PBO纤维表面耐紫外涂层的制备及其光老化性能研究
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摘要
近年来，由于PBO纤维具有优异的力学性能(高比强度和高比模量)和独特的属性(低密度，良好的热稳定性和化学稳定性)而被广泛地用作为树脂基复合材料的增强体。然而，对太阳光特别是紫外线(UV)的敏感性导致PBO纤维及其复合材料结构和性能退化，严重影响了PBO纤维复合材料的使用安全性和可靠性。因此，开展针对PBO纤维紫外防护的研究工作成为热点问题。为了提高PBO纤维对紫外光的抵抗能力，本文选用有机分子和无机纳米粒子紫外线吸收剂，借助等离子体改性方法﹑溶胶-凝胶和自组装技术制备了三种不同形式的PBO纤维表面保护涂层，对涂层结构进行了表征，对材料的性能特别是光老化性能进行了研究。
PBO纤维表面光滑，无极性。为了有利于涂层的引入，PBO纤维进行了氧等离子体活化处理，评估了等离子体处理功率和处理时间对活化效果的影响。结果显示，提高处理功率和延长处理时间均使PBO纤维表面粗糙度增加，表面自由能及其与环氧树脂基体间的IFSS先增加后降低。确定最佳处理条件为：处理功率为175W，处理时间为10min。
经实验优化确定了2-(2-羟基苯)-苯并三氮唑(BTZ)为有机分子紫外线吸收剂，并将其填加到环氧树脂浆料中，制备了PBO纤维表面耐紫外线涂层。上浆剂与环氧树脂间的分子结构相似性改进了PBO纤维与基体间的浸润性。紫外光加速老化实验显示：单纯的环氧树脂基上浆剂涂层不能有效保护纤维本体，而含紫外吸收有机分子的上浆剂涂层能有效地吸收入射紫外线，缓解纤维本体的老化降解。紫外加速老化480h后，原始PBO纤维的拉伸强度保持率和特性粘度保持率分别为29.2%和72.0%。经含1.0wt%BTZ上浆剂处理后，PBO-I纤维的拉伸强度保持率和特性粘度保持率分别提高到52.7%和81.7%。
结合等离子体引发气相表面接枝和溶胶纳米粒子表面涂覆制备了PBO纤维的光稳定性涂层。氧等离子体引发丙烯酸气相接枝活化了PBO纤维表面，纤维表面粗糙度和表面功能基团含量增加，表面自由能提高，拉伸强度略有降低，PBO纤维与环氧树脂间的界面结合增强。伴随着接枝时间的延长，聚丙烯酸层对纤维表面的包覆愈加完整，纤维表面粗糙度逐渐增加，表面自由能和IFSS均先增加后降低，当气相接枝时间为10min时，处理效果最佳。TiO2和ZnO溶胶纳米粒子的平均粒径分别为38nm和50nm，粒径小且分布窄，完全满足纤维表面涂覆的使用需要。表面涂覆纳米粒子溶胶后，纤维表面形成一层光屏蔽无机纳米粒子层，纤维表面粗糙度和表面功能基团含量增加，这些促使纤维表面自由能提高，改进了纤维与环氧树脂间的界面剪切强度(IFSS)。伴随着表面涂覆次数的增加，纳米粒子保护层愈加致密，涂层厚度愈大，增加的纤维表面二氧化钛/氧化锌含量保证了涂层对紫外线的高效吸收。加速老化试验显示纤维表层的无机纳米粒子层能有效隔绝外界紫外光与纤维本体的接触，确保纤维具有较高的拉伸强度保持率和特性粘度保持率，并且该保护作用随着涂层厚度的增加愈加显著。紫外加速老化480h，PBO-II-1纤维和PBO-II-2纤维的拉伸强度保持率和特性粘度保持率分别为56.8%和53.8%，82.6%和79.8%。
结合等离子体表面活化处理和层层自组装技术制备了PBO纤维表面光稳定涂层。借助自组装技术在纤维表面制备(PAA/BPEI)m/(PAA/TiO2)n或(PAA/BPEI)m/(POSS/TiO2)n保护涂层，纤维经过处理后，表面粗糙度和表面功能基团含量增加，表面自由能增加，纤维与环氧树脂间的IFSS增加。XPS谱图上出现明显的钛和硅元素特征吸收峰，且元素含量随自组装次数的增加而增加。紫外加速老化实验显示增加自组装次数可以增加涂层厚度，厚度增加的无机纳米涂层对纤维的保护效果更加明显。比较处理前后PBO纤维的拉伸强度保持率和特性粘度保持率发现，处理后的PBO纤维的耐紫外光稳定性更佳。紫外加速老化480h，PBO-III-1纤维和PBO-III-2纤维的拉伸强度保持率和特性粘度保持率分别为56.0%和60.7%，81%和82.3%。随着涂层厚度的增加，纤维的拉伸强度保持率和特性粘度保持率逐渐增加，这表明在纤维表面制备一定厚度的涂层可以有效地保护了纤维本体的完整性。
In recent years, Poly-p-phenylenebenzobisthiazole (PBO) fiber as reinforcingmaterial has been extensively used in resin-matrix composite, due to its superiormechanical properties including high-specific strength and high-specific modulus,as well as unique characteristics such as low density, high thermal and chemicalstabilities. However, the