聚合物涂层对等离子体处理有机纤维表面及复合材料界面性能的影响
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摘要
高性能有机纤维,如对苯撑苯并二嗯唑(PBO)纤维、芳纶(如Twaron)纤维等,因其卓越的拉伸强度、模量、韧性和优异的耐高温、抗冲击等性能,受到了越来越多的关注。而高性能有机纤维增强热塑性树脂基复合材料则具有较高的断裂韧性、损伤容限、抗冲击性能以及良好的可加工性能。常应用于航空航天、国防军工等高技术领域。但是因为PBO纤维和Twaron纤维都具有表面光滑,缺少极性基团,表面化学惰性等特点,使得其很难与树脂基体产生优良的粘结,造成其增强含二氮杂萘结构聚醚砜酮(PPESK)树脂基复合材料的界面粘结强度很差,导致复合材料的力学性能不能充分发挥。因此,需要对芳纶和PBO纤维表面进行改性,以改变其表面化学性能和表面物理形貌,提高其表面浸润性能,最终有效地提高复合材料的界面粘结性能。
本文用射频感应耦合等离子体(ICP)对PBO和Twaron纤维进行表面处理,随即进行聚合物涂层处理,采用红外光谱(FTIR)、X-射线光电子能谱(XPS)、原子力显微镜(AFM)、扫描电子显微镜(SEM)及动态接触角测试(DCAA)等分析测试手段分析了经聚合物涂层处理前后纤维的表面化学性能、物理形貌以及表面浸润性的变化关系进行测试。采用层间剪切强度(ILSS)、吸湿率和SEM对复合材料的界面粘结强度、耐湿热性能和断面形貌进行分析,并探讨了改性后界面粘结强度改善的机制。
论文以复合材料的ILSS为评价标准,通过正交试验法讨论了涂层液浓度及氧气等离子体放电参数对环氧树脂涂层改性PBO增强PPESK复合材料力学性能的影响。确定最佳工艺条件为：放电时间10min、放电功率为100W、放电气压为30Pa、涂层液浓度为3%。研究表明,涂层改性明显地改善了PBO纤维的表面性能、加大了表面粗糙度,提高了其表面自由能,有利于其与基体树脂的润湿。最终,复合材料的ILSS有了56.3%的提高,吸湿率降低了27.3%,材料的破坏模式也从界面脱粘转变为本体破坏。
用氧气等离子体处理了PBO纤维表面,并用PEK-C和PES-C两种热塑性树脂对纤维进行涂层改性。XPS结果显示两种聚合物涂层处理后的PBO纤维表面氧元素含量升高,且引入了酯基、羰基或者砜基等活性基团。纤维的表面粗糙程度加大,表面自由能提高。PBO/PPESK复合材料的ILSS显著加大,其中PEK-C涂层处理后复合材料的ILSS增大了80.7%,复合材料的吸湿总量和吸湿速率都明显降低。热塑性树脂涂层可以与扩散的PPESK基体分子发生物理缠结作用产生了强大的粘结力,同时,涂层与纤维表面又有着强的化学作用,最终实现了复合材料界面性能的改善。
本文使用氧气等离子体引发环氧树脂涂层对Twaron纤维的表面进行了改性,将经过相同等离子体处理条件下的纤维浸泡在不同浓度的涂层溶液中,发现1wt%的涂层溶液处理后的复合材料的ILSS值最高。涂层分子与纤维表面分子发生了化学键合,C-N基团含量降低、C=O等基团消失,同时出现了大量的C-O基团,这使得纤维表面的极性和反应活性增强,导致纤维的表面自由能提高。系统分析了不同放电时间和功率下,纤维的表观物理形貌和复合材料的界面粘结强度的变化。处理时间过长、放电功率过大都可能导致Twaron纤维表面刻蚀过重而导致复合材料界面粘结强度的下降。结果发现在放电功率为100W,放电时间为10min下,复合材料的ILSS值最高,且此时的吸湿率最低。
论文系统研究了氩气等离子体引发环氧树脂涂层改性对Twaron纤维表面性能影响,及各种放电参数对材料界面性能的影响。大量C-O基团被引入到纤维的表面,改性后的纤维形貌更为复杂,一层树脂覆盖在纤维的表面。纤维的表面自由能由49.9mJ/m2提高到了61.8mJ/m2。不同放电时间和功率条件下,复合材料的ILSS不同,在100W、10min和30Pa下,ILSS达到66.2MPa,增幅达68.9%。经过等离子体处理后的纤维表面,在涂层改性过程中会有大量环氧树脂分子沉积在纤维表面,复合材料的制备过程中,PPESK分子扩散到环氧树脂层中,在模压高温下,环氧树脂发生固化,形成束缚层使得纤维不易在剪切力作用下发生滑移,因而有利于ILSS的提高。
High-performance organic fibers have got much more attentions, due to their excellent strength, modulus, toughness and outstanding resistance to high temperature and shock. The high-performance organic fiber reinforced thermoplastic composites were usually used in the areas of aerospace and modern national defense owing to the high fracture toughness, damage tolerance, impact resistance and good processability. However, the surfaces of Twaron fiber and poly (p-phenylene benzobisoxazole)(PBO) fiber are smooth, lack of polar groups and chemical inert. Thus, the interfacial adhesion is usually poor between the fiber and matrix, which restrict the mechanical properties of the composites. Therefore, surface modification of organic fiber is necessary, to improve the surface chemical properties and morphologies, to increase the surface free energy, and to enhance the interfacial adhesion of the composite.
