CN114277363A - Film growth method with continuously adjustable optical constant - Google Patents
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Abstract
本发明属于薄膜生长领域，具体涉及一种光学常数连续可调的薄膜生长方法，包括制备前驱液；对基底进行表面处理；处理完成后，在基底上吸附生长一层均匀的液膜；将吸附生长一层均匀的液膜的基底放置在300‑400℃的炉管中低温热处理；为提高效率和提高薄膜质量，低温热处理完成后，可重复液膜生长和低温热处理的操作，得到较厚的膜层；接着将炉管温度升至800‑1300℃进行高温热处理，进而得到光学常数连续可调节的光学薄膜；本发明通过改变前驱液成分、薄膜沉积条件和热处理条件，实现光学常数连续可调，使得滤光膜的膜系结构可以大大简化，缩短工艺时间和成本。
The invention belongs to the field of thin film growth, and in particular relates to a thin film growth method with continuously adjustable optical constants, which includes preparing a precursor liquid; performing surface treatment on a substrate; The substrate on which a uniform liquid film is grown is placed in a furnace tube at 300-400°C for low-temperature heat treatment; in order to improve efficiency and film quality, after the low-temperature heat treatment is completed, the operations of liquid film growth and low-temperature heat treatment can be repeated to obtain a thicker film. film layer; then the furnace tube temperature is raised to 800-1300 DEG C for high-temperature heat treatment, thereby obtaining an optical film with continuously adjustable optical constants; the present invention realizes continuously adjustable optical constants by changing the composition of the precursor liquid, the film deposition conditions and the heat treatment conditions , so that the film structure of the filter film can be greatly simplified, and the process time and cost can be shortened.
Description
技术领域technical field
本发明属于薄膜生长领域，具体涉及一种光学常数连续可调的薄膜生长方法。The invention belongs to the field of thin film growth, in particular to a thin film growth method with continuously adjustable optical constants.
背景技术Background technique
光学薄膜，例如反射膜、增透膜、滤光膜等是光学器件的重要组成部分，在激光器、光通信、医学、刑侦、生化等许多应用领域都有着及其重要的作用。光学薄膜的光学常数对于光学膜系结构设计有着重大影响，现有的光学薄膜通常是由多层不同光学常数的膜层叠加而成，通常有10-30层，有的更多达100层；并且不同光学常数的膜层采用不同的材料，同一种材料的光学常数也通常受到工艺方法、设备、工艺参数的影响，但是光学薄膜的光学常数通常是在一个较小范围波动。如果能实现光学常数在一个较大范围连续可调的光学薄膜生长，则可以大大简化膜系结构，缩短工艺时间；另一方面，常规光学薄膜的制备多采用溅射、电子束蒸发等PVD方法，如果采用化学溶液法制备高质量光学薄膜则可以大大降低成本。Optical films, such as reflective films, anti-reflection films, filter films, etc., are an important part of optical devices and play an important role in many application fields such as lasers, optical communications, medicine, criminal investigation, and biochemistry. The optical constant of the optical film has a significant impact on the structural design of the optical film system. The existing optical film is usually composed of multiple layers of films with different optical constants, usually 10-30 layers, and some more than 100 layers; And the film layers with different optical constants use different materials, and the optical constant of the same material is usually affected by the process method, equipment, and process parameters, but the optical constant of the optical film usually fluctuates in a small range. If it is possible to realize the growth of optical films with continuously adjustable optical constants in a large range, the film structure can be greatly simplified and the process time can be shortened; on the other hand, PVD methods such as sputtering and electron beam evaporation are mostly used for the preparation of conventional optical films. , if the chemical solution method is used to prepare high-quality optical films, the cost can be greatly reduced.
