技术领域technical field
本发明涉及激光技术领域，尤其涉及可调控的掺染料和金属纳米粒子的PDLC光纤及其光纤随机激光器。The invention relates to the field of laser technology, in particular to a PDLC optical fiber doped with dyes and metal nanoparticles and an optical fiber random laser which can be regulated.
背景技术Background technique
近年来，随机激光已经成为国际激光学界的热门研究领域。随机激光辐射源自激活无序介质，通过辐射光在介质中的多次散射提供光学反馈，从而获得较大的增益，无需外加谐振腔。随机激光由于独特的物理机制和在光电子和生物医学方面的潜在应用而吸引了越来越多的关注。许多有源和无源材料能够被用来产生随机激光，例如：ZnO粉末，聚合物，染料掺杂液晶，染料掺杂聚合物分散液晶。最近几年，研究发现金属纳米结构体能够极大增强半导体量子阱，稀土，染料的自发辐射率，这是由于辐射中心和金属表面等离子之间的相互共振所影响。利用这些特点，一些研究者报道了随机激光器是由金属纳米颗粒产生的非相干辐射。他们观察到了辐射谱的窄化和辐射强度的增强。这是非相干随机激光器的典型特征。In recent years, random lasers have become a hot research field in the international laser community. The random laser radiation originates from the excited disordered medium, and provides optical feedback through the multiple scattering of the radiated light in the medium, so as to obtain a large gain without an external resonant cavity. Random lasers have attracted increasing attention due to their unique physical mechanisms and potential applications in optoelectronics and biomedicine. Many active and passive materials can be used to generate random lasing, for example: ZnO powder, polymers, dye-doped liquid crystals, dye-doped polymer dispersed liquid crystals. In recent years, studies have found that metal nanostructures can greatly enhance the spontaneous emission rate of semiconductor quantum wells, rare earths, and dyes, which is due to the mutual resonance between the radiation center and the metal surface plasmon. Taking advantage of these features, some researchers reported that random lasers are incoherent radiation produced by metallic nanoparticles. They observed a narrowing of the radiation spectrum and an increase in radiation intensity. This is typical of incoherent random lasers.
聚合物分散液晶(PDLC)是将低分子液晶（liquidcrystal，缩写为LC)与预聚物相混合，在一定条件下经聚合反应，形成微米级或纳米级的液晶微滴均匀地分散在高分子网络中，再利用液晶分子的介电各向异性获得具有电光响应特性的材料，它主要工作在散射态和透明态之间并具有一定的灰度。聚合物分散液晶膜是将液晶和聚合物结合得到的一种综合性能优异的膜材料。液晶分子赋予了聚合物分散液晶膜显著的电光特性，使其受到了广泛的关注，并有着广阔的应用前景。聚合物分散液晶（PDLC）材料已经在可调窗口，平板显示和可调谐布拉格光栅等领域被广泛研究及应用。通用的形成PDLC结构的方法是用光引发聚合包含反应性单聚体和液晶（LC）分子的均匀混合物。这些预聚物一般是无溶剂，低粘度。LC液滴的尺寸取决于LC的浓度以及固化辐射光的强度。通常聚合物的折射率np被调制为接近于液晶的寻常折射率n0。无加载电压时，液晶分子形成随机分布的液滴，即在液晶分子和聚合物接触面形成折射率差，这引起在PDLCs中的光散射。一旦加上电压，液晶分子的轴向将会沿着电场的方向排布，液晶分子与聚合物由于折射率差形成的散射将消失。Polymer-dispersed liquid crystal (PDLC) is to mix low-molecular liquid crystal (liquid crystal, abbreviated as LC) with prepolymer, and undergo polymerization reaction under certain conditions to form micron-scale or nano-scale liquid crystal droplets uniformly dispersed in polymer In the network, the dielectric anisotropy of liquid crystal molecules is used to obtain materials with electro-optic response characteristics. It mainly works between the scattering state and the transparent state and has a certain gray scale. Polymer dispersed liquid crystal film is a film material with excellent comprehensive performance obtained by combining liquid crystal and polymer. Liquid crystal molecules endow polymer-dispersed liquid crystal films with remarkable electro-optic properties, which have attracted extensive attention and have broad application prospects. Polymer dispersed liquid crystal (PDLC) materials have been widely studied and applied in the fields of tunable windows, flat panel displays and tunable Bragg gratings. A common approach to form PDLC structures is photoinitiated polymerization of homogeneous mixtures containing reactive monomers and liquid crystal (LC) molecules. These prepolymers are generally solvent-free, low viscosity. The size of the LC droplets depends on the concentration of the LC and the intensity of the curing radiation. Usually the refractive indexnp of the polymer is modulated to be close to the ordinary refractive indexn0 of the liquid crystal. When no voltage is applied, the liquid crystal molecules form randomly distributed droplets, that is, a refractive index difference is formed at the interface between the liquid crystal molecules and the polymer, which causes light scattering in PDLCs. Once the voltage is applied, the axial direction of the liquid crystal molecules will be arranged along the direction of the electric field, and the scattering formed by the liquid crystal molecules and the polymer due to the difference in refractive index will disappear.
