技术领域technical field
本发明属于有机纳米材料制备技术领域，特别涉及一种基于纳米孔隙结构的无序增益介质的制备方法。The invention belongs to the technical field of preparation of organic nanomaterials, in particular to a preparation method of a disordered gain medium based on a nanoporous structure.
背景技术Background technique
随机激光指的是光子在无序增益介质中的多重散射所形成的受激辐射现象，其振荡模式决定于多重散射过程，并输出一个非定向的相关光。由于光子在介质中的行进路径是随机的，“随机激光(Random Laser)”这一名称在1995年首次被提出。随后，各国科学家在多种无序增益介质中都观测到了随机激光辐射现象，对无序增益介质中所发生的复杂物理过程的认识也逐渐清晰。随机激光由于其独特的物理机制和广泛的应用前景，近年来在激光物理与光电子技术领域受到了广泛的关注。Random laser refers to the stimulated emission phenomenon formed by the multiple scattering of photons in the disordered gain medium. Its oscillation mode is determined by the multiple scattering process and outputs a non-directional correlated light. Since the path of photons in the medium is random, the name "Random Laser" was first proposed in 1995. Subsequently, scientists from various countries have observed random laser radiation phenomena in various disordered gain media, and their understanding of the complex physical processes that occur in disordered gain media has gradually become clear. Due to its unique physical mechanism and wide application prospects, random laser has received extensive attention in the fields of laser physics and optoelectronics technology in recent years.
近年来，关于随机激光在光电子领域中的应用研究引起了科学家们的极大兴趣，而研究热点又主要集中在无序增益介质的制备方法上。目前比较常见的无序增益介质的类型主要有激光晶体粉末，激光染料与金属氧化物颗粒组成的胶体悬浮溶液，掺有激光染料与散射颗粒的聚合物薄片或薄膜，半导体薄膜或团簇样品，激光染料与液晶混合物等。然而，上述这些制备方法在应用上都有着多方面的不足，例如随机构型不可控、稳定性差、集成度低等。由随机激光的工作原理可知，辐射光的特性决定于光子在介质中的多重散射过程，而多重散射又受散射颗粒的形态参数影响。因此，要实现对辐射光的控制，就必须通过改变散射颗粒的形状、尺寸以及填充密度等方面参数来实现。另一方面，根据Mie散射理论，要使光子发生有效的多重散射过程，其散射颗粒的尺度必须与光波长可比拟。对于我们感兴趣的有源光器件的光学波段，对应的散射颗粒尺度应该是纳米量级。In recent years, the research on the application of random lasers in the field of optoelectronics has aroused great interest among scientists, and the research hotspots mainly focus on the preparation methods of disordered gain media. At present, the common types of disordered gain media mainly include laser crystal powder, colloidal suspension solution composed of laser dye and metal oxide particles, polymer flakes or films mixed with laser dye and scattering particles, semiconductor thin film or cluster samples, Laser dye and liquid crystal mixture, etc. However, the above-mentioned preparation methods have many shortcomings in application, such as uncontrollable random configuration, poor stability, and low integration degree. According to the working principle of random laser, the characteristics of radiated light are determined by the multiple scattering process of photons in the medium, and the multiple scattering is affected by the shape parameters of the scattering particles. Therefore, in order to realize the control of radiated light, it must be realized by changing the parameters such as the shape, size and packing density of the scattering particles. On the other hand, according to the Mie scattering theory, in order for photons to undergo an effective multiple scattering process, the size of the scattering particles must be comparable to the wavelength of light. For the optical band of the active optical device we are interested in, the corresponding scattering particle size should be on the order of nanometers.
目前，纳米结构的制备方法很多，如电子束光刻、反应离子刻蚀、电子束蒸发和剥离技术以及飞秒激光直写等技术。但是，这些技术所需的设备比较昂贵，成本高，工艺复杂，不利于纳米有源光器件的大规模推广，而纳米孔隙结构的制备工艺则能够解决上述的问题。At present, there are many methods for preparing nanostructures, such as electron beam lithography, reactive ion etching, electron beam evaporation and lift-off technology, and femtosecond laser direct writing technology. However, the equipment required by these technologies is expensive, costly, and complicated, which is not conducive to the large-scale promotion of nano-active optical devices, and the preparation process of nano-porous structures can solve the above problems.
