碳纤维表面能、表面粗糙度及化学组成的表征
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摘要
碳纤维具有高强度、高模量、耐疲劳等优异性能,碳纤维作为复合材料的增强体已经被广泛地应用于飞机、导弹、汽车部件等众多领域。碳纤维表面特征对碳纤维及其复合材料的性能有很大的影响。本课题确立稳定地表征碳纤维表面能、表面粗糙度、化学组成的测试方法、研究国产碳纤维与T300表面的特征、碳纤维表面特征随制备复合材料过程中的工艺温度的变化。
确定稳定的碳纤维表面特征的测试方法,以便能够得到真实的碳纤维表面特征。在碳纤维表面能的测试方法中,采用表面界面张力仪进行测试,分别研究制样方法和测试过程所采用的参数对测试结果的影响。在碳纤维表面粗糙度的测试方法中,采用原子力显微镜(AFM)进行测试,系统地研究了扫描次数以及测试过程中所采用的扫描面积这两方面因素对测试结果的影响,并借助激光共聚焦显微镜,最终确定了较好的测试参数。在碳纤维表面化学组成的测试方法中,采用X射线光电子能谱(XPS)进行测试,通过对测试结果重复性和刻蚀趋势两方面进行研究,最终确定测试过程中样品状态和采用的仪器参数。
在已确定的稳定的测试方法的基础上,系统地研究国产碳纤维和T300的表面能、表面能的极性和色散分量、表面形貌、表面粗糙度以及表面化学组成等表面特征。研究结果表明,不同批次碳纤维的性能有所不同。对于性能较稳定的批次的碳纤维,国产碳纤维表面能的极性分量小于T300。国产碳纤维和T300表面都有数目众多的沟槽,且分布较均匀;二者粗糙度属于同一水平。国产碳纤维表面的C、Si含量大于T300表面的C、Si,而O、N含量小于T300表面的O、N。国产碳纤维本体的O、Si含量大于T300本体中的O、Si含量,而C、N含量小于T300本体结构中的C、N含量。通过对C1s谱进行分峰拟合,得到两种碳纤维表面官能团主要有-C-C-、-C-O-和-O-C=O三种,其中国产碳纤维表面-C-C-含量要高于T300表面官能团的含量,而-O-C=O含量却低于T300。
研究在复合材料制备工艺过程中,碳纤维表面能、表面形貌、表面粗糙度及化学组成随温度的变化趋势。结果表明,国产碳纤维和T300的表面能均随着处理温度的升高,先升高而后降低。国产碳纤维表面粗糙度随处理温度的升高而增大,在200℃时粗糙度最大,而T300表面沟槽数目随处理温度的升高,先增加后减少,在180℃时粗糙度最大。两种碳纤维表面元素含量随温度的升高而发生变化,当温度达到180℃时,表面C含量最低,O含量最高。
研究在碳纤维复合材料制备工艺过程中,碳纤维的力学性能所发生的变化。通过单丝拉伸实验和Weibull分布研究了国产碳纤维和T300单丝强度随处理温度的变化。结果表明,国产碳纤维的拉伸强度受温度的影响较大,T300的单丝拉伸强度受温度影响比较小。
Carbon fiber and its composites have been widely used in aircraft, missiles, automobile parts and many other fields, because of its high strength, high modulus and excellent fatigue performance. Surface characteristics can influence the properties of carbon fibers and their composites. of In the work, the methods to measure surface energy, surface roughness and chemical component of carbon fiber stably were determined. The differences between surface properties of domestic carbon fiber and Japanese carbon fiber (T300) have been investigated. Then the relationship between the processing temperatures and surface properties of domestic and T300 carbon fibers were also studied.
The methods of testing the surface characteristics were determined in the work. In the method to test the surface energy of carbon fiber, the surface tensionmeter was used. Effects of the specimen preparing method and testing parameters on results were systematically studied. Finally, the specimen preparing method was standardized and the testing parameters were determined. The roughness of carbon fiber was tested by atom force microscope (AFM). In the roughness method, the optimum scanning area was determined assisted with laser scanning confocal microscope. The chemical component of carbon fiber was tested by X-ray photoelectron spectroscopy (XPS). Through the study of tested repeatability and the trend of etching, the state of sample and instrument paramenters were determined.
