耐温光纤布拉格光栅传感器涂层的研究
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摘要
在大飞机上更多地使用碳纤维树脂基复合材料替代金属材料,可以减轻重量、提高续航能力、节省油耗。将光纤布拉格光栅(FBG:Fiber Bragg Grating)传感器埋入碳纤维树脂基复合材料中,对复合材料成型时的固化过程进行监测,控制固化过程参数,稳定复合材料的性能,在成型后,FBG传感器仍能存活于复合材料内部,对复合材料服役过程进行实时监测,及时得到复合材料的健康状况的信息,对大飞机的结构健康进行有效预警,是一件非常有意义的工作。但大飞机结构用树脂基复合材料需在高温和压力下成型,现有光纤光栅传感器涂层不耐高温,因此系统地了解FBG传感器埋入树脂基复合材料时,传感器涂层对传感器传感性能的影响,并在此基础上研究一种适合埋入热压罐成型的碳纤维复合材料耐高温光纤光栅涂层很有必要。
本文首先对比了无涂层光栅和现有通用聚氨酯丙烯酸酯(PUA: polyurethane acrylate)涂层光栅传感器在200℃下加热1小时,结果显示,加热后无涂层和PUA涂层光纤的抗张强度变小,然后将两者埋入热压罐成型复合材料中,发现光纤截面经过高温和压力,PUA树脂熔融,使光纤与基体之间形成空洞。然后复合材料进行固化监测和力学性能测试的准确性的研究,结果表明,现有聚氨酯丙烯酸酯光栅涂层在常温下可提高FBG传感器的温度灵敏系数,但在高温下使用会降低传感器的稳定性,准确性低于无涂层光栅,高温成型冷却后,涂层损坏引起光栅失效,而无涂层光栅由于没有缓冲保护,也在材料失效之前失效,无法完整监测整个失效过程。
在对现有光纤涂层和光栅二次涂覆涂层性能评价的基础上,本文设计了一种内层为化学镀镍层,外层为紫外光固化纳米二氧化硅／环氧丙烯酸酯(EA:Epoxy acrylate)/聚氨酯丙烯酸酯(纳米SiO2/EA/PUA)杂化材料的双涂层结构的FBG传感器涂层,用于提高FBG传感器在高温成型时复合材料中传感的灵敏度和使用性能。
文中首先确定了光纤镀镍的预处理方法,然后对比了三种化学镀镍方式,采用盐基胶体钯浸泡,然后用20%NaOH解胶的无粗化镀镍方法进行化学镀覆,得到镀镍光栅在空气中加热,30℃至100℃的温度灵敏系数为8.914pm/K,在100℃至200℃的温度灵敏系数为10.167pm/K,应变灵敏系数为0.58nm/N,线性度为100%。
在进行二次涂覆涂层外涂层的研制时,首先通过甲苯-2,4-二异氰酸酯(TDI:2,4-toluene diisocyanate)、聚丙二醇(PPG:Poly propylene glycol)与丙烯酸羟乙酯(HEA:Hydroxyethyl methacrylate)合成PUA预聚体,对由不同分子量PPG制备而成的PUA预聚体进行了性能评价,研究表明,PPG2000制备的PUA热稳定性最好,开始失重温度在280℃,玻璃化转变温度(Tg)为104℃；然后研究了PUA与EA的物理共混配比,通过硬度测试、固化度测试以及热失重分析(TGA:Thermal gravimetric analysis)分析,得到在光引发剂以及活性稀释剂不变的情况下,聚氨酯丙烯酸酯与环氧丙烯酸酯的质量比为2：1时,共混体系能表现出最优异的热稳定性能。最后采用溶胶-凝胶法制备二氧化硅颗粒,通过原位聚合制备纳米SiO2/EA/PUA杂化材料,研究了不同催化剂、不同硅烷偶联剂以及不同配比对杂化材料性能的影响。通过场发射扫描电镜(FESEM:Field emission scanning electron microscope)测试杂化体系中二氧化硅的分散情况,采用差热扫描量热法(DSC:Differential scanning calorimetry)、TGA来确定最佳的热稳定性能。研究表明,采用盐酸作为催化剂、KH-570硅烷偶联剂作为二氧化硅表面处理剂、正硅酸乙酯(TEOS:Tetraethyl orthosilicate):(PUA+EA)为0.4：1时,制备的杂化材料热稳定性最佳,耐温可达143.8℃。利用模型拟合法进行了SiO2/EA/PUA杂化材料紫外光固化动力学分析,分析表明SiO2/EA/PUA杂化材料紫外光固化时为一级反应,速率常数为0.09486,处于EA和PUA固化速率常数之间。
论文最后将内层镀镍外层为纳米SiO2/EA/PUA杂化材料的双涂层涂覆于FBG传感器上,测量了传感器的基本性质、温度灵敏系数和应力灵敏系数,然后埋入复合材料中,监测热压罐成型碳纤维／环氧树脂复合材料的固化成型过程,结果表明自制双涂层FBG传感器可完整监测固化成型过程；随后监测了成型后复合材料的弯曲性能,结果表明双涂层FBG传感器可以完整监测复合材料弯曲直至材料失效的整个过程,而无涂层FBG和EA涂层FBG传感器在材料失效之前就已经失效。
Nowadays, many composite materials, instead of metal matierials, have been applied in large aircrafts for decreasing weight, improving endurance ability and saving energy. It is a significiant work that FBG (Fiber Bragg Grating) sensors to be embedded in the composites for monitoring the structural health of large aircraft curing and service process. However, under the molding step of resin-based composites used in large aircraft, the optical fiber should be suffered to high temperature and suitable pressure. Since most of the existing high temperature fiber grating coatings were used for civil engineering, they are not competent for aircraft. Therefore, it is necessary to develop a new kind of high temperature coating for embedded in resin-based carbon fiber, which are generally used for aircrafts.
