CN109298481B - The metallic silver filling photonic crystal fiber and its preparation method of spontaneous generation SPR effect - Google Patents
The metallic silver filling photonic crystal fiber and its preparation method of spontaneous generation SPR effect Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 87
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Abstract
一种自发产生SPR效应的金属银填充光子晶体光纤及其制法,属于光纤智能通信技术领域。该光纤包括纤芯和包层,纤芯为实心石英玻璃棒,包层包括石英玻璃毛细管、空气孔和银丝,所述的纤芯的纵向四周设置有多层石英玻璃毛细管,在第二层石英玻璃毛细管中,其中一根石英玻璃毛细管的气孔设置银丝。其制法为:设计结构,排布结构和拉制光纤,制得的光纤可以自发的产生SPR效应。该方法可制作出不同空气孔结构和尺寸的自发产生SPR效应的光子晶体光纤,无需后续对光纤进行镀膜或填充,并且通过调整空气孔的直径、填充银丝直径、毛细管外径可使共振峰的位置可调,性能良好,同时还具有结构简单,制备方便,可调节等优点,可应用于多种光学元件的制作。
The invention relates to a silver-filled photonic crystal optical fiber spontaneously generating SPR effect and a manufacturing method thereof, belonging to the technical field of optical fiber intelligent communication. The optical fiber comprises a core and a cladding, the core is a solid silica glass rod, and the cladding includes a silica glass capillary, air holes and silver wires, the longitudinal periphery of the core is provided with multi-layer silica glass capillaries, and the second layer In the quartz glass capillary, the air hole of one of the quartz glass capillary is provided with a silver wire. The preparation method is as follows: designing the structure, arranging the structure and drawing the optical fiber, and the prepared optical fiber can spontaneously generate the SPR effect. This method can produce photonic crystal fibers with different air hole structures and sizes that spontaneously generate the SPR effect, without subsequent coating or filling of the optical fiber, and by adjusting the diameter of the air hole, the diameter of the filled silver wire, and the outer diameter of the capillary, the resonance peak can be made The position is adjustable, the performance is good, and it also has the advantages of simple structure, convenient preparation, adjustable, etc., and can be applied to the production of various optical elements.
Description
技术领域technical field
本发明属于光纤智能通信技术领域,涉及光纤器件的制造,具体涉及一种自发产生SPR效应的金属银填充光子晶体光纤及其制法。The invention belongs to the technical field of optical fiber intelligent communication, relates to the manufacture of optical fiber devices, in particular to a metallic silver-filled photonic crystal optical fiber with SPR effect spontaneously generated and a manufacturing method thereof.
背景技术Background technique
1996年Knight,J.C.等人成功拉制出第一根折射率引导型光子晶体光纤后,光子晶体光纤进入了广大研究学者的视野,激发了巨大的研究热情,同时也为科研领域带来了新的发展方向。与传统光纤相比,光子晶体光纤的结构设计更为灵活,可以产生许多“奇异”的特性,如无截止的单模传输、损耗低、色散可控、非线性特性、高双折射特性等等,因此光子晶体光纤受到极大的重视,使其在通信领域、传感检测、以及光学器件的制备等领域有了广泛的应用。In 1996, after Knight, J.C. and others successfully drew the first refractive index-guided photonic crystal fiber, photonic crystal fiber entered the field of vision of many researchers, aroused great enthusiasm for research, and brought new technologies to the field of scientific research. direction of development. Compared with traditional optical fibers, the structural design of photonic crystal fibers is more flexible, and can produce many "singular" characteristics, such as unlimited single-mode transmission, low loss, controllable dispersion, nonlinear characteristics, high birefringence characteristics, etc. , so photonic crystal fiber has received great attention, making it widely used in the field of communication, sensing and detection, and the preparation of optical devices.
表面等离子体共振(Surface Plasmon Resonance,SPR)是金属的表面等离子体激源被激发而产生的一种共振现象。早在1968年,奥托和克雷奇曼就各自报道了一种用玻璃棱镜可见光的耦合器激发表面等离子体激源的方法。这种方便的结构引起了广泛的关注,早期将SPR原理用于生物传感器的设计。随着研究的不断深入,越来越多的学者将SPR原理与光纤结构相结合,应用也越来越广泛,不仅应用于传感领域,在滤波器、分束器等光学器件的设计中也有所应用。2018年,Yong Wang等人在商用的光子晶体光纤光纤表面镀上一层几十纳米厚的银膜,利用PDMS材料实现温度传感。这种方法需要在光纤的表面再次进行修饰进而产生SPR效应。2007年,Alireza Hassani设计了光子晶体光纤结构,结合SPR效应提出了一种新型的传感器,并在理论上分析了该传感器的性能。虽然传感器的性能很好,但是这种光纤并没有制作出来。不仅在传感领域有所应用,2016年Guowen An等人利用光子晶体光纤与SPR原理的结合设计了一种光纤滤波器。Surface plasmon resonance (Surface Plasmon Resonance, SPR) is a resonance phenomenon produced by the excitation of metal surface plasmon sources. As early as 1968, Otto and Krechman each reported a method of exciting a surface plasmon source using a glass prism visible light coupler. This convenient structure has attracted extensive attention, and the principle of SPR was used in the design of biosensors in the early days. With the deepening of research, more and more scholars have combined the SPR principle with the fiber structure, and the application has become more and more extensive, not only in the field of sensing, but also in the design of optical devices such as filters and beam splitters. applied. In 2018, Yong Wang et al. coated a layer of silver film tens of nanometers thick on the surface of a commercial photonic crystal fiber, and used PDMS material to realize temperature sensing. This method requires another modification on the surface of the fiber to generate the SPR effect. In 2007, Alireza Hassani designed a photonic crystal fiber structure, combined with the SPR effect to propose a new type of sensor, and theoretically analyzed the performance of the sensor. Although the sensor performed well, the fiber had not yet been fabricated. Not only has it been applied in the field of sensing, in 2016, Guowen An et al. designed a fiber filter by combining the principle of photonic crystal fiber and SPR.