sensitivity to solar light, especially ultraviolet (UV), whichcan deteriorate structures and properties of PBO fiber and corresponding composites,seriously affects the safety and reliability of PBO fibers-composite materials.Therefore, research on the anti-UV protection of PBO fiber becomes a fascinatingfield. In the present research, organic-molecule and inorganic-nanoparticleUV-absorbed agents were used, and three different surface protective coatings wereprepared on PBO fiber surface by plasma modification method, sol-gol andself-assembly technology for improving UV-resistance of PBO fiber. The structureof coating on PBO fiber surface was characterized, and the properties of materialespecially photo-aging property were studied.
PBO fiber surface is smooth, and non-polar. PBO fiber was activated byoxygen plasma modification for the successful preparation of coating. Theinfluences of voltage and time of plasma treatment on activation were evaluated.Results show that increasing power and time of plasma treatment both make surfaceroughness of fiber increase, surface free energy and IFSS between fiber and epoxyresin matrix first increase and then decrease. The optimal treatment condition wereobtained: voltage is175W and time is10min.
2-(2-hydroxyphenyl)-benzotriazole (BTZ) was selected as organic-moleculeUV-absorbed agent after experimental optimization, and added into sizing agent ofepoxy resin for creation of anti-UV coating on PBO fiber surface. The similarity ofmolecular strcture between sizing agent and epoxy resin improves the wettabilitybetween PBO fiber and matrix. UV accelerated aging test shows that coating createdby pure epoxy resin based sizing agent can not protect fiber body, whereas coatingcreated by UV-absorbed organic-molecue containing sizing agent can effectivelyabsorb incident UV light, and relieve aging degradation of fiber body. After480hUV-accelerated aging, tensile strength (TS) retention and intrinsic viscosity (IV)retention of original PBO fiber is29.2%and72.0%, respectively. TS retention andIV retention of PBO-I fiber treated by sizing agent containing1.0wt%BTZ isincreased to52.7%and81.7%, respectively.
