微结构聚合物光纤的制备及其应用基础研究
摘要
微结构光纤以其独特的结构特征和诸多新颖的光学特性，已成为纤维光学领域的重要组成部分。而微结构聚合物光纤的柔软性、易加工性等特点，已经成为聚合物光纤技术研究的热门课题。本文从微结构聚合物光纤的制备，孔道表面修饰，孔道填充到微结构聚合物光纤的应用（特别是在作为图像传递介质和化学传感介质的应用），进行了一系列的探索性研究。
第一章，简要的介绍了光纤技术的发展史，微结构光纤技术发展现状，以及光纤传像技术，光纤化学传感器的研究与发展现状。在此基础上，提出了本论文的研究意义和特色。
第二章，介绍了国际国内现有的微结构聚合物光纤制备方法。在比较了几种方法优缺点的基础上，提出了大尺寸微结构聚合物光纤预制棒制备的新方法--挤出成型法。研究了该方法制备大尺寸微结构光纤预制棒的工艺，以及该预制棒拉制成微结构保持完好的光纤所需的各种条件（温度、送棒速度、牵引速度等等）。
第三章，首先对自制的525孔四方排列，547孔六方排列的微结构光纤作为空气芯阵列光纤的传像特性进行了研究。然后在其孔道阵列中灌入高折射率液体，制备了具有传像功能的液芯阵列微结构光纤。研究结果证明：微结构光纤自身，以及液芯微结构光纤都具有传像功能。尤其是我们制备的液芯阵列微结构光纤，在世界上是首次报道，打破了液芯光纤不能传像的历史。
第四章，首先研制出带有传像功能的光纤传感探头。方法是将pH传感膜固定在自聚焦透镜的一个端面上，而它的另一端与塑料传像光纤束的一个端头紧密相连，成为能传感图像和pH值的双功能传感探头。将塑料传像光纤的另一头与激光器，CCD相机，改进的金相显微镜、光谱仪等组装，建立了完整的具有传像功能和pH值测定功能的双功能光学传感器演示系统。利用该系统，一方面可以解决传统pH计不能实现远距离测量，也无法进入生物体内实时测量的难题。另一方面，也解决了大的样品无法用显微镜直接观察的难点，同时为生物体，或其它难以到达之处等的pH值测量，提供实时的图像信息。我们应用此系统成功的测量了金属腐蚀过程，所测数据表明，在pH2.0缓冲溶液中，铁制螺丝钉表面的pH值比其缓冲溶液高0.2个pH，而覆盖有较厚铁锈的螺丝钉表面pH值比其缓冲溶液高0.65个pH。在pH2.9缓冲溶液中，铁钉表面的pH值比缓冲溶液提升了0.16个pH值，而铁锈表面的pH值比缓冲溶液提升了0.9个pH值。
在第五章中，在第四章已经建立的双功能光学传感器演示系统的基础上，又提出了研发锌离子传感器的新思路。我们选用了极其普通的染料罗丹明B和PAN联合作为指示剂，取代了昂贵的锌离子敏感的荧光染料，并把该联合指示剂固定在适当的传感膜中。该传感膜的制备是一个技术难点。常用的如纤维素膜和传统的酸催化的sol-gel膜都不适合作锌离子指示剂支撑膜。我们首次尝试采用碱催化法制备sol-gle膜，并加入两种偶联剂对其改性，使制得的传感膜一方面适合于锌离了的检测，另一方面又与玻璃结合牢固。此系统在锌离子浓度为0.1到1mmol/L时，存在较好的线性关系；且该系统可以同时用于可视化监测，图像的分辨率为18.73lp/mm。
在第六章中，设计了一种新颖的微结构光纤二氧化碳传感器。以具有547孔的微结构光纤作为二氧化碳气体传感器的基质材料，在其内表面修饰二氧化碳传感膜——苯酚红与十六烷基三甲基氢氧化铵形成的离子对的乙基纤维素膜。在该传感器中，微结构光纤一方面起到传光的作用，另一方面也作为气体的传输通道和反应室，通过离子对的颜色变化实现对二氧化碳浓度的检测。这种结构不仅使传感探头的结构微小化，紧凑化，而且获得了较大的传感膜面积。除此之外，此气体传感器可分别采用自动和手动进气，使用灵活方便。经过对二氧化碳的响应能力进行考察，此传感器性能稳定、重复性好。
在第七章，对博士研究期间的工作进行了总结，并对今后的发展提出了展望。
Microstructured optical fiber (MOF) has become an important part in fiber field forits unique structure characteristics and optical properties. The characteristics offlexibleness and easy process etc. of microstructured polymer optical fiber (MPOF) arealso an active research focus. In this thesis, we have explored and studied a series of thefabrication technology of MPOF, the modification of the holes, the filling of the holesand the application of MPOF, especially its application as imaging-transmitting andchemical sensing medium.