由此可以见得,光子晶体光纤光纤与SPR原理的结合有着广泛的应用,而且有着很好的应用前景。It can be seen that the combination of photonic crystal fiber and SPR principle has a wide range of applications, and has a good application prospect.
发明内容Contents of the invention
本发明所要解决的技术问题是:针对现有技术的不足,免除复杂的金属膜制作工艺,提供一种自发产生SPR效应的金属银填充光子晶体光纤及其制法,该光纤可以自发的产生SPR效应。通过本发明的方法可以精确的制作出不同空气孔结构和尺寸的自发产生SPR效应的光子晶体光纤,不需要后续对光纤进行镀膜或填充,并且通过调整空气孔的直径、填充银丝直径、石英玻璃毛细管外径可以使共振峰的位置可调,性能良好,同时还具有结构简单,制备方便,可调节等优点,可以应用于传感器、滤波器、偏振器、分束器等光学元件的制作。The technical problem to be solved by the present invention is: aiming at the deficiencies of the prior art, avoiding the complex metal film manufacturing process, providing a metal silver-filled photonic crystal fiber and its manufacturing method that spontaneously generates the SPR effect, and the fiber can spontaneously generate the SPR effect. The method of the present invention can accurately produce photonic crystal fibers with different air hole structures and sizes that spontaneously generate the SPR effect. The outer diameter of the glass capillary can make the position of the resonance peak adjustable, and has good performance. It also has the advantages of simple structure, convenient preparation, and adjustment. It can be applied to the production of optical components such as sensors, filters, polarizers, and beam splitters.
本发明解决上述技术问题所采用的技术方案为:The technical solution adopted by the present invention to solve the problems of the technologies described above is:
一种自发产生SPR效应的金属银填充光子晶体光纤,为光纤包层结构,具体包括纤芯和包层,所述的纤芯为实心石英玻璃棒,所述的包层包括石英玻璃毛细管、空气孔和银丝,空气孔分为三种:A metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect is an optical fiber cladding structure, specifically comprising a core and a cladding, the core being a solid silica glass rod, the cladding comprising a silica glass capillary, air Holes and silver wires, air holes are divided into three types:
第一种:石英玻璃毛细管的气孔;The first type: the pores of the quartz glass capillary;
第二种:石英玻璃毛细管彼此之间间隔的缝隙;The second type: the gap between the quartz glass capillary tubes;
第三种:石英玻璃毛细管和实心石英玻璃棒之间间隔的缝隙;The third type: the gap between the quartz glass capillary and the solid quartz glass rod;
所述的纤芯的纵向四周设置有多层石英玻璃毛细管,在第二层石英玻璃毛细管中,其中一根石英玻璃毛细管的气孔设置银丝。There are multiple layers of quartz glass capillary tubes arranged around the longitudinal periphery of the fiber core, and in the second layer of quartz glass capillary tubes, a silver wire is arranged in the pores of one of the quartz glass capillary tubes.
所述的空气孔可以使所述的包层的有效折射率低于纤芯,保证光在光纤纤芯中传播。The air hole can make the effective refractive index of the cladding lower than that of the fiber core, so as to ensure the propagation of light in the fiber core.
所述的银丝,其设置在石英玻璃毛细管的空气孔中,该银丝可以使光纤形成SPR效应。The silver wire is arranged in the air hole of the quartz glass capillary, and the silver wire can make the optical fiber form the SPR effect.
所述的自发产生SPR效应的金属银填充光子晶体光纤中,所述的包层还包括石英玻璃外套管和实心石英玻璃填充丝,将设置有多层石英玻璃毛细管的纤芯,套入石英玻璃外套管中,在最外层石英玻璃毛细管和石英玻璃外套管之间的缝隙填充实心石英玻璃填充丝。In the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect, the cladding also includes a quartz glass outer sleeve and a solid quartz glass filling wire, and the core that is provided with a multilayer quartz glass capillary is inserted into the quartz glass In the outer sleeve, the gap between the outermost quartz glass capillary and the outer sleeve is filled with solid quartz glass filling wire.
所述的石英透明毛细管在纤芯纵向四周呈六边形分布,即从纤芯里向外方向,第一层石英透明毛细管为6个,第二层石英透明毛细管为12个,第三层石英透明毛细管为18个,……,第n层石英透明毛细管为6n个。The quartz transparent capillaries are distributed in a hexagonal shape around the longitudinal direction of the fiber core, that is, from the inside of the fiber core to the outside, there are 6 quartz transparent capillaries in the first layer, 12 quartz transparent capillaries in the second layer, and 12 quartz transparent capillaries in the third layer. There are 18 transparent capillaries, ..., and there are 6n quartz transparent capillaries in the nth layer.
所述的自发产生SPR效应的金属银填充光子晶体光纤的直径为120~200微米;所述的实心石英玻璃棒的直径为7~20微米,优选为10~15微米,所述的石英玻璃毛细管的直径为7~20微米,优选为10~15微米;石英玻璃毛细管的气孔形成的空气孔孔径为4~6微米;填充银丝的石英玻璃毛细管的气孔孔径为6~7微米。The diameter of the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect is 120-200 microns; the diameter of the solid quartz glass rod is 7-20 microns, preferably 10-15 microns, and the quartz glass capillary The diameter of the pore is 7-20 microns, preferably 10-15 microns; the pore diameter of the air hole formed by the pores of the quartz glass capillary is 4-6 microns; the pore diameter of the quartz glass capillary filled with silver wire is 6-7 microns.