然而，金属纳米粒子作为在染料掺杂液晶或者聚合物分散液晶随机激光器中的散射颗粒很少被关注。很少有人做增益随机介质是由三种不同材料（聚合物分散液晶，金属粒子和染料）的实验，这些材料可以增强多重散射和光增益。而这种增益介质还没有应用于空心光纤中。However, metal nanoparticles have received little attention as scattering particles in dye-doped liquid crystals or polymer-dispersed liquid crystals in random lasers. Few experiments have been done on gain random media consisting of three different materials (polymer-dispersed liquid crystals, metal particles, and dyes) that enhance multiple scattering and optical gain. However, this gain medium has not been used in hollow-core fibers.
发明内容Contents of the invention
为了解决上述技术问题，本发明提出了一种掺染料和金属纳米粒子的聚合物分散液晶PDLC光纤，其包括：空心光纤，空心光纤内固化的掺染料和金属纳米粒子的PDLC聚合物，空心光纤外表面沿轴向镀有氧化铟锡ITO导电层，其特征在于：In order to solve the above technical problems, the present invention proposes a polymer-dispersed liquid crystal PDLC fiber doped with dye and metal nanoparticles, which includes: a hollow fiber, a PDLC polymer doped with dye and metal nanoparticles solidified in the hollow fiber, and a hollow fiber The outer surface is coated with an indium tin oxide ITO conductive layer along the axial direction, which is characterized in that:
所述空心光纤外层采用真空磁控溅射法形成与光纤内径等宽的ITO导电层；将聚合物分散液晶PDLC与激光染料和金属纳米粒子的乙醇溶液以一定质量比制成均相溶液，以毛细孔效应吸入所述空心光纤，经过光照固化填充满所述空心光纤内径使得聚合物折射率大于光纤折射率；通过ITO导电层接正负电压形成电场改变液晶分子轴向，控制随机激光输出。The outer layer of the hollow fiber adopts the vacuum magnetron sputtering method to form an ITO conductive layer with the same width as the inner diameter of the fiber; the polymer dispersed liquid crystal PDLC and the ethanol solution of laser dye and metal nanoparticles are made into a homogeneous solution in a certain mass ratio, The hollow fiber is sucked in by the capillary effect, and the inner diameter of the hollow fiber is filled with light curing so that the refractive index of the polymer is greater than the refractive index of the fiber; the ITO conductive layer is connected with positive and negative voltages to form an electric field to change the axis of the liquid crystal molecules and control the random laser output .
其中，所述空心光纤内径为市售8μm至1000μm空心光纤。Wherein, the inner diameter of the hollow-core fiber is a commercially available hollow-core fiber of 8 μm to 1000 μm.
其中，用丙酮超声或用浓酸腐蚀光纤外层保护树脂，将光纤嵌入高精度玻璃模板中采用真空磁控溅射法形成ITO导电层，导电层与光纤内径等宽。Among them, acetone is used to ultrasonically or concentrated acid is used to corrode the outer protective resin of the optical fiber, and the optical fiber is embedded in a high-precision glass template to form an ITO conductive layer by vacuum magnetron sputtering. The conductive layer is as wide as the inner diameter of the optical fiber.