The development history of optical fiber technology, the current status ofdevelopments of MOF, the technology of fiber imaging, and the current status ofdevelopments and research of optical fiber chemical sensor are briefly introduced in thefirst chapter. Based on this introduction, this thesis’characteristics and significance areproposed.
In the second chapter, the fabrication methods of MPOF was introduced andcompared, based on which the excuding-moulding method is proposed for fabrication oflarge-sized preforms. The study is made on the tehchnics of fabricating large-sizedMPOF performs and the required conditions (temperature, the rate of delivering perform,drawing speed) how to fabricate a well regular MPOF.
In the third chapter, the imaging capabilities of home-made MPOF with525holesrectangular array and547holes hexagonal array as air-core-array fiber are investigated.Then the liquid core array MOF which has imaging capabilities is fabricated byinjecting the high refractive index liquid into the array holes of MOF. The experimentsdemonstrate that the self of MOF and liquid core MOF have the imaging capabilities.Especially the liquid core array MOF that we make is firstly reported in the world andbreaks the history of liquid core fiber without the abilities of imaging.
In the fourth chapter, a fiber optical probe with function of imaging is firstly prepared. Namely, a gradient index (GRIN) lens rod which was modified by pHsensitive film is connected with a polymer imaging fiber. By connecting the other endface of imaging fiber, Laser, CCD camera, improved metallographic microscope andspectrometer, a demo system of bifunctional optical sensor with imaging capabilities isprepared. On the one hand, the technique overcomes the difficulties that the traditionalpH meter is difficult for remote detection and can not detect in organism. On the otherhand, it overcomes the difficulties that the large sample can not brought to themicroscope stage when fine observing. Moreover, it can provide real-time imagingwhen pH sensing in organism. The corrosion behavior of iron was successfullyinvestivated by employing this sensor. The experiments demonstrated that in pH2.0buffer solutions, the pH value of the iron surface was about0.2pH unit higher than thatof the buffer solutions, the pH value of screw with thick rust cladding about0.65pHunit higher than that of the buffer solutions. In the pH2.9buffer solutions, the pHvalues of iron surface and rust surface were approximately0.16and0.9pH unit higherthan that of buffer solutions, respectively.
In the fifth chapter, based on the tester assembled in fourth chapter, a new ideaabout Zn(II) sensor was proposed. A novel fluorescent sensor for Zn(II) detection isdeveloped by incorporating1-(2-pyridylazo)-2-naphthol (PAN) and Rhodamine B (RB)instead of expensive zinc ion sensitive fluorescent dye in a sol–gel film. Anothertechnical difficulty is the preparation of sensing film. The common film such ascellulose film and traditional acid catalyzed sol-gel is not suitable for immobilizing Zincion indicators. The base catalyzed sol was prepared, with the addition of two couplingreagents for improving the adherence of the sensing film with glass, and more suitablefor zinc ion detection. The sensor has the linear range of Zn(II) from0.1to1mmol/L.Simultaneously, it has the capabilities of real-time imaging with the whole system’sresolution of18.73line pairs/mm.
In the sixth chapter, a novel carbon dioxide sensor of MPOF is designed. A MOFwith547holes is firstly employed as the substrate of carbon dioxide sensor. The inner surface of MOF is modified by sensing film of ethyl cellulose embedding ion pair ofphenol red and hexadecyltrimethylammonium hydroxide. In this sensor, the fiber on theone hand has the role of light transmission; On the other hand, the MOF is thetransmission channel of gases and reaction chamber for the detection of carbon dioxideconcentration through the cholor changes of ion pair. The structure of this sensor makeitself minimal and compact with big sensing acreage. Besides, this sensor can inhalegases by automatic and manual operation which makes it agiler. The investigation of thesensor’s response capabilities demonstrates that the sensor has steady performance andwell repetition.