所述的自发产生SPR效应的金属银填充光子晶体光纤,其实心石英玻璃填充丝为不同直径的实心石英玻璃填充丝,其设置的目的在于,在拉制形成的自发产生SPR效应的金属银填充光子晶体光纤不会留有缝隙。The metallic silver-filled photonic crystal optical fiber that spontaneously produces the SPR effect, its solid quartz glass filling filaments are solid quartz glass filling filaments of different diameters. Photonic crystal fibers leave no gaps.
本发明的自发产生SPR效应的金属银填充光子晶体光纤的制备方法,包括以下步骤:The preparation method of the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect of the present invention comprises the following steps:
步骤1:根据实际需求进行自发产生SPR效应的金属银填充光子晶体光纤结构的设计,并利用仿真软件对自发产生SPR效应的金属银填充光子晶体光纤的传输性能进行理论模拟,得到拟制备自发产生SPR效应的金属银填充光子晶体光纤的光谱;Step 1: Design the metal silver-filled photonic crystal fiber structure that spontaneously generates the SPR effect according to actual needs, and use simulation software to theoretically simulate the transmission performance of the metal silver-filled photonic crystal fiber that spontaneously generates the SPR effect, and obtain the proposed spontaneous generation Spectrum of metallic silver filled photonic crystal fiber with SPR effect;
步骤2:根据设计的满足要求的自发产生SPR效应的金属银填充光子晶体光纤的结构,制作实心石英玻璃棒、石英玻璃毛细管和多个实心石英玻璃填充丝,筛选、清洗后,将银丝插入其中一根石英玻璃毛细管的气孔内;其中,实心石英玻璃棒、石英玻璃毛细管的外径相等;Step 2: According to the designed structure of the metallic silver-filled photonic crystal fiber that can spontaneously generate the SPR effect and meet the requirements, make a solid quartz glass rod, a quartz glass capillary, and multiple solid quartz glass filling wires. After screening and cleaning, insert the silver wire into the In the stomata of one of the quartz glass capillary tubes; wherein, the outer diameters of the solid quartz glass rod and the quartz glass capillary tube are equal;
以实心石英玻璃棒作为纤芯,从纤芯纵向四周逐层排列设置多层石英玻璃毛细管,将插入银丝的石英玻璃毛细管置于第二层,每层设置的石英毛细管以六边形排布,每层设置后均固定,设置完成后,将设置有石英玻璃毛细管的纤芯放置在石英玻璃外套管中,石英玻璃毛细管和石英玻璃外套管之间的缝隙用不同直径的实心石英玻璃填充丝填充,得到光纤预制棒;A solid quartz glass rod is used as the core, and multilayer quartz glass capillaries are arranged layer by layer from the longitudinal periphery of the fiber core, and the quartz glass capillaries inserted with silver wires are placed on the second layer, and the quartz capillaries arranged in each layer are arranged in a hexagonal shape , each layer is fixed after being set, and after the setting is completed, the core with the quartz glass capillary is placed in the quartz glass outer sleeve, and the gap between the quartz glass capillary and the quartz glass outer sleeve is filled with solid quartz glass filaments of different diameters Filling to obtain an optical fiber preform;
步骤3:使用拉丝塔的固定装置将光纤预制棒固定,将光纤预制棒的一端穿入两端开口的石墨炉中,光纤预制棒的最低端面低于石墨炉中最高温度点位置,石墨炉加热至光纤预制棒软化;Step 3: Use the fixing device of the drawing tower to fix the optical fiber preform, and put one end of the optical fiber preform into the graphite furnace with openings at both ends. The lowest end face of the optical fiber preform is lower than the highest temperature point in the graphite furnace, and the graphite furnace is heated until the optical fiber preform is softened;
光纤预制棒的最低端面料头掉落,光纤预制棒被拉细,控制拉丝塔的辅助牵引轮,实现持续拉丝,通过调节加热温度、牵引速度和送棒速度,控制拉丝的尺寸,得到自发产生SPR效应的金属银填充光子晶体光纤。The lowest end fabric head of the optical fiber preform falls, and the optical fiber preform is thinned. Control the auxiliary pulley of the drawing tower to achieve continuous drawing. By adjusting the heating temperature, pulling speed and rod feeding speed, the size of the drawing is controlled to obtain spontaneous production. Metallic silver filled photonic crystal fiber for SPR effect.
所述的步骤2中,所述的纤芯,纤芯的折射率为1.45,纤芯的直径为1~2mm。In the step 2, the refractive index of the fiber core is 1.45, and the diameter of the fiber core is 1-2 mm.
所述的步骤2中,所述的石英玻璃毛细管的直径为1~2mm,并且其直径与纤芯直径相等,所述的石英玻璃毛细管的气孔直径为0.325~0.65mm。In the step 2, the diameter of the quartz glass capillary is 1-2 mm, which is equal to the diameter of the fiber core, and the diameter of the pores of the quartz glass capillary is 0.325-0.65 mm.
所述的步骤2中,所述的石英玻璃毛细管的气孔直径根据实际需要进行设计,尺寸不同得到光纤的传输性能不同,SPR效应的吸收峰的位置不同,优选内径为0.325~0.65mm。In the step 2, the pore diameter of the quartz glass capillary is designed according to actual needs. Different sizes result in different transmission properties of optical fibers and different positions of absorption peaks of the SPR effect. The preferred inner diameter is 0.325-0.65 mm.