发明内容Contents of the invention
本发明克服了现有技术中的缺点，提供了一种基于纳米孔隙结构的无序增益介质的制备方法，该方法步骤简单、成本低廉、绿色通用。利用该技术制备的纳米孔隙薄膜，其孔隙形貌均一，分散性好，而且孔隙的尺寸和填充率等结构参数可通过制备过程中的工艺参数进行有效控制。所获得的无序增益介质，其随机激光的发光强度较高，模式稳定性好，可用于制备有源光波导器件，也可光学显示、光学传感等方面得到广泛应用。The invention overcomes the disadvantages in the prior art, and provides a preparation method of a disordered gain medium based on a nanoporous structure, and the method has simple steps, low cost, and is green and universal. The nanoporous film prepared by this technology has uniform pore morphology and good dispersion, and the structural parameters such as pore size and filling rate can be effectively controlled by the process parameters in the preparation process. The obtained disordered gain medium has high luminous intensity of random laser and good mode stability, can be used to prepare active optical waveguide devices, and can also be widely used in optical display, optical sensing and the like.
为了解决上述技术问题，本发明是通过以下技术方案实现的：In order to solve the above technical problems, the present invention is achieved through the following technical solutions:
一种基于纳米孔隙结构的无序增益介质的制备方法，包括以下步骤：A method for preparing a disordered gain medium based on a nanoporous structure, comprising the following steps:
a、基片清洗；a. Substrate cleaning;
b、将甲醇和THF以4:1的比例混合均匀作为溶剂；取相同重量的PMMA和PS混合作为溶质，PMMA和PS的平均分子量分别为100000和70000，以质量百分比为4％的比例配置溶液，并搅拌均匀；b. Mix methanol and THF uniformly in a ratio of 4:1 as a solvent; mix PMMA and PS with the same weight as a solute, the average molecular weights of PMMA and PS are 100,000 and 70,000 respectively, and configure the solution at a ratio of 4% by mass , and stir evenly;
c、将激光染料若丹明6G(Rh6G)加入步骤b所得溶液中，并加入1-2ml甲基丙烯酸羟乙酯作为助溶剂，染料浓度控制在5*10-3mol/L左右，磁力搅拌20-30分钟，得到橙色透明溶液；c. Add the laser dye rhodamine 6G (Rh6G) to the solution obtained in step b, and add 1-2ml hydroxyethyl methacrylate as a co-solvent, control the dye concentration at about 5*10-3 mol/L, and stir magnetically After 20-30 minutes, an orange transparent solution was obtained;
d、利用旋涂仪将步骤c所得溶液旋涂在硅片上，环境温度控制在20～25℃左右，相对湿度低于40％；d. Spin-coat the solution obtained in step c on the silicon wafer with a spin coater, the ambient temperature is controlled at about 20-25°C, and the relative humidity is lower than 40%;
e、将步骤d所得薄膜放入真空干燥箱中，以70℃干燥15分钟，对薄膜进行热固化，即可得到薄膜样品；e. Put the film obtained in step d into a vacuum drying oven, dry at 70°C for 15 minutes, and heat-cure the film to obtain a film sample;
f、将步骤e所得的薄膜样品放入环己烷溶液中，并加热到60℃，1分钟后取出，可将样品中的PS去除；再将样品以70℃干燥15分钟，最终获得PMMA和空气孔隙结构的薄膜样品。f. Put the film sample obtained in step e into a cyclohexane solution, and heat it to 60°C, take it out after 1 minute, and remove the PS in the sample; then dry the sample at 70°C for 15 minutes, and finally obtain PMMA and Film samples with air-porous structures.
进一步，所述基片清洗包括去离子水冲洗，浓硫酸去除金属氧化物，丙酮去除油脂，氨水去除残余浓硫酸，双氧水冲洗以及烘干。Further, the cleaning of the substrate includes rinsing with deionized water, removing metal oxides with concentrated sulfuric acid, removing grease with acetone, removing residual concentrated sulfuric acid with ammonia water, rinsing with hydrogen peroxide and drying.
进一步，所述旋涂过程先以500～700rpm的低速预转，时间为几秒钟，并在预转过程中往硅片上滴入溶液，目的是初步将多余的溶液甩掉；然后进行高速旋转，转速在2000～4000rpm之间选择，持续时间为40秒左右，通过改变转速和持续时间控制薄膜厚度。Further, the spin coating process is first pre-rotated at a low speed of 500-700rpm for a few seconds, and the solution is dripped onto the silicon wafer during the pre-rotation process, the purpose is to initially shake off the excess solution; Rotate, the speed is selected between 2000 ~ 4000rpm, the duration is about 40 seconds, and the thickness of the film is controlled by changing the speed and duration.