Plasma induced vapor surface grafting technology and surface coatingmethod of sol nanoparticle were combined to prepare coating with photostability on PBO fiber surface. PBO fiber surface was activated through oxygen plasma inducedacrylic acid grafting reaction, Roughness, functional group content and surface freeenergy on PBO fiber increase, tensile strength decrease in a small extent, andinterface bonding between PBO fiber and epoxy resin increase. With the extensionof grafting time, polyacrylic acid coating on PBO fiber surface becomes moreperfect, fiber surface becomes more rough, surface free energy and IFSS both firstincrease and then decrease. The best result was obtained when vapor grafting time is10min. The average size of TiO2and ZnO sol nanoparticles is38nm and50nm.Small size and narrow size distribution of these particles can completely meet withthe demand of fiber surface coating. A photo-shielded inorganic nanoparticle layerwas formed on fiber surface after surface coating of nanoparticle. Increased surfaceroughness and surface functional group content of fiber cause surface free energy offiber increase, and interface shear strength (IFSS) between fiber and epoxy resin isimproved. With the increase in number of surface coating, nanoparticle protectivelayer becomes denser, coating thickness become greater, and increased TiO2andZnO content on fiber surface supply coating with a efficient absorption for UV ray.Accelerated aging test proved that inorganic nanoparticles on fiber surface build aeffective barrier between UV ray from external environment and fiber body, providefiber with high tensile strength retention and intrinsic viscosity retention, and thisprotective effect is more significant with coating thickness increase. TS retentionand IV retention of PBO-II-1fiber and PBO-II-2fiber is56.8%and53.8%,82.6%and79.8%, respectively.
Coordinative usage of plasma surface active treatent and layer-by-layerself-assembly technology to create coating with photostability on PBO fiber surface.Protective coating of (PAA/BPEI)m/(PAA/TiO2)nor (PAA/BPEI)m/(POSS/TiO2)nwas prepared on fiber surface by virtue of self-assembly. After treatment, surfaceroughness and surface functional group content increase, surface free energyincrease, IFSS between fiber and epoxy resin also increase. Characteristicabsorption peaks of Ti and Si element appear on XPS spectrum, and element contentincreased with the increase in number of self-assembly. UV accelerated aging testshowed the increase in number of self-assembly can increase the thickness ofcoating, and increased thickness of inorganic nanoparticle coating can moreeffectively protect fiber. By comparing TS retention and IV retention of untreatedand treated PBO fiber after accelerated aging, a phenomenon is found that anti-UVstability of treated PBO fiber is better. After480h UV accelerated aging, TSretention and IV retention of PBO-III-1fiber and PBO-III-2fiber can reach56.0%and60.7%,81%and82.3%, respectively. With the increase in thickness of coating, TS retention and IV retention of fiber gradually increase, this result indicate thatpreparing a certain thickness of coating on fiber surface can effectively protectintegrity of fiber.