所述的步骤2中,设置有银丝的石英玻璃毛细管的气孔直径根据实际需要进行设计,尺寸不同得到光纤的传输性能不同,SPR效应的吸收峰的位置不同。In step 2, the pore diameter of the quartz glass capillary provided with the silver wire is designed according to actual needs. Different sizes result in different transmission properties of the optical fiber and different positions of the absorption peaks of the SPR effect.
所述的步骤2中,所述的银丝的直径<石英玻璃毛细管的气孔直径,这是因为,由于熔化的银与空气相比,粘度和表面张力都较大,其目的是为保证拉制出来的光纤中填充银的空气孔与其他空气孔尺寸相近。In the described step 2, the diameter of the silver wire<the pore diameter of the quartz glass capillary, this is because, compared with air, the viscosity and surface tension of the molten silver are larger, and its purpose is to ensure that the drawn The silver-filled air holes in the emerging fiber are similar in size to the other air holes.
所述的步骤2中,所述的实心石英玻璃填充丝的直径<实心石英玻璃棒的直径。In the step 2, the diameter of the solid quartz glass filling filament is smaller than the diameter of the solid quartz glass rod.
所述的步骤2中,所述的石英玻璃外套管的外径为13~20mm,内径为7.5~14.5mm,便于光纤预制棒的制作。In the step 2, the outer diameter of the quartz glass outer tube is 13-20 mm, and the inner diameter is 7.5-14.5 mm, which is convenient for making the optical fiber preform.
所述的步骤3中,所述的加热温度为1790℃~1820℃。In the step 3, the heating temperature is 1790°C-1820°C.
所述的步骤3中,所述的牵引速度为0.8~2.4m/min。In the step 3, the pulling speed is 0.8-2.4m/min.
所述的步骤3中,所述的送棒速度为1.5mm/min~3.8mm/min。In the step 3, the rod feeding speed is 1.5mm/min-3.8mm/min.
本发明的一种自发产生SPR效应的金属银填充光子晶体光纤及其制法,其工作原理为:A kind of metal silver filled photonic crystal fiber and its preparation method that spontaneously produces SPR effect of the present invention, its working principle is:
该结构光子晶体光纤的中心是由实心石英玻璃棒制成,周围由带有空气孔的石英毛细管组成,空气孔可使所述包层的有效折射率低于纤芯,形成纤芯折射率高于周围包层的结构,使光在该光纤中以全内反射的形式向前传输,空气孔中填充银丝可使光纤形成SPR效应。光在纤芯和包层的界面发生全反射,形成的倏逝波具有一定的穿透能力。当倏逝波与银相接触时,会激发金属银表面的自由电子规律的震荡,形成表面等离子波。光波与表面等离子体波满足相位匹配条件时就会发生共振,称之为SPR。当共振发生时,会有大部分能量被吸收,所以会在吸收光谱中形成一个明显的吸收峰。The center of the structured photonic crystal fiber is made of a solid silica glass rod, surrounded by a quartz capillary with air holes, the air holes can make the effective refractive index of the cladding lower than that of the core, forming a core with a high refractive index. The structure of the surrounding cladding enables the light to transmit forward in the form of total internal reflection in the fiber, and the air hole is filled with silver wire to make the fiber form the SPR effect. The light is totally reflected at the interface between the core and the cladding, and the evanescent wave formed has a certain penetrating ability. When the evanescent wave contacts the silver, it will excite the free electrons on the surface of the silver metal to vibrate regularly, forming a surface plasmon wave. Resonance occurs when light waves and surface plasmon waves meet the phase matching conditions, which is called SPR. When resonance occurs, most of the energy will be absorbed, so an obvious absorption peak will be formed in the absorption spectrum.
与现有技术相比,本发明的优点在于:本发明公开的一种可自发产生SPR效应的光子晶体光纤制备方法,其制作过程简单、方便、可控,相比于现有的在光纤表面镀膜以及在光纤空气孔内壁镀金属膜的方法优势显著。而且,这种新型光子晶体光纤的制作方法是通用的,可以灵活的设计光子晶体光纤的结构,通过调整空气孔的排列,尺寸的大小等参数,改变光纤的性能。本发明的提出为光子晶体光纤,特别是结合SPR效应的光子晶体光纤的设计与制作提供了一种行之有效的新方法。Compared with the prior art, the present invention has the advantages of: a photonic crystal optical fiber preparation method that can spontaneously generate the SPR effect disclosed by the present invention, its manufacturing process is simple, convenient and controllable, compared with the existing method on the surface of the optical fiber The method of coating and coating the metal film on the inner wall of the optical fiber air hole has significant advantages. Moreover, the manufacturing method of this new type of photonic crystal fiber is universal, and the structure of the photonic crystal fiber can be flexibly designed, and the performance of the fiber can be changed by adjusting parameters such as the arrangement and size of air holes. The proposal of the invention provides an effective new method for the design and manufacture of photonic crystal fiber, especially photonic crystal fiber combined with SPR effect.
本发明设计了一种自发产生SPR效应的金属银填充光子晶体光纤,可以自发产生SPR效应,无需后续对光纤进行复杂的镀膜或填充处理,同样可以应用于传感领域以及光学器件的制作,省去了复杂而昂贵的磁控溅射、化学气相沉积等镀膜方法,并且在纤芯和石英玻璃毛细管之间的缝隙、以及石英玻璃毛细管彼此之间的缝隙,认为是规则排列空气孔,大大的降低了制作的复杂度以及成本。本发明是一种通用的设计和制备方法,同样适用于其他光子晶体光纤结构。The present invention designs a metal silver-filled photonic crystal fiber that spontaneously produces the SPR effect, which can spontaneously produce the SPR effect without subsequent complicated coating or filling treatment on the optical fiber, and can also be applied to the sensing field and the production of optical devices, saving Complicated and expensive coating methods such as magnetron sputtering and chemical vapor deposition have been eliminated, and the gap between the fiber core and the quartz glass capillary, and the gap between the quartz glass capillary, is considered to be a regular arrangement of air holes, a large The complexity and cost of production are reduced. The invention is a general design and preparation method, which is also applicable to other photonic crystal fiber structures.