与现有技术相比，本发明的有益效果是：Compared with prior art, the beneficial effect of the present invention is:
本发明所述的一种基于纳米孔隙结构无序增益介质的制备方法，采用操作简易的旋涂成膜法，采用甲醇和四氢呋喃(THF)作为混合溶剂，利用PMMA和PS作为薄膜基材，通过旋涂法在薄膜中形成相分离结构，用选择性溶剂环己烷将PS去除后即可获得由PMMA与空气纳米孔隙组成的二维无序介质样品，该方法成本低、简便、环保，适用于多种不同基材和发光中心的无序增益介质的制备。采用本方法获得的纳米孔隙无序增益介质，其散射单元大小较均一、分散性好，并可以通过改变制备工艺参数来控制其尺寸、形状和填充率等形貌参数，从而实现对随机激光输出模式的控制。这种高发光效率的无序增益介质可用于制备有源光波导器件，也可光学显示、光学传感等方面得到广泛应用。A method for preparing a disordered gain medium based on a nanoporous structure according to the present invention adopts an easy-to-operate spin-coating film-forming method, uses methanol and tetrahydrofuran (THF) as a mixed solvent, and uses PMMA and PS as a film substrate. The spin-coating method forms a phase-separated structure in the film, and the two-dimensional disordered medium sample composed of PMMA and air nanopores can be obtained after removing the PS with the selective solvent cyclohexane. Preparation of disordered gain media on a variety of different substrates and luminescent centers. The nanoporous disordered gain medium obtained by this method has a relatively uniform size of the scattering unit and good dispersion, and its size, shape and filling rate can be controlled by changing the preparation process parameters, so as to achieve random laser output. mode control. The disordered gain medium with high luminous efficiency can be used to prepare active optical waveguide devices, and can also be widely used in optical display, optical sensing and the like.
附图说明Description of drawings
附图用来提供对本发明的进一步理解，与本发明的实施例一起用于解释本发明，并不构成对本发明的限制，在附图中：Accompanying drawing is used for providing further understanding to the present invention, is used for explaining the present invention together with the embodiment of the present invention, does not constitute limitation of the present invention, in accompanying drawing:
图1为制备纳米孔隙薄膜的扫描电子显微镜图；Fig. 1 is the scanning electron microscope picture that prepares nanoporous film;
图2为制备的无序增益介质在不同激光脉冲能量激发下的辐射光谱图；Figure 2 is the radiation spectrum diagram of the prepared disordered gain medium excited by different laser pulse energies;
图3为制备的无序增益介质随机激光辐射的输入—输出曲线；Fig. 3 is the input-output curve of the random laser radiation of the prepared disordered gain medium;
具体实施方式detailed description
以下结合附图对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。The preferred embodiments of the present invention will be described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.
基于纳米孔隙结构的无序增益介质制备，具体步骤如下：The preparation of disordered gain medium based on nanoporous structure, the specific steps are as follows:
1、选用硅片的直径为1英寸，晶向为[111]型，表明不平整度小于1微米。用去离子水反复冲洗基片，去掉基片上面物理吸附的灰尘；将基片放入浓硫酸中煮沸，以便去除基片表面的有机杂质和金属氧化物；用去离子水反复冲洗基片；然后用丙酮超声清洗，去掉各种油脂；将基片放入氨水中煮沸，去除残存的浓硫酸；用双氧水与去离子水反复冲洗用氨水清洗过的基片；将基片放入烘箱中烘干，备用。1. The diameter of the selected silicon wafer is 1 inch, and the crystal orientation is [111] type, indicating that the unevenness is less than 1 micron. Rinse the substrate repeatedly with deionized water to remove physically adsorbed dust on the substrate; boil the substrate in concentrated sulfuric acid to remove organic impurities and metal oxides on the surface of the substrate; repeatedly rinse the substrate with deionized water; Then ultrasonically clean with acetone to remove all kinds of grease; boil the substrate in ammonia water to remove the remaining concentrated sulfuric acid; rinse the substrate cleaned with ammonia water repeatedly with hydrogen peroxide and deionized water; put the substrate in an oven for drying Dried and set aside.