Firstly, the heat-resistance performances of existing optical fiber coatings were evaluated in this thesis. The ordinary layers (PUA:polyurethane acrylate) coated optical fiber and uncoated optical fiber embedded in composite material were compared.The results show that after heated, the optical loss and flexible of fibes have no inficantly change, but the tensile strength decrease. Then FBG sensor coated with PUA(polyurethane acrylate) and FBG sensor without coating were embedded in the composites respectively.The accuracy of curing process and the mechine properties testing monitoring was studied. The results show that the FBG sensor coated with EA (Expoxy acrylate) has higher temperature sensitivity coefficient at normal atmospheric conditions, while it has lower stability and accuracy at high temperature. After the molding was complete, the coating was damaged, leading to the failure of sensors. FBG sensor without coating was damaged before the materials were failure because of the absence of protection buffers. As a result, the research of heat resistance FBG sensor coating is necessary.
A new double layers FBG sensor coating was designed after evaluation of properties of the existing optical fiber coating and optical grating coating. The inner layer of the new coating was nickel plating, and the outer layer was nano-SiO2/PUA/EA hybrid material.This kind of coating could improve the sensitivity of FBG sensor and its performance during molding process at high temperature.
First of all, the pretreatment methods of the fiber before nickel plating were determined. Then three kinds of electroless nickel plating method were compared. The best method was following:the fiber without coarsening was immersed in the colloid palladium.After that, it was treated with20%NaOH solution. Finally, it was chemical plated with nickel. It was found that the temperature sensitivity coefficient of nickel-plated FBG sensor was8.914pm/K from30℃to100℃, and10.167pm/K from100℃to200℃when the sensors were heat in the air. The strain sensitivity coefficient was0.58nm/N, and linear degree was100%.
Secondly, preparation of the outer coating was studied. TDI (2,4-toluene diisocyanate), PPG (Poly propylene glycol) and HEA (Hydroxyethyl methacrylate) were used to synthesize PUA prepolymer. The performance of PUA prepolymer with different molecular weight of PPG was determined. The result indicated that PUA prepared with PPG2000showed best heat stability, which demonstrated starting weight loss at280℃under TG. The vitrification transition temperature (Tg) was104℃. Then the blend ratio of the polyurethane acrylate and polyurethane epoxy acrylate was studied. It was found that when the photoinitiator and reactive diluent were kept constant, and the quality of acrylic polyurethane and epoxy acrylate was2:1, blending system showed the most excellent thermal stability under hardness testing, curing degree test and TGA (Thermal gravimetric analysis).
Silica particles were prepared via sol-gel method; nano silica epoxy acrylate/polyurethane acrylate hybrid materials were prepared via in-situ polymerization. Several catalysts, different silane coupling agents and their proportions on the properties of hybrid material were studied. The dispersion of silica in the hybrid system was determined by FESEM (field emission scanning electron microscopy) test, the thermal stability was determinded through DSC (Differential scanning calorimetry) and TGA. It showed that the hybrid materials (prepared with KH-570silane coupling agent as surface treatment agent, TEOS(Tetraethyl orthosilicate):(PUA+EA) was0.4:1) displayed best thermal stability, heat resistance was up to143.8℃when using hydrochloric acid as a catalyst. The UV curing kinetics of SiO2/EA/PUA hybrid materials were analyzed by model fitting, it showed that the UV curing of SiO2/EA/PUA hybrid materials was a first order reaction with a reaction constant of0.09486.