其中，用于在空心光纤内固化的掺染料和金属粒子的聚合物分散液晶PDLC溶液是将三羟甲基丙烷三丙烯酸酯单体；N-乙烯基吡咯烷酮；玫瑰红；N-苯基甘氨酸；辛酸；液晶；激光染料；金属纳米粒子乙醇溶液以一定质量分数比混合加热遮光搅拌2小时,使混合均匀，形成的均相溶液，均相溶液中各组分所占质量分数范围为：三羟甲基丙烷三丙烯酸酯40.00wt%至50.00wt%；N-乙烯基吡咯烷酮5.00wt%至10.00wt%；玫瑰红0.10wt%至1.00wt%；N-苯基甘氨酸5.00wt%至10.00wt%；辛酸5.00wt%至10.00wt%；液晶30.00wt%至40.00wt%；激光染料1.00wt%至2.00wt%；金属纳米粒子乙醇溶液1.00wt%至3.00wt%。Among them, the polymer-dispersed liquid crystal PDLC solution mixed with dye and metal particles used for solidification in the hollow-core optical fiber is trimethylolpropane triacrylate monomer; N-vinylpyrrolidone; rose bengal; N-phenylglycine; Caprylic acid; liquid crystal; laser dye; metal nanoparticle ethanol solution was mixed with a certain mass fraction ratio, heated and stirred for 2 hours to make the mixture uniform and form a homogeneous solution. The mass fraction range of each component in the homogeneous solution is: trihydroxy Methylpropane triacrylate 40.00wt% to 50.00wt%; N-vinylpyrrolidone 5.00wt% to 10.00wt%; Rose Bengal 0.10wt% to 1.00wt%; N-phenylglycine 5.00wt% to 10.00wt%; Caprylic acid 5.00wt% to 10.00wt%; liquid crystal 30.00wt% to 40.00wt%; laser dye 1.00wt% to 2.00wt%; metal nanoparticle ethanol solution 1.00wt% to 3.00wt%.
其中，选用的金属纳米粒子能够对选用的激光染料有表面等离激元共振荧光增强。Wherein, the selected metal nanoparticles can enhance the surface plasmon resonance fluorescence of the selected laser dye.
其中，所述聚合物均相溶液通过毛细效应吸入空心光纤，之后通过紫外固化灯或Nd:YAG激光器进行光照固化。Wherein, the polymer homogeneous solution is sucked into the hollow fiber by capillary effect, and then cured by ultraviolet light or Nd:YAG laser.
其中，所述空心光纤内固化聚合物折射率大于光纤折射率。Wherein, the refractive index of the cured polymer in the hollow-core optical fiber is greater than that of the optical fiber.
本发明还提出了一种光纤随机激光器，其包括：如上所述掺染料和金属纳米粒子的聚合物分散液晶PDLC光纤、交流电源和泵浦光源扩束汇聚光路,其特征在于:泵浦光经过扩束汇聚光路形成条形光束，垂直照射沿光纤轴向的ITO导电层区域，形成随机激光出射；通过ITO导电层加交流电压在ITO导电层之间形成电场改变液晶分子轴向，控制随机激光输出。The present invention also proposes a fiber optic random laser, which includes: a polymer-dispersed liquid crystal PDLC optical fiber doped with dyes and metal nanoparticles as described above, an AC power supply and a pumping light source beam expanding and converging optical path, characterized in that: the pumping light passes through The beam expands and converges the optical path to form a strip beam, which vertically irradiates the ITO conductive layer area along the fiber axis to form random laser emission; through the ITO conductive layer and AC voltage, an electric field is formed between the ITO conductive layers to change the liquid crystal molecular axis to control the random laser output.