2、分别取甲醇和四氢呋喃40ml和10ml混合均匀作为溶剂；取PMMA和PS各0.8g混合作为溶质，PMMA和PS的平均分子量分别为100000和70000。磁力搅拌至PMMA和PS完全溶解。2. Take 40ml and 10ml of methanol and tetrahydrofuran and mix them uniformly as a solvent; take 0.8g of PMMA and PS and mix them as a solute. The average molecular weights of PMMA and PS are 100,000 and 70,000, respectively. Stir magnetically until the PMMA and PS are completely dissolved.
3、将0.12g若丹明6G(Rh6G)加入步骤2所得溶液中，并加入2ml甲基丙烯酸羟乙酯(HEMA)作为助溶剂，磁力搅拌30分钟至染料充分溶解，得到橙色透明溶液。3. Add 0.12g of rhodamine 6G (Rh6G) to the solution obtained in step 2, and add 2ml of hydroxyethyl methacrylate (HEMA) as a co-solvent, stir magnetically for 30 minutes until the dye is fully dissolved, and an orange transparent solution is obtained.
4、利用旋涂仪将步骤3所得溶液旋涂在硅片上，环境温度控制在20～25℃左右，相对湿度低于40％。旋涂过程先以500rpm的低速预转，时间通常为几秒钟，并在预转过程中往硅片上滴入溶液，目的是初步将多余的溶液甩掉；然后进行高速旋转，转速为3000rpm，持续时间通常为40秒。这一阶段中固定在转盘轴心上的硅片飞速旋转，同时空气的流动使溶剂挥发加剧，在基片上形成一层均匀的聚合物薄膜。4. The solution obtained in step 3 is spin-coated on the silicon wafer by using a spin coater, and the ambient temperature is controlled at about 20-25° C., and the relative humidity is lower than 40%. The spin coating process is pre-rotated at a low speed of 500rpm, usually for a few seconds, and the solution is dripped onto the silicon wafer during the pre-rotation process, the purpose is to initially shake off the excess solution; then high-speed rotation, the speed is 3000rpm , usually with a duration of 40 seconds. In this stage, the silicon wafer fixed on the axis of the turntable rotates rapidly, and at the same time, the flow of air intensifies the volatilization of the solvent, forming a uniform polymer film on the substrate.
5、将步骤4所得薄膜放入真空干燥箱中，以70℃干燥15分钟，对薄膜进行热固化，即可得到粘附性和机械强度较好的薄膜样品。5. Put the film obtained in step 4 into a vacuum drying oven, dry at 70° C. for 15 minutes, and heat-cure the film to obtain a film sample with good adhesion and mechanical strength.
6、将步骤5所得的薄膜样品放入环己烷溶液中，并加热到60℃，1分钟后取出，可将样品中的聚苯乙烯(PS)去除。将样品以70℃干燥15分钟，最终获得PMMA和空气孔隙结构的薄膜样品。样品的SEM形貌如图1所示。6. Put the film sample obtained in step 5 into the cyclohexane solution, and heat it to 60° C., take it out after 1 minute, and the polystyrene (PS) in the sample can be removed. The samples were dried at 70°C for 15 minutes to finally obtain film samples with PMMA and air pore structures. The SEM morphology of the samples is shown in Figure 1.
7、利用倍频的Nd:YAG激光作为激励光，对样品进行光致发光实验，可获得随机激光辐射的光谱图和输入—输出曲线，分别如图2、3所示，图2的上中下线分别是0.018mJ，0.012mJ，0.006mJ。7. Use the frequency-doubled Nd:YAG laser as the excitation light to conduct a photoluminescence experiment on the sample, and obtain the spectrum diagram and input-output curve of random laser radiation, as shown in Figures 2 and 3, respectively, and the upper middle of Figure 2 The lower line is 0.018mJ, 0.012mJ, 0.006mJ respectively.
如果在有机溶液配置的过程中加入适量的激光染料，使染料分子嵌入聚甲基丙烯酸甲脂(PMMA)基质中，即可获得用于产生随机激光的无序增益介质。以纳米孔隙作为无序介质的散射中心，为随机激光的产生提供多重散射过程。If an appropriate amount of laser dye is added during the preparation of the organic solution to embed the dye molecules in the polymethyl methacrylate (PMMA) matrix, a disordered gain medium for generating random laser light can be obtained. Using nanopores as scattering centers in disordered media provides multiple scattering processes for random laser generation.
