFSS decreased the most, followed by the T300 filament, then the carbon fiber coated with 1% sizing, the carbon fiber after binary grafted POSS, the carbon fiber modified by BAPPO, and the tensile strength of the precursor fiber was found by comparison. When the carbon fiber was extracted, the decreasing proportion of the sizing carbon fibers decreased in turn, while the tensile strength of the grafted BAPPO and POSS fibers remained unchanged. The protective mechanism of carbon fiber modified by SEM,AFM,XPS was characterized by atomic oxygen exposure. The surface morphology of carbon fiber modified by three methods was observed by SEM,AFM. The methods of grafted BAPPO and binary grafted POSS formed irregular and uneven films on their surfaces. The results of XPS analysis showed that the surface of grafted BAPPO and sizing fibers were exposed to AO to form P-O membrane similar to phosphate ester structure as a protective layer. After AO exposure to binary grafted POSS fibers, it is assumed that silicon-like oxides and phosphorous oxides are used to protect the interfacial layers of the fibers.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB332
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，本文编号：2262122
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