使用本发明的调控掺染料和金属纳米粒子的PDLC光纤随机激光器可以保证随机激光定向输出；空心光纤内无流动液体，为固化聚合物，无沉淀，结构稳定；随机激光阈值相较于其他光纤随机激光器将会显著降低，出射强度显著增强；通过电场控制随机激光出射强度，通断。The use of the PDLC fiber random laser device doped with dyes and metal nanoparticles of the present invention can ensure random laser directional output; there is no flowing liquid in the hollow fiber, which is solidified polymer, no precipitation, and stable structure; the random laser threshold is higher than that of other fiber random lasers. The laser will be significantly reduced, and the output intensity will be significantly enhanced; the random laser output intensity is controlled by the electric field, on and off.
附图说明Description of drawings
图1为与本发明实施例一致的装置结构示意图；Fig. 1 is a schematic diagram of a device structure consistent with an embodiment of the present invention;
图2为与本发明实施例一致的掺染料和金属纳米粒子的PDLC光纤结构示意图，其中，1为Nd：YAG激光器、2为格林兰镜组、3为准直扩束透镜组、4为反射镜，5为柱面透镜、6为掺染料和金属纳米粒子的PDLC心光纤、7为交流电源、8为随机激光输出、9为ITO导电层、10为掺染料和金属纳米粒子的PDLC聚合物、11为空心光纤。Fig. 2 is the schematic diagram of the structure of the PDLC optical fiber doped with dyes and metal nanoparticles consistent with the embodiment of the present invention, wherein, 1 is Nd: YAG laser, 2 is the Greenland mirror group, 3 is the collimating beam expander lens group, 4 is the reflection 5 is cylindrical lens, 6 is PDLC core fiber doped with dye and metal nanoparticles, 7 is AC power supply, 8 is random laser output, 9 is ITO conductive layer, 10 is PDLC polymer doped with dye and metal nanoparticles , 11 is a hollow fiber.
具体实施方法Specific implementation method
下面结合附图和具体实施方式对本发明做进一步说明。The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
本发明的工作原理为：掺染料和金属纳米粒子的PDLC聚合物在空心光纤内径固化过程中，使得微米或纳米尺寸的液晶分子，染料分子，金属纳米粒子均匀固化在聚合物形成的网状结构中，形成稳定结构。用柱面透镜将泵浦光汇聚成条状光斑垂直透过ITO膜照射到光纤上，在不加电压时，液晶的指向矢随机分布，聚合物与液晶折光指数不匹配，泵浦光被液晶分子散射，发生多重散射，形成相干反馈，同时当金属纳米粒子表面等离子共振波长与激发光相匹配，金属纳米粒子局域表面等离子共振场将有效增强纳米粒子附近染料分子的辐射效率，当增益大于损耗时发生受激辐射放大。掺染料和金属纳米粒子的PDLC聚合物的折射率大于空心光纤的折射率，形成二维局域，利用全反射使得出射随机激光局域在光纤内形成定向输出；在加电压时，通过控制电压大小，克服聚合物网络对液晶分子的锚定能，使得液晶分子指向矢统一沿电场方向，液晶微粒折射率与聚合物折射率达到一定程度的匹配，散射能力变化，随机激光出射强度，通断随之改变。The working principle of the present invention is: during the solidification process of the PDLC polymer doped with dyes and metal nanoparticles in the inner diameter of the hollow fiber, the liquid crystal molecules, dye molecules, and metal nanoparticles of micron or nanometer size are uniformly solidified in the network structure formed by the polymer , forming a stable structure. Use a cylindrical lens to gather the pump light into a striped spot and irradiate it on the optical fiber through the ITO film vertically. When no voltage is applied, the director of the liquid crystal is randomly distributed. Molecular scattering, multiple scattering occurs, and coherent feedback is formed. At the same time, when the metal nanoparticle surface plasmon resonance wavelength matches the excitation light, the metal nanoparticle localized surface plasmon resonance field will effectively enhance the radiation efficiency of the dye molecules near the nanoparticle. When the gain is greater than Amplification by stimulated emission occurs when loss occurs. The refractive index of the PDLC polymer doped with dye and metal nanoparticles is greater than that of the hollow fiber, forming a two-dimensional local area, and using total reflection to make the outgoing random laser local area form a directional output in the fiber; when applying voltage, by controlling the voltage Size, to overcome the anchoring energy of the polymer network to the liquid crystal molecules, so that the directors of the liquid crystal molecules are unified along the direction of the electric field, the refractive index of the liquid crystal particles and the polymer refractive index match to a certain extent, the scattering ability changes, the random laser emission intensity, on-off Change accordingly.