PBO纤维表面光滑，无极性。为了有利于涂层的引入，PBO纤维进行了氧等离子体活化处理，评估了等离子体处理功率和处理时间对活化效果的影响。结果显示，提高处理功率和延长处理时间均使PBO纤维表面粗糙度增加，表面自由能及其与环氧树脂基体间的IFSS先增加后降低。确定最佳处理条件为：处理功率为175W，处理时间为10min。
经实验优化确定了2-(2-羟基苯)-苯并三氮唑(BTZ)为有机分子紫外线吸收剂，并将其填加到环氧树脂浆料中，制备了PBO纤维表面耐紫外线涂层。上浆剂与环氧树脂间的分子结构相似性改进了PBO纤维与基体间的浸润性。紫外光加速老化实验显示：单纯的环氧树脂基上浆剂涂层不能有效保护纤维本体，而含紫外吸收有机分子的上浆剂涂层能有效地吸收入射紫外线，缓解纤维本体的老化降解。紫外加速老化480h后，原始PBO纤维的拉伸强度保持率和特性粘度保持率分别为29.2%和72.0%。经含1.0wt%BTZ上浆剂处理后，PBO-I纤维的拉伸强度保持率和特性粘度保持率分别提高到52.7%和81.7%。
结合等离子体引发气相表面接枝和溶胶纳米粒子表面涂覆制备了PBO纤维的光稳定性涂层。氧等离子体引发丙烯酸气相接枝活化了PBO纤维表面，纤维表面粗糙度和表面功能基团含量增加，表面自由能提高，拉伸强度略有降低，PBO纤维与环氧树脂间的界面结合增强。伴随着接枝时间的延长，聚丙烯酸层对纤维表面的包覆愈加完整，纤维表面粗糙度逐渐增加，表面自由能和IFSS均先增加后降低，当气相接枝时间为10min时，处理效果最佳。TiO2和ZnO溶胶纳米粒子的平均粒径分别为38nm和50nm，粒径小且分布窄，完全满足纤维表面涂覆的使用需要。表面涂覆纳米粒子溶胶后，纤维表面形成一层光屏蔽无机纳米粒子层，纤维表面粗糙度和表面功能基团含量增加，这些促使纤维表面自由能提高，改进了纤维与环氧树脂间的界面剪切强度(IFSS)。伴随着表面涂覆次数的增加，纳米粒子保护层愈加致密，涂层厚度愈大，增加的纤维表面二氧化钛/氧化锌含量保证了涂层对紫外线的高效吸收。加速老化试验显示纤维表层的无机纳米粒子层能有效隔绝外界紫外光与纤维本体的接触，确保纤维具有较高的拉伸强度保持率和特性粘度保持率，并且该保护作用随着涂层厚度的增加愈加显著。紫外加速老化480h，PBO-II-1纤维和PBO-II-2纤维的拉伸强度保持率和特性粘度保持率分别为56.8%和53.8%，82.6%和79.8%。
结合等离子体表面活化处理和层层自组装技术制备了PBO纤维表面光稳定涂层。借助自组装技术在纤维表面制备(PAA/BPEI)m/(PAA/TiO2)n或(PAA/BPEI)m/(POSS/TiO2)n保护涂层，纤维经过处理后，表面粗糙度和表面功能基团含量增加，表面自由能增加，纤维与环氧树脂间的IFSS增加。XPS谱图上出现明显的钛和硅元素特征吸收峰，且元素含量随自组装次数的增加而增加。紫外加速老化实验显示增加自组装次数可以增加涂层厚度，厚度增加的无机纳米涂层对纤维的保护效果更加明显。比较处理前后PBO纤维的拉伸强度保持率和特性粘度保持率发现，处理后的PBO纤维的耐紫外光稳定性更佳。紫外加速老化480h，PBO-III-1纤维和PBO-III-2纤维的拉伸强度保持率和特性粘度保持率分别为56.0%和60.7%，81%和82.3%。随着涂层厚度的增加，纤维的拉伸强度保持率和特性粘度保持率逐渐增加，这表明在纤维表面制备一定厚度的涂层可以有效地保护了纤维本体的完整性。
In recent years, Poly-p-phenylenebenzobisthiazole (PBO) fiber as reinforcingmaterial has been extensively used in resin-matrix composite, due to its superiormechanical properties including high-specific strength and high-specific modulus,as well as unique characteristics such as low density, high thermal and chemicalstabilities. However, the sensitivity to solar light, especially ultraviolet (UV), whichcan deteriorate structures and properties of PBO fiber and corresponding composites,seriously affects the safety and reliability of PBO fibers-composite materials.Therefore, research on the anti-UV protection of PBO fiber becomes a fascinatingfield. In the present research, organic-molecule and inorganic-nanoparticleUV-absorbed agents were used, and three different surface protective coatings wereprepared on PBO fiber surface by plasma modification method, sol-gol andself-assembly technology for improving UV-resistance of PBO fiber. The structureof coating on PBO fiber surface was characterized, and the properties of materialespecially photo-aging property were studied.
PBO fiber surface is smooth, and non-polar. PBO fiber was activated byoxygen plasma modification for the successful preparation of coating. Theinfluences of voltage and time of plasma treatment on activation were evaluated.Results show that increasing power and time of plasma treatment both make surfaceroughness of fiber increase, surface free energy and IFSS between fiber and epoxyresin matrix first increase and then decrease. The optimal treatment condition wereobtained: voltage is175W and time is10min.