采用相位分离原理和传统的旋涂成膜工艺制备纳米孔隙聚合物薄膜。这种工艺只包括简单的溶液涂布和蒸发两个过程，它要求形成膜层的物质必须能溶解在某种溶剂中。由于旋涂成膜工艺及设备较其它成膜技术简单很多，它已经被广泛应用于微电路制造、光盘镀膜、光器件制备、增透膜制作等多个领域。对于大部分的聚合物来讲，只要选择合适的溶剂就能够将其溶解并形成均匀稳定的溶液；而且聚合物的分子量一般都很大，其溶液具有足够好的粘滞力和成膜特性。The nanoporous polymer film was prepared by phase separation principle and traditional spin-coating film-forming process. This process only includes two processes of simple solution coating and evaporation, and it requires that the material forming the film must be soluble in a certain solvent. Because the spin-coating film-forming process and equipment are much simpler than other film-forming technologies, it has been widely used in many fields such as microcircuit manufacturing, optical disk coating, optical device preparation, and anti-reflection film production. For most polymers, as long as a suitable solvent is selected, they can be dissolved and form a uniform and stable solution; and the molecular weight of the polymer is generally large, and the solution has good enough viscosity and film-forming properties.
纳米孔隙聚合物薄膜的制备又不同于简单的旋膜，它的主要特点是将两种聚合物共溶于一种溶剂，成膜后两种聚合物发生相分离，从而形成其中一相是离散分布，另一相是连续分布的特殊结构。然后，将薄膜浸入选择性溶剂中，这种溶剂只能溶解其中一种聚合物而不能溶解另一种。当去除掉其中离散分布的聚合物后就形成了纳米孔隙聚合物薄膜，从而获得一种二维的无序介质结构。我们只要在聚合物溶液的配置过程中加入适当的激光染料，染料分子基团就会嵌入到聚合物中，从而形成能够产生随机激光输出的无序增益介质。The preparation of nanoporous polymer films is different from that of simple spinning films. Its main feature is that two polymers are co-dissolved in a solvent. After film formation, the two polymers undergo phase separation, thereby forming one of the phases is discrete distribution, and the other phase is a special structure of continuous distribution. Then, the film is dipped in a selective solvent that dissolves only one of the polymers but not the other. A nanoporous polymer film is formed when the discretely distributed polymers are removed, resulting in a two-dimensional disordered dielectric structure. As long as we add appropriate laser dyes during the configuration of the polymer solution, the dye molecular groups will be embedded in the polymer, thereby forming a disordered gain medium capable of generating random laser output.
采用激光对样品进行激发，则染料分子作为发光中心会形成受激跃迁并产生随机激光输出。该方法成本低，操作简便，适用于其他有机基质材料和增益物质的有源纳米器件的制备。Laser is used to excite the sample, and the dye molecules, as the luminescent center, will form excited transitions and generate random laser output. The method is low in cost and easy to operate, and is suitable for the preparation of active nanometer devices of other organic matrix materials and gain substances.
采用本方法制得的无序增益介质，其散射颗粒形状规则、均匀性好、尺寸可控。这种高发光效率的纳米孔隙无序增益材料可作为新型的有源光功能材料，在有机光波导器件、光学显示、光学传感等方面都具有广泛的应用前景。开发基于纳米孔隙结构的无序增益介质的简易制备技术，对化学、材料以及光电子等学科的发展都具有重要的推动意义。The disordered gain medium prepared by the method has regular shape of scattering particles, good uniformity and controllable size. This nanoporous disordered gain material with high luminous efficiency can be used as a new type of active optical functional material, and has broad application prospects in organic optical waveguide devices, optical displays, and optical sensing. The development of a simple preparation technology for disordered gain media based on nanoporous structures is of great significance to the development of chemistry, materials, and optoelectronics.
这种高发光效率的无序增益介质可用于制备有源光波导器件，也可光学显示、光学传感等方面得到广泛应用。The disordered gain medium with high luminous efficiency can be used to prepare active optical waveguide devices, and can also be widely used in optical display, optical sensing and the like.
最后应说明的是：以上仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换，但是凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。Finally, it should be noted that the above are only preferred embodiments of the present invention, and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the embodiments, those skilled in the art can still understand the foregoing The technical solutions recorded in each embodiment are modified, or some of the technical features are equivalently replaced, but within the spirit and principles of the present invention, any modifications, equivalent replacements, improvements, etc., shall be included in the present invention within the scope of protection.
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| CN201610861230.6ACN106329306B (en) | 2016-09-28 | 2016-09-28 | A kind of preparation method of disordered gain medium based on nanoporous structure |
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| CN201610861230.6ACN106329306B (en) | 2016-09-28 | 2016-09-28 | A kind of preparation method of disordered gain medium based on nanoporous structure |
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