Based on the determined stable methods, a systematic analysis of surface energy, polar parts and dispersive parts, surface morphology, roughness and chemical component of domestic carbon fiber and T300 was studied. Different blocks of carbon fibers had different surface characteristics. For the blocks of carbon fiber with stable characteristics, the polar surface energy of domestic carbon fiber was lower than that of T300. It was not favorable for the well wettability between domestic carbon fiber and resin during preparing composite materials. It was found that there were a number of grooves which uniformly dispersed on their surface. The depth of grooves on the surface of domestic carbon fiber was smaller than that of T300. The results of roughness measured by AFM showed that the roughness of domestic carbon fiber and T300 belonged to one range. The chemical characteristic comparison of two kinds of fibers was investigated by XPS. The results showed that the element contents of domestic carbon fiber were C, Si, which were higher than C、Si of T300. O, N of domestic carbon fiber were lower than O, N of T300. In order to investigate differences in the bodies of them, surface etching has been done. It was found that O, Si element contents of domestic carbon fiber were higher than O, Si of T300 and the other element contents were lower. Contents of functional groups were calculated by fitting C1s spectra. The results showed that there were three kinds of function groups (-C-C-, -C-O-, -O-C=O)on the surface of carbon fiber. The -C-C- content of domestic carbon fiber was higher than that of T300 and the -O-C=O content was lower.
The changes of surface characteristics of carbon fiber treated in manufacturing process of composites were determined. Carbon fibers were treated with programmed controlled temperature experiment which was aimed to simulate actual process of manufacturing composite materials. Taking manufacturing process of CF/BMI composite for example, three temperature stages were chosen, 150℃, 180℃, 200℃. The results showed that the surface energies of domestic carbon fiber and T300 treated at 150℃were highest. Combined with SEM and AFM images, it was found that the roughness of domestic carbon fiber went higher as the treating temperature rose. The roughness of T300 increased when the temperature was lower than 180℃and decreased when it was higher than 180℃. Element contents of the two types of carbon fibers changed after they were treated at different temperatures. Treated at 180℃, the C contents on the surface of both domestic carbon fiber and T300 were lowest, but the O contents were highest.
Change of mechanical properties of carbon fiber with manufacturing process of composites was studied. The relationship between filament tensile strength and treating temperatures was investigated by filament strength test and Weibull distribution models. The results showed that tensile strength of domestic carbon fiber was influenced more obviously than that of T300.
确定稳定的碳纤维表面特征的测试方法,以便能够得到真实的碳纤维表面特征。在碳纤维表面能的测试方法中,采用表面界面张力仪进行测试,分别研究制样方法和测试过程所采用的参数对测试结果的影响。在碳纤维表面粗糙度的测试方法中,采用原子力显微镜(AFM)进行测试,系统地研究了扫描次数以及测试过程中所采用的扫描面积这两方面因素对测试结果的影响,并借助激光共聚焦显微镜,最终确定了较好的测试参数。在碳纤维表面化学组成的测试方法中,采用X射线光电子能谱(XPS)进行测试,通过对测试结果重复性和刻蚀趋势两方面进行研究,最终确定测试过程中样品状态和采用的仪器参数。
在已确定的稳定的测试方法的基础上,系统地研究国产碳纤维和T300的表面能、表面能的极性和色散分量、表面形貌、表面粗糙度以及表面化学组成等表面特征。研究结果表明,不同批次碳纤维的性能有所不同。对于性能较稳定的批次的碳纤维,国产碳纤维表面能的极性分量小于T300。国产碳纤维和T300表面都有数目众多的沟槽,且分布较均匀;二者粗糙度属于同一水平。国产碳纤维表面的C、Si含量大于T300表面的C、Si,而O、N含量小于T300表面的O、N。国产碳纤维本体的O、Si含量大于T300本体中的O、Si含量,而C、N含量小于T300本体结构中的C、N含量。通过对C1s谱进行分峰拟合,得到两种碳纤维表面官能团主要有-C-C-、-C-O-和-O-C=O三种,其中国产碳纤维表面-C-C-含量要高于T300表面官能团的含量,而-O-C=O含量却低于T300。
研究在复合材料制备工艺过程中,碳纤维表面能、表面形貌、表面粗糙度及化学组成随温度的变化趋势。结果表明,国产碳纤维和T300的表面能均随着处理温度的升高,先升高而后降低。国产碳纤维表面粗糙度随处理温度的升高而增大,在200℃时粗糙度最大,而T300表面沟槽数目随处理温度的升高,先增加后减少,在180℃时粗糙度最大。两种碳纤维表面元素含量随温度的升高而发生变化,当温度达到180℃时,表面C含量最低,O含量最高。
研究在碳纤维复合材料制备工艺过程中,碳纤维的力学性能所发生的变化。通过单丝拉伸实验和Weibull分布研究了国产碳纤维和T300单丝强度随处理温度的变化。结果表明,国产碳纤维的拉伸强度受温度的影响较大,T300的单丝拉伸强度受温度影响比较小。
Carbon fiber and its composites have been widely used in aircraft, missiles, automobile parts and many other fields, because of its high strength, high modulus and excellent fatigue performance. Surface characteristics can influence the properties of carbon fibers and their composites. of In the work, the methods to measure surface energy, surface roughness and chemical component of carbon fiber stably were determined. The differences between surface properties of domestic carbon fiber and Japanese carbon fiber (T300) have been investigated. Then the relationship between the processing temperatures and surface properties of domestic and T300 carbon fibers were also studied.
