碳纤维增强树脂基复合材料表面功能涂层制备研究

发布时间：2018-07-13 15:43

【摘要】：本研究旨在提高碳纤维增强树脂基复合材料在特殊应用下的耐特殊介质腐蚀能力,采用等离子体表面技术在碳纤维增强树脂基复合材料表面进行功能涂层的制备。为了克服碳纤维增强树脂基复合材料表面极性弱、表面膜层结合强度低等缺点,先使用霍尔源放电等离子体对碳纤维增强树脂基复合材料进行表面活化处理,以提高其表面极性和浸润性,再通过直流磁控溅射技术在碳纤维增强树脂基复合材料表面低温制备Al涂层。设计不同等离子体处理工艺,改变等离子体类型,通过接触角测试、拉伸试验、金相分析、扫描电镜分析和红外光谱分析,对比等离子体处理前后碳纤维增强树脂基复合材料表面浸润性、表面形貌、力学性能和表面官能团的变化,并探究等离子体处理碳纤维增强树脂基复合材料的最佳工艺。利用X射线衍射(XRD)和扫描电子显微镜(SEM)分析碳纤维增强树脂基复合材料表面Al涂层组织结构,自行设计垂直拉伸装置测定涂层与基体间的结合强度,并探究不同等离子体处理功率和处理前后不同涂层厚度对膜基结合强度的影响。通过耐含氟介质腐蚀性实验,对比Al涂层制备前后碳纤维增强树脂基复合材料的耐含氟介质腐蚀能力,结果表明： (1)等离子体处理后碳纤维增强树脂基复合材料与蒸馏水的接触角明显降低,表面浸润性和自由能显著提高。等离子体处理效果与工艺参数和等离子体类型密切相关,接触角随处理电流、气压的增加先降低后上升,随处理时间的延长先迅速降低后趋于稳定,当处理电流为1A、气压为1Pa、处理时间为10min时,接触角达到极小值,表面浸润性最佳。相同工艺参数下,不同类型等离子体处理效果依次为：O2N2Ar。 (2)经等离子体处理后,碳纤维增强树脂基复合材料表面的处理效果存在时效性,即随着放置时间的延长处理效果下降。等离子体处理时效性与气体源和保存环境有关,常温去离子水中保存可提高时效性,氧等离子体处理后时效性较好,氩等离子体次之,氮等离子体最差。 (3)金相显微镜和SEM观察可知,等离子体处理后碳纤维增强树脂基复合材料表面吸附的杂质小颗粒明显减少,刻蚀痕迹明显,表面粗糙度增加,纤维树脂间粘连程度增加。红外光谱分析结果显示,氩等离子体处理后,碳纤维增强树脂基复合材料表面C-C数量减少,C-O数量增加,同时酯基数量减少,酮基、羧基和醇羟基数量相应增加；氧等离子体处理后CH2-O-CH2吸收峰强度增大；氮等离子体处理后出现C=N和C≡N两个较明显的含氮吸收峰。 (4)等离子体处理后,Al涂层与碳纤维增强树脂基复合材料间结合强度显著上升,且随处理电流的增大先上升再降低,在电流为1A时最佳。膜基结合强度随涂层厚度增加而降低的趋势减弱,在涂层厚度达到25um时,膜基结合强度仍较大,为2.88MPa,而未经等离子体处理时仅为1.22MPa。 (5)耐含氟介质腐蚀性实验表明,Al涂层制备后碳纤维增强树脂基复合材料在含氟介质中的平均腐蚀速率为4.17×10-3g/m2.h-1,相比较Al涂层制备前的3.78×10-2g/m2·h-1,减小了一个量级,耐含氟介质腐蚀能力显著提高。
[Abstract]:The purpose of this study is to improve the specific corrosion resistance of carbon fiber reinforced resin matrix composites in special applications. The preparation of functional coatings on the surface of carbon fiber reinforced resin matrix composites by plasma surface technology is used to overcome the weak surface polarity of carbon fiber reinforced resin matrix composites and the bonding strength of the surface film layer. The surface activation of carbon fiber reinforced resin matrix composites was first treated with Holzer source discharge plasma to improve the surface polarity and wettability. The Al coating was prepared at low temperature on the surface of carbon fiber reinforced resin matrix composites by DC magnetron sputtering. Different plasma treatment processes were designed and changed. By means of contact angle test, tensile test, metallographic analysis, scanning electron microscope analysis and infrared spectrum analysis, the surface wettability, surface morphology, mechanical properties and surface functional groups of carbon fiber reinforced resin matrix composites are compared before and after plasma treatment, and the plasma treatment of carbon fiber reinforced resin matrix composites is also explored. X ray diffraction (XRD) and scanning electron microscope (SEM) were used to analyze the structure of Al coating on the surface of carbon fiber reinforced resin matrix composites. The bonding strength between the coating and the substrate was measured by the self designed vertical drawing device, and the strength of different plasma treatment and the bonding strength of different coating thickness to the film base before and after treatment were investigated. The corrosion resistance of carbon fiber reinforced resin matrix composites before and after the preparation of Al coating was compared. The results showed that the corrosion resistance of carbon fiber reinforced resin matrix composites before and after preparation was compared.
(1) the contact angle of the carbon fiber reinforced resin matrix composites and the distilled water decreased obviously after the plasma treatment, and the surface wettability and free energy increased significantly. The plasma treatment effect was closely related to the process parameters and plasma types. The contact angle increased first and then increased with the treatment current. When the current is 1A, the pressure is 1Pa, the treatment time is 10min, the contact angle reaches the minimum and the surface wettability is the best. Under the same process parameters, the effect of different types of plasma treatment is: O2N2Ar.
(2) after the plasma treatment, the treatment effect of the carbon fiber reinforced resin matrix composite surface has the aging effect, that is, the treatment effect decreases with the prolongation of the storage time. The aging property of the plasma treatment is related to the gas source and the preservation environment. The storage of the atmospheric deionized water can be raised to the high aging property, and the aging property after the oxygen plasma treatment is better. The argon plasma is the second, and the nitrogen plasma is the worst.
(3) the metallographic microscope and SEM observation show that the small particles adsorbed on the surface of the carbon fiber reinforced resin matrix composites after the plasma treatment are obviously reduced, the etching marks are obvious, the surface roughness is increased and the degree of adhesion between the fiber resin is increased. The infrared spectrum analysis results show that the carbon fiber reinforced resin matrix composite after the argon plasma treatment. The number of C-C on the surface of the material is reduced, the number of C-O increases, the number of ester groups decreases, the number of ketones, carboxyl and alcohol hydroxyl increases, and the peak intensity of CH2-O-CH2 absorption increases after the treatment of oxygen plasma, and there are two obvious nitrogen absorption peaks of C=N and C N after the treatment of nitrogen plasma.
(4) after plasma treatment, the bonding strength between the Al coating and the carbon fiber reinforced resin matrix composites increases significantly, and increases first and then decreases with the increase of the treatment current. The film base binding strength decreases with the increase of the coating thickness. When the coating thickness reaches 25um, the adhesion strength of the film base is still larger, which is 2.88M. Pa, and only 1.22MPa. without plasma treatment
(5) the corrosion resistance test of fluorine resistant medium shows that the average corrosion rate of the carbon fiber reinforced resin matrix composites in the fluorine containing medium after the preparation of Al coating is 4.17 x 10-3g/m2.h-1, compared with 3.78 x 10-2g/m2 / H-1 before the preparation of Al coating, which is reduced by one order of magnitude and the corrosion resistance of fluorine resistant medium is significantly improved.
【学位授予单位】：中国科学技术大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ327.3;TB33

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