In the seventh chapter, a conclusion is made about the word during the studies ofPh.D. candidate, and the developments in the future is proposed.
第一章，简要的介绍了光纤技术的发展史，微结构光纤技术发展现状，以及光纤传像技术，光纤化学传感器的研究与发展现状。在此基础上，提出了本论文的研究意义和特色。
第二章，介绍了国际国内现有的微结构聚合物光纤制备方法。在比较了几种方法优缺点的基础上，提出了大尺寸微结构聚合物光纤预制棒制备的新方法--挤出成型法。研究了该方法制备大尺寸微结构光纤预制棒的工艺，以及该预制棒拉制成微结构保持完好的光纤所需的各种条件（温度、送棒速度、牵引速度等等）。
第三章，首先对自制的525孔四方排列，547孔六方排列的微结构光纤作为空气芯阵列光纤的传像特性进行了研究。然后在其孔道阵列中灌入高折射率液体，制备了具有传像功能的液芯阵列微结构光纤。研究结果证明：微结构光纤自身，以及液芯微结构光纤都具有传像功能。尤其是我们制备的液芯阵列微结构光纤，在世界上是首次报道，打破了液芯光纤不能传像的历史。
第四章，首先研制出带有传像功能的光纤传感探头。方法是将pH传感膜固定在自聚焦透镜的一个端面上，而它的另一端与塑料传像光纤束的一个端头紧密相连，成为能传感图像和pH值的双功能传感探头。将塑料传像光纤的另一头与激光器，CCD相机，改进的金相显微镜、光谱仪等组装，建立了完整的具有传像功能和pH值测定功能的双功能光学传感器演示系统。利用该系统，一方面可以解决传统pH计不能实现远距离测量，也无法进入生物体内实时测量的难题。另一方面，也解决了大的样品无法用显微镜直接观察的难点，同时为生物体，或其它难以到达之处等的pH值测量，提供实时的图像信息。我们应用此系统成功的测量了金属腐蚀过程，所测数据表明，在pH2.0缓冲溶液中，铁制螺丝钉表面的pH值比其缓冲溶液高0.2个pH，而覆盖有较厚铁锈的螺丝钉表面pH值比其缓冲溶液高0.65个pH。在pH2.9缓冲溶液中，铁钉表面的pH值比缓冲溶液提升了0.16个pH值，而铁锈表面的pH值比缓冲溶液提升了0.9个pH值。
在第五章中，在第四章已经建立的双功能光学传感器演示系统的基础上，又提出了研发锌离子传感器的新思路。我们选用了极其普通的染料罗丹明B和PAN联合作为指示剂，取代了昂贵的锌离子敏感的荧光染料，并把该联合指示剂固定在适当的传感膜中。该传感膜的制备是一个技术难点。常用的如纤维素膜和传统的酸催化的sol-gel膜都不适合作锌离子指示剂支撑膜。我们首次尝试采用碱催化法制备sol-gle膜，并加入两种偶联剂对其改性，使制得的传感膜一方面适合于锌离了的检测，另一方面又与玻璃结合牢固。此系统在锌离子浓度为0.1到1mmol/L时，存在较好的线性关系；且该系统可以同时用于可视化监测，图像的分辨率为18.73lp/mm。
在第六章中，设计了一种新颖的微结构光纤二氧化碳传感器。以具有547孔的微结构光纤作为二氧化碳气体传感器的基质材料，在其内表面修饰二氧化碳传感膜——苯酚红与十六烷基三甲基氢氧化铵形成的离子对的乙基纤维素膜。在该传感器中，微结构光纤一方面起到传光的作用，另一方面也作为气体的传输通道和反应室，通过离子对的颜色变化实现对二氧化碳浓度的检测。这种结构不仅使传感探头的结构微小化，紧凑化，而且获得了较大的传感膜面积。除此之外，此气体传感器可分别采用自动和手动进气，使用灵活方便。经过对二氧化碳的响应能力进行考察，此传感器性能稳定、重复性好。
在第七章，对博士研究期间的工作进行了总结，并对今后的发展提出了展望。
Microstructured optical fiber (MOF) has become an important part in fiber field forits unique structure characteristics and optical properties. The characteristics offlexibleness and easy process etc. of microstructured polymer optical fiber (MPOF) arealso an active research focus. In this thesis, we have explored and studied a series of thefabrication technology of MPOF, the modification of the holes, the filling of the holesand the application of MPOF, especially its application as imaging-transmitting andchemical sensing medium.