掺染料和金属纳米粒子的PDLC光纤制备处理，包含以下步骤：The preparation process of PDLC optical fiber doped with dye and metal nanoparticles comprises the following steps:
（1）选用空心光纤市售内径尺寸（8～1000um），对空心光纤进行处理，对于内径小于100um的空心光纤用丙酮超声5分钟除去光纤表面保护涂覆树脂，对于内径大于100um的空心光纤用强酸腐蚀，洗净吹干。将处理过的光纤嵌入预制好的高精度玻璃模板，只露出光纤上表面和下表面的一部分，利用真空磁控镀膜溅射技术在光纤上下表面沿轴向镀与空心光纤内径等宽的ITO膜。(1) Select the commercially available inner diameter size (8-1000um) of the hollow-core fiber, and process the hollow-core fiber. For the hollow-core fiber whose inner diameter is less than 100um, use acetone to ultrasonically remove the coating resin on the surface of the fiber for 5 minutes. For the hollow-core fiber whose inner diameter is larger than 100um, use Strong acid corrosion, wash and dry. Embed the processed optical fiber into a prefabricated high-precision glass template, and only expose a part of the upper and lower surfaces of the optical fiber, and use the vacuum magnetron coating sputtering technology to coat the upper and lower surfaces of the optical fiber with an ITO film with the same width as the inner diameter of the hollow fiber in the axial direction .
（2）将单体（三羟甲基丙烷三丙烯酸酯）；交联单体（N-乙烯基吡咯烷酮）；光引发剂（玫瑰红）；共引发剂（N-苯基甘氨酸）；表面活性剂（辛酸）；液晶；激光染料；金属纳米粒子乙醇溶液以一定质量分数比混合加热遮光搅拌2小时,使混合均匀，形成的均相溶液。溶液中各组分所占质量分数范围为：三羟甲基丙烷三丙烯酸酯40.00wt%至50.00wt%；N-乙烯基吡咯烷酮5.00wt%至10.00wt%；玫瑰红质量分数0.10wt%至1.00wt%；N-苯基甘氨酸质5.00wt%至10.00wt%；辛酸5.00wt%至10.00wt%；液晶30.00wt%至40.00wt%；激光染料1.00wt%至2.00wt%；金属纳米粒子乙醇溶液1.00wt%至3.00wt%。利用毛细效应将聚合物均相溶液吸入空心光纤，之后用聚合引发相分离法使聚合物固化，具体为用Nd:YAG激光器以532nm波长，光强均匀照射光纤5min～1min进行固化或以紫外固化灯进行固化，改变光照强度以及光照时间控制液晶分子大小，以及聚合物阈值电压。同时，选用金属纳米粒子能够对选用的激光染料有表面等离激元共振荧光增强。聚合物固化后，固化聚合物折射率大于光纤折射率。(2) The monomer (trimethylolpropane triacrylate); cross-linking monomer (N-vinylpyrrolidone); photoinitiator (rose bengal); co-initiator (N-phenylglycine); surface active Liquid crystals; laser dyes; metal nanoparticle ethanol solutions were mixed at a certain mass fraction ratio, heated and stirred for 2 hours in shading to make the mixture uniform and form a homogeneous solution. The mass fraction of each component in the solution ranges from: 40.00wt% to 50.00wt% of trimethylolpropane triacrylate; 5.00wt% to 10.00wt% of N-vinylpyrrolidone; 0.10wt% to 1.00wt% of rose bengal wt%; N-phenylglycine 5.00wt% to 10.00wt%; octanoic acid 5.00wt% to 10.00wt%; liquid crystal 30.00wt% to 40.00wt%; laser dye 1.00wt% to 2.00wt%; metal nanoparticles ethanol solution 1.00wt% to 3.00wt%. The polymer homogeneous solution is sucked into the hollow fiber by capillary effect, and then the polymer is solidified by the polymerization-induced phase separation method, specifically using a Nd:YAG laser with a wavelength of 532nm, The light intensity is uniformly irradiated on the optical fiber for 5 minutes to 1 minute for curing or cured with a UV curing lamp. Change the light intensity and light time to control the size of liquid crystal molecules and the threshold voltage of the polymer. At the same time, the selection of metal nanoparticles can enhance the surface plasmon resonance fluorescence of the selected laser dye. After the polymer is cured, the cured polymer has a refractive index greater than that of the optical fiber.