附图说明Description of drawings
图1是本发明自发产生SPR效应的金属银填充光子晶体光纤截面结构示意图;Fig. 1 is the schematic diagram of the cross-sectional structure of a photonic crystal fiber filled with metallic silver that spontaneously produces the SPR effect of the present invention;
图中,1为石英玻璃毛细管的气孔;2为银丝;3为纤芯;4为石英玻璃毛细管;5为最外层石英玻璃毛细管和石英玻璃外套管之间的缝隙;6为石英玻璃外套管;7为石英玻璃毛细管彼此之间间隔的缝隙;In the figure, 1 is the air hole of the quartz glass capillary; 2 is the silver wire; 3 is the fiber core; 4 is the quartz glass capillary; 5 is the gap between the outermost quartz glass capillary and the quartz glass outer tube; 6 is the quartz glass jacket Tube; 7 is the gap between the quartz glass capillary tubes;
d1为石英玻璃毛细管的直径;d2为石英玻璃毛细管的气孔形成的空气孔孔径;d3为填充银丝的石英玻璃毛细管的气孔孔径。d 1 is the diameter of the quartz glass capillary; d 2 is the diameter of the air hole formed by the pores of the quartz glass capillary; d 3 is the diameter of the air hole in the quartz glass capillary filled with silver wire.
图2是本发明实施例的自发产生SPR效应的金属银填充光子晶体光纤截面显微镜图。Fig. 2 is a microscope view of a section of a metal silver-filled photonic crystal fiber that spontaneously produces the SPR effect according to an embodiment of the present invention.
图3是本发明自发产生SPR效应的金属银填充光子晶体光纤制作过程示意图。Fig. 3 is a schematic diagram of the manufacturing process of the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect of the present invention.
图4是本发明用仿真软件模拟的自发产生SPR效应的金属银填充光子晶体光纤的光谱。Fig. 4 is the spectrum of the metal silver filled photonic crystal fiber which spontaneously produces the SPR effect simulated by the simulation software of the present invention.
图5是本发明制备的自发产生SPR效应的金属银填充光子晶体光纤的测量光谱。Fig. 5 is the measured spectrum of the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect prepared by the present invention.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步的详细说明。The present invention will be described in further detail below in conjunction with embodiment.
以下实施例中,采用仿真软件为Comsol。In the following embodiments, the simulation software used is Comsol.
为使上述目的、优点更加易懂,下面将通过实施例详细描述本发明提供的一种自发产生SPR效应的金属银填充光子晶体光纤及其制备方法。但是本领域的技术人员应该意识到在权利要求的范围内,可以做出形式和细节上多种变形,因此本发明绝不仅限于以下所述的实施例。In order to make the above purpose and advantages easier to understand, a metallic silver-filled photonic crystal fiber that spontaneously generates the SPR effect provided by the present invention and its preparation method will be described in detail below through examples. However, those skilled in the art will appreciate that various changes in form and details may be made within the scope of the claims, and therefore the present invention is by no means limited to the embodiments described below.
实施例1Example 1
一种自发产生SPR效应的金属银填充光子晶体光纤,为光纤包层结构,具体包括纤芯和包层,所述的纤芯3为实心石英玻璃棒,所述的包层包括石英玻璃毛细管4、空气孔和银丝2,空气孔分为三种:A metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect, which is an optical fiber cladding structure, specifically including a core and a cladding, the core 3 is a solid silica glass rod, and the cladding includes a silica glass capillary 4 , air hole and silver wire 2, the air hole is divided into three types:
第一种:石英玻璃毛细管的气孔1;The first type: the pores 1 of the quartz glass capillary;
第二种:石英玻璃毛细管彼此之间间隔的缝隙7;The second type: the gap 7 between the quartz glass capillary tubes;
第三种:石英玻璃毛细管和实心石英玻璃棒之间间隔的缝隙;The third type: the gap between the quartz glass capillary and the solid quartz glass rod;
所述的纤芯3的纵向四周设置有多层石英玻璃毛细管4,在第二层石英玻璃毛细管中,其中一根石英玻璃毛细管的气孔设置银丝2。The fiber core 3 is provided with multiple layers of quartz glass capillary tubes 4 around its vertical direction, and in the second layer of quartz glass capillary tubes, a silver wire 2 is provided in the pores of one of the quartz glass capillary tubes.
所述的空气孔可以使所述的包层的有效折射率低于纤芯,保证光在光纤纤芯中传播。The air hole can make the effective refractive index of the cladding lower than that of the fiber core, so as to ensure the propagation of light in the fiber core.
所述的银丝2,其设置在石英玻璃毛细管的空气孔中,该银丝可以使光纤形成SPR效应。The silver wire 2 is arranged in the air hole of the quartz glass capillary, and the silver wire can make the optical fiber form the SPR effect.
所述的自发产生SPR效应的金属银填充光子晶体光纤中,所述的包层还包括石英玻璃外套管6和实心石英玻璃填充丝,将设置有多层石英玻璃毛细管的纤芯,套入石英玻璃外套管6中,在最外层石英玻璃毛细管和石英玻璃外套管之间的缝隙5填充实心石英玻璃填充丝。In the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect, the cladding also includes a quartz glass outer sleeve 6 and a solid quartz glass filling wire, and the core that is provided with a multilayer quartz glass capillary is inserted into the quartz glass In the glass outer tube 6 , the gap 5 between the outermost quartz glass capillary and the quartz glass outer tube is filled with solid quartz glass filler wire.