Finally, the double layer coating with the nickel-plated inner layer and outer layer of SiO2/EA/PUA hybrid materials was coated on the grating portion of the FBG sensors, the basic properties, the temperature sensitivity coefficient and the stress sensitivity coefficient of the sensor were tested, which was then embedded in the composite so as to monitor the curing process of carbon fiber/epoxy composite during autoclave molding. The results showed that the double layer FBG sensor could monitor the whole molding process. The bend testing process was also monitored. The results showed the double layer coated grate could monitor the bending properties of composite more accurately than the uncoated or EA-coated FBG sensors. The FBG sensors without coating and coated EA were break down before failure of the materials.
本文首先对比了无涂层光栅和现有通用聚氨酯丙烯酸酯(PUA: polyurethane acrylate)涂层光栅传感器在200℃下加热1小时,结果显示,加热后无涂层和PUA涂层光纤的抗张强度变小,然后将两者埋入热压罐成型复合材料中,发现光纤截面经过高温和压力,PUA树脂熔融,使光纤与基体之间形成空洞。然后复合材料进行固化监测和力学性能测试的准确性的研究,结果表明,现有聚氨酯丙烯酸酯光栅涂层在常温下可提高FBG传感器的温度灵敏系数,但在高温下使用会降低传感器的稳定性,准确性低于无涂层光栅,高温成型冷却后,涂层损坏引起光栅失效,而无涂层光栅由于没有缓冲保护,也在材料失效之前失效,无法完整监测整个失效过程。
在对现有光纤涂层和光栅二次涂覆涂层性能评价的基础上,本文设计了一种内层为化学镀镍层,外层为紫外光固化纳米二氧化硅／环氧丙烯酸酯(EA:Epoxy acrylate)/聚氨酯丙烯酸酯(纳米SiO2/EA/PUA)杂化材料的双涂层结构的FBG传感器涂层,用于提高FBG传感器在高温成型时复合材料中传感的灵敏度和使用性能。
文中首先确定了光纤镀镍的预处理方法,然后对比了三种化学镀镍方式,采用盐基胶体钯浸泡,然后用20%NaOH解胶的无粗化镀镍方法进行化学镀覆,得到镀镍光栅在空气中加热,30℃至100℃的温度灵敏系数为8.914pm/K,在100℃至200℃的温度灵敏系数为10.167pm/K,应变灵敏系数为0.58nm/N,线性度为100%。
在进行二次涂覆涂层外涂层的研制时,首先通过甲苯-2,4-二异氰酸酯(TDI:2,4-toluene diisocyanate)、聚丙二醇(PPG:Poly propylene glycol)与丙烯酸羟乙酯(HEA:Hydroxyethyl methacrylate)合成PUA预聚体,对由不同分子量PPG制备而成的PUA预聚体进行了性能评价,研究表明,PPG2000制备的PUA热稳定性最好,开始失重温度在280℃,玻璃化转变温度(Tg)为104℃；然后研究了PUA与EA的物理共混配比,通过硬度测试、固化度测试以及热失重分析(TGA:Thermal gravimetric analysis)分析,得到在光引发剂以及活性稀释剂不变的情况下,聚氨酯丙烯酸酯与环氧丙烯酸酯的质量比为2：1时,共混体系能表现出最优异的热稳定性能。最后采用溶胶-凝胶法制备二氧化硅颗粒,通过原位聚合制备纳米SiO2/EA/PUA杂化材料,研究了不同催化剂、不同硅烷偶联剂以及不同配比对杂化材料性能的影响。通过场发射扫描电镜(FESEM:Field emission scanning electron microscope)测试杂化体系中二氧化硅的分散情况,采用差热扫描量热法(DSC:Differential scanning calorimetry)、TGA来确定最佳的热稳定性能。研究表明,采用盐酸作为催化剂、KH-570硅烷偶联剂作为二氧化硅表面处理剂、正硅酸乙酯(TEOS:Tetraethyl orthosilicate):(PUA+EA)为0.4：1时,制备的杂化材料热稳定性最佳,耐温可达143.8℃。利用模型拟合法进行了SiO2/EA/PUA杂化材料紫外光固化动力学分析,分析表明SiO2/EA/PUA杂化材料紫外光固化时为一级反应,速率常数为0.09486,处于EA和PUA固化速率常数之间。
论文最后将内层镀镍外层为纳米SiO2/EA/PUA杂化材料的双涂层涂覆于FBG传感器上,测量了传感器的基本性质、温度灵敏系数和应力灵敏系数,然后埋入复合材料中,监测热压罐成型碳纤维／环氧树脂复合材料的固化成型过程,结果表明自制双涂层FBG传感器可完整监测固化成型过程；随后监测了成型后复合材料的弯曲性能,结果表明双涂层FBG传感器可以完整监测复合材料弯曲直至材料失效的整个过程,而无涂层FBG和EA涂层FBG传感器在材料失效之前就已经失效。
Nowadays, many composite materials, instead of metal matierials, have been applied in large aircrafts for decreasing weight, improving endurance ability and saving energy. It is a significiant work that FBG (Fiber Bragg Grating) sensors to be embedded in the composites for monitoring the structural health of large aircraft curing and service process. However, under the molding step of resin-based composites used in large aircraft, the optical fiber should be suffered to high temperature and suitable pressure. Since most of the existing high temperature fiber grating coatings were used for civil engineering, they are not competent for aircraft. Therefore, it is necessary to develop a new kind of high temperature coating for embedded in resin-based carbon fiber, which are generally used for aircrafts.