如图1所示，可调控的掺染料和金属纳米粒子的PDLC光纤随机激光器，包含以下步骤：As shown in Figure 1, the tunable PDLC fiber random laser doped with dyes and metal nanoparticles includes the following steps:
（1）Nd：YAG出射激光1经过格林兰镜组2、准直扩束透镜组3、反射镜4、柱面透镜5聚焦的条形泵浦光垂直照射透过ITO导电层9。(1) The Nd:YAG laser beam 1 passes through the ITO conductive layer 9 vertically through the strip-shaped pump light focused by the Greenland mirror group 2 , the collimator beam expander lens group 3 , the mirror 4 , and the cylindrical lens 5 .
（2）条形泵浦光照射空心光纤11内掺染料和金属纳米粒子的PDLC聚合物10，形成随机激光出射8。(2) Strip pump light irradiates the PDLC polymer 10 doped with dye and metal nanoparticles in the hollow fiber 11 to form random laser emission 8 .
（3）交流电源7连接ITO导电层9，交流电源电极为与光纤ITO层贴合的弧形电极，在ITO层之间形成电场控制液晶分子轴向，调控随机激光出射8。(3) The AC power supply 7 is connected to the ITO conductive layer 9, and the AC power supply electrode is an arc-shaped electrode bonded to the ITO layer of the optical fiber. An electric field is formed between the ITO layers to control the axis of the liquid crystal molecules and regulate the random laser emission 8.
本发明实现掺染料和金属纳米粒子的PDLC光纤随机激光器的随机激光出射，以及对随机激光的电光调控输出。The invention realizes the random laser output of the PDLC fiber random laser doped with the dye and the metal nano particles, and the electro-optical control output of the random laser.
本发明优点在于，首次将掺染料和金属纳米粒子的PDLC聚合物与空心光纤相结合；与液晶盒随机激光相比，光纤结构对出射光形成二维局域，随机激光定向输出；与一般空心光纤随机激光相比，空心光纤内无流动液体，为固化聚合物，无沉淀，结构稳定，金属纳米粒子的局域表面共振有助于降低随机激光阈值，增强出射强度；可通过电压进行对出射随机激光的调控。可以在光通信、传感、生物医学，可调谐窄带相干光源等方面获得应用。The advantage of the present invention is that, for the first time, the PDLC polymer doped with dye and metal nanoparticles is combined with the hollow optical fiber; compared with the random laser of the liquid crystal box, the optical fiber structure forms a two-dimensional local area for the outgoing light, and the random laser directional output; compared with the general hollow laser Compared with fiber random laser, there is no flowing liquid in the hollow fiber, which is a solidified polymer, no precipitation, and stable structure. The local surface resonance of metal nanoparticles helps to reduce the random laser threshold and enhance the output intensity; the output can be controlled by voltage Regulation of random lasers. It can be applied in optical communication, sensing, biomedicine, tunable narrowband coherent light source and so on.
以上所述仅是本发明的优选实施方式，应当指出：对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干可以预期的改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, some predictable improvements and modifications can also be made, these improvements And retouching should also be regarded as the protection scope of the present invention.
| Application Number | Priority Date | Filing Date | Title |
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| CN201310238920.2ACN103311784B (en) | 2013-06-17 | 2013-06-17 | A kind of PDLC optical fiber and optical fiber random laser device thereof mixing dyestuff and metal nanoparticle |
| Application Number | Priority Date | Filing Date | Title |
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| CN201310238920.2ACN103311784B (en) | 2013-06-17 | 2013-06-17 | A kind of PDLC optical fiber and optical fiber random laser device thereof mixing dyestuff and metal nanoparticle |
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