In this thesis, the PBO and Twaron fibers were treated by inductively coupled gas plasma (ICP) and immediately coated in the polymer solutions. The surface chemical properties, surface morphologies and the surface free energies of the fibers before and after coating were examined by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), and dynamic contact angle analysis (DCAA). The interlaminar shear strength (ILSS), moisture absorption and SEM were selected to determine the interfacial adhesion strength, water absorption and the interlaminar shear fracture morphologies of the composites. The mechanisms of the enhancement of the interfacial adhesion by thermoset and thermoplastic coatings were discussed.
Optimal treatment condition was obtained using the orthogonal design, which could be stated as:the concentration of the coating resin is3%, the plasma power is100W, the treatment time is10min and the discharge pressure is30Pa. Oxygen-plasma-induced coating could modify the surface properties of PBO fibers, roughen the fiber surface and increase the surface free energy. The ILSS was improved significantly, moisture absorption was lower than the untreated sample, and the fracture mode was changed from interface debonding to matrix fracture.
To improve the interfacial adhesion of PBO/PPESK composite, thermoplastic resins were coated onto the fiber surface after oxygen plasma pretreatment. Phenolphthalein poly (ether ketone)(PEK-C) and phenolphthalein poly (ether sulfone)(PES-C) were selected to be the coating resins. The XPS results showed that after the two resins coated the concentration of oxygen was increased, and the O=C-O, C=O or O=S=O were introduced onto the fiber surface. The fiber surfaces were roughened and the surface wettabilities were improved. After coating, the primary failure mode of the composites was changed from interface debonding to matrix fracture. The enhancement of the interface may be attributed to the stronger molecular entanglement. The matrix molecules physically to entangle with or diffuse into the molecular network of polymer coatings applied on the fibers. Therefore, the interfacial adhesion was enhanced.
Epoxy resin was selected to coat onto the surface of Twaron fibers induced by the oxygen plasma. The highest ILSS value was got when the concentration of epoxy resin was1wt%under the same plasma discharge condition. The concentration of C-N decreased, and the C=O group was disappeared; meanwhile the C-O group was appeared on the fiber surface with a concentration of22.4%. The polarity of the fiber surface was improved and the surface free energy was increased. Too long plasma treatment time and too high discharge power could damage the fiber body, which may lead to the damage of the interfacial adhesion of the fiber and matrix.