The methods of testing the surface characteristics were determined in the work. In the method to test the surface energy of carbon fiber, the surface tensionmeter was used. Effects of the specimen preparing method and testing parameters on results were systematically studied. Finally, the specimen preparing method was standardized and the testing parameters were determined. The roughness of carbon fiber was tested by atom force microscope (AFM). In the roughness method, the optimum scanning area was determined assisted with laser scanning confocal microscope. The chemical component of carbon fiber was tested by X-ray photoelectron spectroscopy (XPS). Through the study of tested repeatability and the trend of etching, the state of sample and instrument paramenters were determined.
Based on the determined stable methods, a systematic analysis of surface energy, polar parts and dispersive parts, surface morphology, roughness and chemical component of domestic carbon fiber and T300 was studied. Different blocks of carbon fibers had different surface characteristics. For the blocks of carbon fiber with stable characteristics, the polar surface energy of domestic carbon fiber was lower than that of T300. It was not favorable for the well wettability between domestic carbon fiber and resin during preparing composite materials. It was found that there were a number of grooves which uniformly dispersed on their surface. The depth of grooves on the surface of domestic carbon fiber was smaller than that of T300. The results of roughness measured by AFM showed that the roughness of domestic carbon fiber and T300 belonged to one range. The chemical characteristic comparison of two kinds of fibers was investigated by XPS. The results showed that the element contents of domestic carbon fiber were C, Si, which were higher than C、Si of T300. O, N of domestic carbon fiber were lower than O, N of T300. In order to investigate differences in the bodies of them, surface etching has been done. It was found that O, Si element contents of domestic carbon fiber were higher than O, Si of T300 and the other element contents were lower. Contents of functional groups were calculated by fitting C1s spectra. The results showed that there were three kinds of function groups (-C-C-, -C-O-, -O-C=O)on the surface of carbon fiber. The -C-C- content of domestic carbon fiber was higher than that of T300 and the -O-C=O content was lower.
The changes of surface characteristics of carbon fiber treated in manufacturing process of composites were determined. Carbon fibers were treated with programmed controlled temperature experiment which was aimed to simulate actual process of manufacturing composite materials. Taking manufacturing process of CF/BMI composite for example, three temperature stages were chosen, 150℃, 180℃, 200℃. The results showed that the surface energies of domestic carbon fiber and T300 treated at 150℃were highest. Combined with SEM and AFM images, it was found that the roughness of domestic carbon fiber went higher as the treating temperature rose. The roughness of T300 increased when the temperature was lower than 180℃and decreased when it was higher than 180℃. Element contents of the two types of carbon fibers changed after they were treated at different temperatures. Treated at 180℃, the C contents on the surface of both domestic carbon fiber and T300 were lowest, but the O contents were highest.
Change of mechanical properties of carbon fiber with manufacturing process of composites was studied. The relationship between filament tensile strength and treating temperatures was investigated by filament strength test and Weibull distribution models. The results showed that tensile strength of domestic carbon fiber was influenced more obviously than that of T300.
引文
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