The development history of optical fiber technology, the current status ofdevelopments of MOF, the technology of fiber imaging, and the current status ofdevelopments and research of optical fiber chemical sensor are briefly introduced in thefirst chapter. Based on this introduction, this thesis’characteristics and significance areproposed.
In the second chapter, the fabrication methods of MPOF was introduced andcompared, based on which the excuding-moulding method is proposed for fabrication oflarge-sized preforms. The study is made on the tehchnics of fabricating large-sizedMPOF performs and the required conditions (temperature, the rate of delivering perform,drawing speed) how to fabricate a well regular MPOF.
In the third chapter, the imaging capabilities of home-made MPOF with525holesrectangular array and547holes hexagonal array as air-core-array fiber are investigated.Then the liquid core array MOF which has imaging capabilities is fabricated byinjecting the high refractive index liquid into the array holes of MOF. The experimentsdemonstrate that the self of MOF and liquid core MOF have the imaging capabilities.Especially the liquid core array MOF that we make is firstly reported in the world andbreaks the history of liquid core fiber without the abilities of imaging.
In the fourth chapter, a fiber optical probe with function of imaging is firstly prepared. Namely, a gradient index (GRIN) lens rod which was modified by pHsensitive film is connected with a polymer imaging fiber. By connecting the other endface of imaging fiber, Laser, CCD camera, improved metallographic microscope andspectrometer, a demo system of bifunctional optical sensor with imaging capabilities isprepared. On the one hand, the technique overcomes the difficulties that the traditionalpH meter is difficult for remote detection and can not detect in organism. On the otherhand, it overcomes the difficulties that the large sample can not brought to themicroscope stage when fine observing. Moreover, it can provide real-time imagingwhen pH sensing in organism. The corrosion behavior of iron was successfullyinvestivated by employing this sensor. The experiments demonstrated that in pH2.0buffer solutions, the pH value of the iron surface was about0.2pH unit higher than thatof the buffer solutions, the pH value of screw with thick rust cladding about0.65pHunit higher than that of the buffer solutions. In the pH2.9buffer solutions, the pHvalues of iron surface and rust surface were approximately0.16and0.9pH unit higherthan that of buffer solutions, respectively.
In the fifth chapter, based on the tester assembled in fourth chapter, a new ideaabout Zn(II) sensor was proposed. A novel fluorescent sensor for Zn(II) detection isdeveloped by incorporating1-(2-pyridylazo)-2-naphthol (PAN) and Rhodamine B (RB)instead of expensive zinc ion sensitive fluorescent dye in a sol–gel film. Anothertechnical difficulty is the preparation of sensing film. The common film such ascellulose film and traditional acid catalyzed sol-gel is not suitable for immobilizing Zincion indicators. The base catalyzed sol was prepared, with the addition of two couplingreagents for improving the adherence of the sensing film with glass, and more suitablefor zinc ion detection. The sensor has the linear range of Zn(II) from0.1to1mmol/L.Simultaneously, it has the capabilities of real-time imaging with the whole system’sresolution of18.73line pairs/mm.
In the sixth chapter, a novel carbon dioxide sensor of MPOF is designed. A MOFwith547holes is firstly employed as the substrate of carbon dioxide sensor. The inner surface of MOF is modified by sensing film of ethyl cellulose embedding ion pair ofphenol red and hexadecyltrimethylammonium hydroxide. In this sensor, the fiber on theone hand has the role of light transmission; On the other hand, the MOF is thetransmission channel of gases and reaction chamber for the detection of carbon dioxideconcentration through the cholor changes of ion pair. The structure of this sensor makeitself minimal and compact with big sensing acreage. Besides, this sensor can inhalegases by automatic and manual operation which makes it agiler. The investigation of thesensor’s response capabilities demonstrates that the sensor has steady performance andwell repetition.
In the seventh chapter, a conclusion is made about the word during the studies ofPh.D. candidate, and the developments in the future is proposed.
引文
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