2-(2-hydroxyphenyl)-benzotriazole (BTZ) was selected as organic-moleculeUV-absorbed agent after experimental optimization, and added into sizing agent ofepoxy resin for creation of anti-UV coating on PBO fiber surface. The similarity ofmolecular strcture between sizing agent and epoxy resin improves the wettabilitybetween PBO fiber and matrix. UV accelerated aging test shows that coating createdby pure epoxy resin based sizing agent can not protect fiber body, whereas coatingcreated by UV-absorbed organic-molecue containing sizing agent can effectivelyabsorb incident UV light, and relieve aging degradation of fiber body. After480hUV-accelerated aging, tensile strength (TS) retention and intrinsic viscosity (IV)retention of original PBO fiber is29.2%and72.0%, respectively. TS retention andIV retention of PBO-I fiber treated by sizing agent containing1.0wt%BTZ isincreased to52.7%and81.7%, respectively.
Plasma induced vapor surface grafting technology and surface coatingmethod of sol nanoparticle were combined to prepare coating with photostability on PBO fiber surface. PBO fiber surface was activated through oxygen plasma inducedacrylic acid grafting reaction, Roughness, functional group content and surface freeenergy on PBO fiber increase, tensile strength decrease in a small extent, andinterface bonding between PBO fiber and epoxy resin increase. With the extensionof grafting time, polyacrylic acid coating on PBO fiber surface becomes moreperfect, fiber surface becomes more rough, surface free energy and IFSS both firstincrease and then decrease. The best result was obtained when vapor grafting time is10min. The average size of TiO2and ZnO sol nanoparticles is38nm and50nm.Small size and narrow size distribution of these particles can completely meet withthe demand of fiber surface coating. A photo-shielded inorganic nanoparticle layerwas formed on fiber surface after surface coating of nanoparticle. Increased surfaceroughness and surface functional group content of fiber cause surface free energy offiber increase, and interface shear strength (IFSS) between fiber and epoxy resin isimproved. With the increase in number of surface coating, nanoparticle protectivelayer becomes denser, coating thickness become greater, and increased TiO2andZnO content on fiber surface supply coating with a efficient absorption for UV ray.Accelerated aging test proved that inorganic nanoparticles on fiber surface build aeffective barrier between UV ray from external environment and fiber body, providefiber with high tensile strength retention and intrinsic viscosity retention, and thisprotective effect is more significant with coating thickness increase. TS retentionand IV retention of PBO-II-1fiber and PBO-II-2fiber is56.8%and53.8%,82.6%and79.8%, respectively.
Coordinative usage of plasma surface active treatent and layer-by-layerself-assembly technology to create coating with photostability on PBO fiber surface.Protective coating of (PAA/BPEI)m/(PAA/TiO2)nor (PAA/BPEI)m/(POSS/TiO2)nwas prepared on fiber surface by virtue of self-assembly. After treatment, surfaceroughness and surface functional group content increase, surface free energyincrease, IFSS between fiber and epoxy resin also increase. Characteristicabsorption peaks of Ti and Si element appear on XPS spectrum, and element contentincreased with the increase in number of self-assembly. UV accelerated aging testshowed the increase in number of self-assembly can increase the thickness ofcoating, and increased thickness of inorganic nanoparticle coating can moreeffectively protect fiber. By comparing TS retention and IV retention of untreatedand treated PBO fiber after accelerated aging, a phenomenon is found that anti-UVstability of treated PBO fiber is better. After480h UV accelerated aging, TSretention and IV retention of PBO-III-1fiber and PBO-III-2fiber can reach56.0%and60.7%,81%and82.3%, respectively. With the increase in thickness of coating, TS retention and IV retention of fiber gradually increase, this result indicate thatpreparing a certain thickness of coating on fiber surface can effectively protectintegrity of fiber.
引文
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