所述的石英透明毛细管4在纤芯3纵向四周呈六边形分布,即从纤芯里向外方向,第一层石英透明毛细管为6个,第二层石英透明毛细管为12个,第三层石英透明毛细管为18个。Described quartz transparent capillary 4 is hexagonally distributed around the longitudinal direction of fiber core 3, that is, from the inside of the fiber core outward, there are 6 quartz transparent capillaries in the first layer, 12 quartz transparent capillaries in the second layer, and 12 in the third layer. There are 18 layers of quartz transparent capillaries.
所述的自发产生SPR效应的金属银填充光子晶体光纤的直径为150微米;所述的实心石英玻璃棒的直径为15微米,所述的石英玻璃毛细管4的直径d1为15微米;石英玻璃毛细管的气孔1形成的空气孔孔径d2为4.9微米;填充银丝的石英玻璃毛细管的气孔孔径d3为7微米。The diameter of the photonic crystal fiber filled with metallic silver that spontaneously produces the SPR effect is 150 microns; the diameter of the solid quartz glass rod is 15 microns, and the diameter d1 of the quartz glass capillary 4 is 15 microns; The air hole diameter d2 formed by the pores 1 of the capillary is 4.9 microns; the air hole diameter d3 of the quartz glass capillary filled with silver wire is 7 microns.
所述的自发产生SPR效应的金属银填充光子晶体光纤,其实心石英玻璃填充丝为不同直径的实心石英玻璃填充丝,其设置的目的在于,在拉制形成的自发产生SPR效应的金属银填充光子晶体光纤不会留有缝隙。The metallic silver-filled photonic crystal optical fiber that spontaneously produces the SPR effect, its solid quartz glass filling filaments are solid quartz glass filling filaments of different diameters. Photonic crystal fibers leave no gaps.
一种自发产生SPR效应的金属银填充光子晶体光纤的制备方法,包括以下步骤:A method for preparing a metal silver-filled photonic crystal fiber that spontaneously produces an SPR effect, comprising the following steps:
步骤1:根据实际需求进行自发产生SPR效应的金属银填充光子晶体光纤结构的设计,其自发产生SPR效应的金属银填充光子晶体光纤截面结构示意图见图1,设计得到的自发产生SPR效应的金属银填充光子晶体光纤的直径为150微米;所述的实心石英玻璃棒的直径为15微米,所述的石英玻璃毛细管的直径d1为15微米;石英玻璃毛细管的气孔形成的空气孔孔径d2为4.9微米;填充银丝的石英玻璃毛细管的气孔孔径d3为7微米。Step 1: Design the metal silver-filled photonic crystal fiber structure that spontaneously produces the SPR effect according to actual needs. The schematic diagram of the cross-sectional structure of the metal silver-filled photonic crystal fiber that spontaneously produces the SPR effect is shown in Figure 1. The designed metal silver-filled photonic crystal fiber that spontaneously produces the SPR effect The diameter of the silver-filled photonic crystal fiber is 150 microns; the diameter of the solid quartz glass rod is 15 microns, and the diameter d1 of the quartz glass capillary is 15 microns; the air hole diameter d2 formed by the pores of the quartz glass capillary It is 4.9 microns; the pore diameter d3 of the quartz glass capillary filled with silver wire is 7 microns.
并利用仿真软件对自发产生SPR效应的金属银填充光子晶体光纤的传输性能进行理论模拟,得到拟制备自发产生SPR效应的金属银填充光子晶体光纤的光谱;通过光谱可以得到其共振吸收峰位于1450纳米波长处,该光谱见图4。And use the simulation software to theoretically simulate the transmission performance of the metal silver-filled photonic crystal fiber that spontaneously produces the SPR effect, and obtain the spectrum of the metal silver-filled photonic crystal fiber that is to be prepared to spontaneously produce the SPR effect; through the spectrum, it can be obtained that its resonance absorption peak is located at 1450 At nanometer wavelengths, the spectrum is shown in Figure 4.
步骤2:根据设计的满足要求的自发产生SPR效应的金属银填充光子晶体光纤的结构,制作实心石英玻璃棒、石英玻璃毛细管和多个实心石英玻璃填充丝,筛选、清洗后,将直径为0.5毫米的银丝插入其中一根石英玻璃毛细管的气孔内;其中,实心石英玻璃棒、石英玻璃毛细管的外径均为2毫米;Step 2: According to the structure of the metal silver-filled photonic crystal fiber that meets the requirements and spontaneously produces the SPR effect, make a solid quartz glass rod, a quartz glass capillary, and a plurality of solid quartz glass filling wires. After screening and cleaning, the diameter is 0.5 A silver wire of 2 mm is inserted into the air hole of one of the quartz glass capillary tubes; wherein, the outer diameters of the solid quartz glass rod and the quartz glass capillary tube are both 2 mm;
其中,实心石英玻璃棒是对外径为20毫米的玻璃棒拉制,得到直径为2毫米的实心石英玻璃棒,其拉制工艺为:牵引速度0.6m/min,送棒速度6mm/min,加热温度1920℃;Among them, the solid quartz glass rod is drawn from a glass rod with an outer diameter of 20 mm to obtain a solid quartz glass rod with a diameter of 2 mm. The drawing process is as follows: pulling speed 0.6 m/min, rod feeding speed 6 mm/min, heating Temperature 1920°C;
其中,石英玻璃毛细管是对外径为20毫米内径为6.5毫米的玻璃棒拉制,得到外径为2毫米、内径为0.65毫米的石英玻璃毛细管,其拉制工艺为:牵引速度0.59m/min,送棒速度6mm/min,加热温度1920℃。Among them, the quartz glass capillary is drawn from a glass rod with an outer diameter of 20 mm and an inner diameter of 6.5 mm to obtain a quartz glass capillary with an outer diameter of 2 mm and an inner diameter of 0.65 mm. The drawing process is: pulling speed 0.59m/min, The rod feeding speed is 6mm/min, and the heating temperature is 1920°C.