Firstly, the heat-resistance performances of existing optical fiber coatings were evaluated in this thesis. The ordinary layers (PUA:polyurethane acrylate) coated optical fiber and uncoated optical fiber embedded in composite material were compared.The results show that after heated, the optical loss and flexible of fibes have no inficantly change, but the tensile strength decrease. Then FBG sensor coated with PUA(polyurethane acrylate) and FBG sensor without coating were embedded in the composites respectively.The accuracy of curing process and the mechine properties testing monitoring was studied. The results show that the FBG sensor coated with EA (Expoxy acrylate) has higher temperature sensitivity coefficient at normal atmospheric conditions, while it has lower stability and accuracy at high temperature. After the molding was complete, the coating was damaged, leading to the failure of sensors. FBG sensor without coating was damaged before the materials were failure because of the absence of protection buffers. As a result, the research of heat resistance FBG sensor coating is necessary.
A new double layers FBG sensor coating was designed after evaluation of properties of the existing optical fiber coating and optical grating coating. The inner layer of the new coating was nickel plating, and the outer layer was nano-SiO2/PUA/EA hybrid material.This kind of coating could improve the sensitivity of FBG sensor and its performance during molding process at high temperature.
First of all, the pretreatment methods of the fiber before nickel plating were determined. Then three kinds of electroless nickel plating method were compared. The best method was following:the fiber without coarsening was immersed in the colloid palladium.After that, it was treated with20%NaOH solution. Finally, it was chemical plated with nickel. It was found that the temperature sensitivity coefficient of nickel-plated FBG sensor was8.914pm/K from30℃to100℃, and10.167pm/K from100℃to200℃when the sensors were heat in the air. The strain sensitivity coefficient was0.58nm/N, and linear degree was100%.
Secondly, preparation of the outer coating was studied. TDI (2,4-toluene diisocyanate), PPG (Poly propylene glycol) and HEA (Hydroxyethyl methacrylate) were used to synthesize PUA prepolymer. The performance of PUA prepolymer with different molecular weight of PPG was determined. The result indicated that PUA prepared with PPG2000showed best heat stability, which demonstrated starting weight loss at280℃under TG. The vitrification transition temperature (Tg) was104℃. Then the blend ratio of the polyurethane acrylate and polyurethane epoxy acrylate was studied. It was found that when the photoinitiator and reactive diluent were kept constant, and the quality of acrylic polyurethane and epoxy acrylate was2:1, blending system showed the most excellent thermal stability under hardness testing, curing degree test and TGA (Thermal gravimetric analysis).
Silica particles were prepared via sol-gel method; nano silica epoxy acrylate/polyurethane acrylate hybrid materials were prepared via in-situ polymerization. Several catalysts, different silane coupling agents and their proportions on the properties of hybrid material were studied. The dispersion of silica in the hybrid system was determined by FESEM (field emission scanning electron microscopy) test, the thermal stability was determinded through DSC (Differential scanning calorimetry) and TGA. It showed that the hybrid materials (prepared with KH-570silane coupling agent as surface treatment agent, TEOS(Tetraethyl orthosilicate):(PUA+EA) was0.4:1) displayed best thermal stability, heat resistance was up to143.8℃when using hydrochloric acid as a catalyst. The UV curing kinetics of SiO2/EA/PUA hybrid materials were analyzed by model fitting, it showed that the UV curing of SiO2/EA/PUA hybrid materials was a first order reaction with a reaction constant of0.09486.
Finally, the double layer coating with the nickel-plated inner layer and outer layer of SiO2/EA/PUA hybrid materials was coated on the grating portion of the FBG sensors, the basic properties, the temperature sensitivity coefficient and the stress sensitivity coefficient of the sensor were tested, which was then embedded in the composite so as to monitor the curing process of carbon fiber/epoxy composite during autoclave molding. The results showed that the double layer FBG sensor could monitor the whole molding process. The bend testing process was also monitored. The results showed the double layer coated grate could monitor the bending properties of composite more accurately than the uncoated or EA-coated FBG sensors. The FBG sensors without coating and coated EA were break down before failure of the materials.
引文
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