Argon-plasma-induced epoxy resin coating onto the Twaron fiber surface in order to modify the fiber surface properties. C-O group was introduced onto the fiber and the morphologies of the fiber surface were much more complex after coating. A thin and inhomogeneous layer of coating resins had been deposited onto the fiber surface. The surface free energy was improved from49.9to61.8mJ/m2. The optimal treatment condition was that the plasma power was100W, the treatment time was10min and the discharge pressure was30Pa. The coating layer was nonuniform and most of the epoxy resins were still small molecules before compression molding. Hence, the PPESK molecules may dive into the epoxy coating layers during the solution impregnation. Therefore, the coating layer acted as a bridge between the fibers and the matrices. After compression modlding, the cured epoxy resin bounded the fibers to improve the ILSS.
本文用射频感应耦合等离子体(ICP)对PBO和Twaron纤维进行表面处理,随即进行聚合物涂层处理,采用红外光谱(FTIR)、X-射线光电子能谱(XPS)、原子力显微镜(AFM)、扫描电子显微镜(SEM)及动态接触角测试(DCAA)等分析测试手段分析了经聚合物涂层处理前后纤维的表面化学性能、物理形貌以及表面浸润性的变化关系进行测试。采用层间剪切强度(ILSS)、吸湿率和SEM对复合材料的界面粘结强度、耐湿热性能和断面形貌进行分析,并探讨了改性后界面粘结强度改善的机制。
论文以复合材料的ILSS为评价标准,通过正交试验法讨论了涂层液浓度及氧气等离子体放电参数对环氧树脂涂层改性PBO增强PPESK复合材料力学性能的影响。确定最佳工艺条件为：放电时间10min、放电功率为100W、放电气压为30Pa、涂层液浓度为3%。研究表明,涂层改性明显地改善了PBO纤维的表面性能、加大了表面粗糙度,提高了其表面自由能,有利于其与基体树脂的润湿。最终,复合材料的ILSS有了56.3%的提高,吸湿率降低了27.3%,材料的破坏模式也从界面脱粘转变为本体破坏。
用氧气等离子体处理了PBO纤维表面,并用PEK-C和PES-C两种热塑性树脂对纤维进行涂层改性。XPS结果显示两种聚合物涂层处理后的PBO纤维表面氧元素含量升高,且引入了酯基、羰基或者砜基等活性基团。纤维的表面粗糙程度加大,表面自由能提高。PBO/PPESK复合材料的ILSS显著加大,其中PEK-C涂层处理后复合材料的ILSS增大了80.7%,复合材料的吸湿总量和吸湿速率都明显降低。热塑性树脂涂层可以与扩散的PPESK基体分子发生物理缠结作用产生了强大的粘结力,同时,涂层与纤维表面又有着强的化学作用,最终实现了复合材料界面性能的改善。
本文使用氧气等离子体引发环氧树脂涂层对Twaron纤维的表面进行了改性,将经过相同等离子体处理条件下的纤维浸泡在不同浓度的涂层溶液中,发现1wt%的涂层溶液处理后的复合材料的ILSS值最高。涂层分子与纤维表面分子发生了化学键合,C-N基团含量降低、C=O等基团消失,同时出现了大量的C-O基团,这使得纤维表面的极性和反应活性增强,导致纤维的表面自由能提高。系统分析了不同放电时间和功率下,纤维的表观物理形貌和复合材料的界面粘结强度的变化。处理时间过长、放电功率过大都可能导致Twaron纤维表面刻蚀过重而导致复合材料界面粘结强度的下降。结果发现在放电功率为100W,放电时间为10min下,复合材料的ILSS值最高,且此时的吸湿率最低。
论文系统研究了氩气等离子体引发环氧树脂涂层改性对Twaron纤维表面性能影响,及各种放电参数对材料界面性能的影响。大量C-O基团被引入到纤维的表面,改性后的纤维形貌更为复杂,一层树脂覆盖在纤维的表面。纤维的表面自由能由49.9mJ/m2提高到了61.8mJ/m2。不同放电时间和功率条件下,复合材料的ILSS不同,在100W、10min和30Pa下,ILSS达到66.2MPa,增幅达68.9%。经过等离子体处理后的纤维表面,在涂层改性过程中会有大量环氧树脂分子沉积在纤维表面,复合材料的制备过程中,PPESK分子扩散到环氧树脂层中,在模压高温下,环氧树脂发生固化,形成束缚层使得纤维不易在剪切力作用下发生滑移,因而有利于ILSS的提高。
High-performance organic fibers have got much more attentions, due to their excellent strength, modulus, toughness and outstanding resistance to high temperature and shock. The high-performance organic fiber reinforced thermoplastic composites were usually used in the areas of aerospace and modern national defense owing to the high fracture toughness, damage tolerance, impact resistance and good processability. However, the surfaces of Twaron fiber and poly (p-phenylene benzobisoxazole)(PBO) fiber are smooth, lack of polar groups and chemical inert. Thus, the interfacial adhesion is usually poor between the fiber and matrix, which restrict the mechanical properties of the composites. Therefore, surface modification of organic fiber is necessary, to improve the surface chemical properties and morphologies, to increase the surface free energy, and to enhance the interfacial adhesion of the composite.