以实心石英玻璃棒作为纤芯,从纤芯纵向四周逐层排列设置多层石英玻璃毛细管,将插入银丝的石英玻璃毛细管置于第二层,每层设置的石英毛细管以六边形排布,每层设置后均用胶带固定,设置完成后,将设置有石英玻璃毛细管的纤芯放置在石英玻璃外套管中,石英玻璃毛细管和石英玻璃外套管之间的缝隙用不同直径的实心石英玻璃填充丝填充,得到光纤预制棒;由于熔化的银与空气相比,粘度和表面张力都较大,所以为保证拉制出来的光纤中填充银的空气孔与其他空气孔尺寸相近,选择银丝直径小于毛管内径。A solid quartz glass rod is used as the core, and multilayer quartz glass capillaries are arranged layer by layer from the longitudinal periphery of the fiber core, and the quartz glass capillaries inserted with silver wires are placed on the second layer, and the quartz capillaries arranged in each layer are arranged in a hexagonal shape After each layer is set, it is fixed with adhesive tape. After the setting is completed, the core with the quartz glass capillary is placed in the quartz glass outer tube. The gap between the quartz glass capillary and the quartz glass outer tube is made of solid quartz glass with different diameters. Filling with filling wire to obtain optical fiber preform; since molten silver has higher viscosity and surface tension than air, in order to ensure that the air hole filled with silver in the drawn optical fiber is similar to the size of other air holes, silver wire is selected The diameter is smaller than the inner diameter of the capillary.
所述的石英玻璃外套管的外径为13~20mm,内径为7.5~14.5mm,便于光纤预制棒的制作。The outer diameter of the quartz glass outer tube is 13-20mm, and the inner diameter is 7.5-14.5mm, which is convenient for making the optical fiber preform.
步骤3:使用拉丝塔的固定装置三角抓将光纤预制棒固定,将光纤预制棒的一端穿入两端开口的石墨炉中,光纤预制棒的最低端面低于石墨炉中最高温度点位置,石墨炉加热至光纤预制棒软化;Step 3: Fix the optical fiber preform with the triangular grip of the fixing device of the drawing tower, and put one end of the optical fiber preform into the graphite furnace with openings at both ends. The lowest end face of the optical fiber preform is lower than the highest temperature point in the graphite furnace. The furnace is heated until the optical fiber preform is softened;
光纤预制棒的最低端面料头掉落,光纤预制棒被拉细,控制拉丝塔的辅助牵引轮,实现持续拉丝,通过调节加热温度、牵引速度和送棒速度,控制拉丝的尺寸,得到自发产生SPR效应的金属银填充光子晶体光纤。The lowest end fabric head of the optical fiber preform falls, and the optical fiber preform is thinned. Control the auxiliary pulley of the drawing tower to achieve continuous drawing. By adjusting the heating temperature, pulling speed and rod feeding speed, the size of the drawing is controlled to obtain spontaneous production. Metallic silver filled photonic crystal fiber for SPR effect.
在拉丝过程中,加热温度为1790℃~1820℃进行调整;所述的牵引速度为0.8-2.4m/min进行调整;所述的送棒速度为1.5mm/min-3.8mm/min进行调整,控制拉制自发产生SPR效应的金属银填充光子晶体光纤的尺寸。同时不断的使用显微镜观察光纤端面,查看光子晶体光纤的内部结构,直至得到所需要的光子晶体光纤。经光谱仪检测,得到的输出光谱在1450nm附近存在一个吸收峰,该光谱见图5。During the wire drawing process, the heating temperature is adjusted at 1790°C to 1820°C; the pulling speed is adjusted at 0.8-2.4m/min; the rod feeding speed is adjusted at 1.5mm/min-3.8mm/min, Controlling the size of drawn metallic silver-filled photonic crystal fibers that spontaneously generate the SPR effect. At the same time, the end face of the optical fiber is continuously observed with a microscope, and the internal structure of the photonic crystal fiber is checked until the required photonic crystal fiber is obtained. Detected by the spectrometer, the output spectrum obtained has an absorption peak near 1450nm, which is shown in Figure 5.
通过图4的模拟光谱和图5的测量光谱对比,证明得到了设计的自发产生SPR效应的金属银填充光子晶体光纤,并且该光纤能够自发产生SPR效应。By comparing the simulated spectrum in Figure 4 with the measured spectrum in Figure 5, it is proved that the designed metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect is obtained, and the fiber can spontaneously produce the SPR effect.
实施例2Example 2
一种自发产生SPR效应的金属银填充光子晶体光纤,同实施例1。A metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect is the same as that in Embodiment 1.
一种自发产生SPR效应的金属银填充光子晶体光纤的制备方法,其制备工艺流程见图3,包括以下步骤:A method for preparing a metal silver-filled photonic crystal fiber that spontaneously produces an SPR effect, the preparation process of which is shown in Figure 3, including the following steps:
1)设计了如图1所示的自发产生SPR效应的金属银填充光子晶体光纤,根据仿真软件对自发产生SPR效应的金属银填充光子晶体光纤的传输性能进行理论模拟,制备的自发产生SPR效应的金属银填充光子晶体光纤直径为150微米,纤芯3和石英玻璃毛细管4直径d1为15微米,石英玻璃毛细管的气孔形成的空气孔孔径d2为4.9微米,银丝填充的直径d3为7微米。通过仿真软件计算,共振吸收峰位于1450纳米波长处。1) The metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect as shown in Figure 1 is designed, and the transmission performance of the metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect is theoretically simulated according to the simulation software, and the prepared spontaneously produces the SPR effect The metal silver-filled photonic crystal fiber has a diameter of 150 microns, the diameter d1 of the core 3 and the quartz glass capillary 4 is 15 microns, the diameter d2 of the air hole formed by the pores of the quartz glass capillary is 4.9 microns, and the diameter d3 of the silver wire filling is 7 microns. Calculated by simulation software, the resonant absorption peak is located at a wavelength of 1450 nanometers.
2)根据设计的结构制作外径为2毫米的石英玻璃毛细管和实心石英玻璃棒;2) According to the designed structure, the outer diameter is 2 mm quartz glass capillary and solid quartz glass rod;
其中,实心石英玻璃棒的制作过程为:使用直径20毫米的玻璃棒拉制直径2毫米的实心石英玻璃棒,其中,拉制过程中,牵引速度为0.6m/min,送棒速度为6mm/min,加热温度为1920℃。Among them, the production process of the solid quartz glass rod is: use a glass rod with a diameter of 20 mm to draw a solid quartz glass rod with a diameter of 2 mm, wherein, during the drawing process, the pulling speed is 0.6 m/min, and the rod feeding speed is 6 mm/min. min, the heating temperature is 1920°C.
其中,石英玻璃毛细管的制作过程为:外径20毫米,内径6.5毫米的玻璃管,拉制外径2毫米、内径0.65毫米的石英玻璃毛细管,其中,拉制过程中,牵引速度为0.59m/min,送棒速度为6mm/min,加热温度为1920℃。Among them, the production process of the quartz glass capillary is: a glass tube with an outer diameter of 20 mm and an inner diameter of 6.5 mm, drawing a quartz glass capillary with an outer diameter of 2 mm and an inner diameter of 0.65 mm, wherein, during the drawing process, the pulling speed is 0.59m/ min, the rod feeding speed is 6mm/min, and the heating temperature is 1920°C.
3)通过筛选、清洗之后,将直径0.5毫米银丝填入一根石英玻璃毛细管的气孔中,然后排放于第二层,并且每层利用胶带固定,将其放入大直径的石英玻璃外套管中,周围空隙使用不同直径的实心石英玻璃填充丝填满,得到光纤预制棒。由于熔化的银与空气相比,粘度和表面张力都较大,所以为保证拉制出来的光纤中填充银的空气孔与其他空气孔尺寸相近,选择银丝直径小于毛管内径。3) After screening and cleaning, fill the silver wire with a diameter of 0.5 mm into the pores of a quartz glass capillary, and then discharge it on the second layer, and fix each layer with adhesive tape, and put it into a large diameter quartz glass outer tube In the process, the surrounding voids are filled with solid quartz glass filler wires of different diameters to obtain optical fiber preforms. Compared with air, molten silver has higher viscosity and surface tension, so in order to ensure that the air hole filled with silver in the drawn optical fiber is similar to other air holes in size, the diameter of the silver wire is selected to be smaller than the inner diameter of the capillary.
4)使用拉丝塔的三角抓将光纤预制棒固定,将光纤预制棒底端穿过石墨炉中,最低端面低于石墨炉温度最高点位置,加热至光纤预制棒中的石英玻璃软化。利用光纤预制棒的最低端面料头掉落的重力将光纤预制棒拉细,并使用拉丝塔的辅助牵引轮实现持续拉丝。同时不断的在石墨炉内充入高纯氩气,作为保护气。4) Use the triangular grip of the drawing tower to fix the optical fiber preform, pass the bottom end of the optical fiber preform through the graphite furnace, the lowest end surface is lower than the highest temperature point of the graphite furnace, and heat until the quartz glass in the optical fiber preform is softened. The optical fiber preform is thinned by the falling gravity of the lowest end fabric head of the optical fiber preform, and the auxiliary traction wheel of the drawing tower is used to achieve continuous drawing. At the same time, the graphite furnace is continuously filled with high-purity argon as a protective gas.
5)拉丝过程中,在1790℃~1820℃范围内调整加热温度,牵引速度在0.8-2.4m/min之间调整,以及送棒速度在1.5mm/min-3.8mm/min之间调整,控制拉制自发产生SPR效应的金属银填充光子晶体光纤的尺寸。同时不断的使用显微镜观察光纤端面,查看光子晶体光纤的内部结构,直至得到所需要的光子晶体光纤,其中,自发产生SPR效应的金属银填充光子晶体光纤截面示意图见图2。经光谱仪检测,得到的输出光谱在1450nm附近存在一个吸收峰。5) During the wire drawing process, adjust the heating temperature within the range of 1790°C to 1820°C, adjust the pulling speed between 0.8-2.4m/min, and adjust the rod feeding speed between 1.5mm/min-3.8mm/min, control Drawing a metallic silver-filled photonic crystal fiber that spontaneously produces the SPR effect to size. At the same time, use a microscope to observe the end face of the fiber and check the internal structure of the photonic crystal fiber until the required photonic crystal fiber is obtained. Among them, the cross-sectional schematic diagram of the silver-filled photonic crystal fiber that spontaneously produces the SPR effect is shown in Figure 2. Detected by a spectrometer, the obtained output spectrum has an absorption peak around 1450nm.
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