In this thesis, the PBO and Twaron fibers were treated by inductively coupled gas plasma (ICP) and immediately coated in the polymer solutions. The surface chemical properties, surface morphologies and the surface free energies of the fibers before and after coating were examined by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), and dynamic contact angle analysis (DCAA). The interlaminar shear strength (ILSS), moisture absorption and SEM were selected to determine the interfacial adhesion strength, water absorption and the interlaminar shear fracture morphologies of the composites. The mechanisms of the enhancement of the interfacial adhesion by thermoset and thermoplastic coatings were discussed.
Optimal treatment condition was obtained using the orthogonal design, which could be stated as:the concentration of the coating resin is3%, the plasma power is100W, the treatment time is10min and the discharge pressure is30Pa. Oxygen-plasma-induced coating could modify the surface properties of PBO fibers, roughen the fiber surface and increase the surface free energy. The ILSS was improved significantly, moisture absorption was lower than the untreated sample, and the fracture mode was changed from interface debonding to matrix fracture.
To improve the interfacial adhesion of PBO/PPESK composite, thermoplastic resins were coated onto the fiber surface after oxygen plasma pretreatment. Phenolphthalein poly (ether ketone)(PEK-C) and phenolphthalein poly (ether sulfone)(PES-C) were selected to be the coating resins. The XPS results showed that after the two resins coated the concentration of oxygen was increased, and the O=C-O, C=O or O=S=O were introduced onto the fiber surface. The fiber surfaces were roughened and the surface wettabilities were improved. After coating, the primary failure mode of the composites was changed from interface debonding to matrix fracture. The enhancement of the interface may be attributed to the stronger molecular entanglement. The matrix molecules physically to entangle with or diffuse into the molecular network of polymer coatings applied on the fibers. Therefore, the interfacial adhesion was enhanced.
Epoxy resin was selected to coat onto the surface of Twaron fibers induced by the oxygen plasma. The highest ILSS value was got when the concentration of epoxy resin was1wt%under the same plasma discharge condition. The concentration of C-N decreased, and the C=O group was disappeared; meanwhile the C-O group was appeared on the fiber surface with a concentration of22.4%. The polarity of the fiber surface was improved and the surface free energy was increased. Too long plasma treatment time and too high discharge power could damage the fiber body, which may lead to the damage of the interfacial adhesion of the fiber and matrix.
Argon-plasma-induced epoxy resin coating onto the Twaron fiber surface in order to modify the fiber surface properties. C-O group was introduced onto the fiber and the morphologies of the fiber surface were much more complex after coating. A thin and inhomogeneous layer of coating resins had been deposited onto the fiber surface. The surface free energy was improved from49.9to61.8mJ/m2. The optimal treatment condition was that the plasma power was100W, the treatment time was10min and the discharge pressure was30Pa. The coating layer was nonuniform and most of the epoxy resins were still small molecules before compression molding. Hence, the PPESK molecules may dive into the epoxy coating layers during the solution impregnation. Therefore, the coating layer acted as a bridge between the fibers and the matrices. After compression modlding, the cured epoxy resin bounded the fibers to improve the ILSS.
引文
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