金属有机沉积(Metal Organic Deposition,简称MOD)法属于化学溶液沉积(CSD)法的一种，近三十年来以来一直作为铁电、超导薄膜的真空法制备替代方法而被广泛研究，可以制备各种氧化物、氮化物、硫化物电子薄膜。其生长温度较低，原材料利用率高，可以大面积均匀成膜，易于工业化，而且比溶胶凝胶法更简单。MOD法通常采用羧酸盐、乙酰丙酮盐等金属有机物作为金属源，其前驱液成分简单，相比溶胶凝胶法更稳定。MOD法的最大优势在于成本低廉，无需真空设备，而MOD法通常用于高质量电子薄膜的制备，在光学薄膜制备上用得较少。Metal Organic Deposition (MOD) method is a kind of chemical solution deposition (CSD) method. It has been widely studied as an alternative method for vacuum preparation of ferroelectric and superconducting thin films in the past three decades. Various oxide, nitride, sulfide electronic thin films. The growth temperature is low, the utilization rate of raw materials is high, the film can be formed uniformly in a large area, and it is easy to be industrialized and simpler than the sol-gel method. The MOD method usually uses metal organic compounds such as carboxylate and acetylacetonate as the metal source, and its precursor liquid has a simple composition and is more stable than the sol-gel method. The biggest advantage of the MOD method is that it is low in cost and does not require vacuum equipment. The MOD method is usually used for the preparation of high-quality electronic thin films, and is less used in the preparation of optical thin films.
发明内容SUMMARY OF THE INVENTION
为解决上述问题，本发明提出一种光学常数连续可调的薄膜生长方法，包括以下步骤：In order to solve the above-mentioned problems, the present invention proposes a method for growing a thin film with continuously adjustable optical constants, comprising the following steps:
S1.对基底进行表面处理，并根据所制作的光学薄膜类型制备相应的前驱液；S1. Surface treatment is performed on the substrate, and corresponding precursor liquid is prepared according to the type of optical film produced;
S2.根据制备的前驱液，在表面处理后的基底上吸附生长一层均匀的液膜；S2. According to the prepared precursor liquid, a layer of uniform liquid film is adsorbed and grown on the surface-treated substrate;
S3.将步骤S2得到的样品放置在300-400℃的炉管中低温热处理；S3. The sample obtained in step S2 is placed in a furnace tube at 300-400°C for low temperature heat treatment;
S4.低温热处理完成后判断光学薄膜厚度是否达到需求，若是则执行步骤S5，否则返回步骤S2；S4. After the low temperature heat treatment is completed, determine whether the thickness of the optical film meets the requirement, if so, execute step S5, otherwise return to step S2;
S5.低温热处理完成后，将炉管温度升至800-1300℃进行高温热处理；S5. After the low temperature heat treatment is completed, the temperature of the furnace tube is raised to 800-1300°C for high temperature heat treatment;
S6.高温热处理完成后，得到光学常数连续可调节的光学薄膜。S6. After the high temperature heat treatment is completed, an optical film with continuously adjustable optical constants is obtained.
进一步的，在步骤S1中制备的前驱液包括金属有机盐、增稠剂、溶剂，金属有机盐中金属原子的浓度范围是0.1-1.2摩尔，金属原子的浓度根据金属有机盐的溶解度进行调整，金属有机盐的溶解度越大，金属原子的浓度越大。Further, the precursor liquid prepared in step S1 includes a metal organic salt, a thickener, and a solvent, the concentration range of metal atoms in the metal organic salt is 0.1-1.2 moles, and the concentration of metal atoms is adjusted according to the solubility of the metal organic salt, The greater the solubility of the metal organic salt, the greater the concentration of metal atoms.
进一步的，基底采用K9玻璃、石英玻璃、硅片、功能器件等材料。Further, the substrate is made of K9 glass, quartz glass, silicon wafer, functional devices and other materials.
进一步的，在步骤S1中得到的基底上吸附一层液膜采用的方法包括旋涂法、喷涂法、提拉法、丝网印刷、刮刀涂布法等。Further, the methods used for adsorbing a layer of liquid film on the substrate obtained in step S1 include spin coating, spray coating, pulling, screen printing, blade coating, and the like.
进一步的，低温热处理时间为5-15分钟。Further, the low temperature heat treatment time is 5-15 minutes.
进一步的，高温热处理时间为45-90分钟。Further, the high temperature heat treatment time is 45-90 minutes.
进一步的，通过前驱液成分(金属有机盐、增稠剂、溶剂等)改变、薄膜沉积条件和热处理条件(温度区间、升温速率、通气种类和流速等)的改变，实现光学常数连续可调。Further, by changing the composition of the precursor liquid (metal organic salts, thickeners, solvents, etc.), film deposition conditions and heat treatment conditions (temperature interval, heating rate, ventilation type and flow rate, etc.), the optical constant is continuously adjustable.
本发明的有益效果：Beneficial effects of the present invention:
本发明采用了金属有机沉积(MOD)法，根据不同的薄膜需求制备相应的前驱液，从而生长光学常数连续可调的高质量光学薄膜，MOD法制备光学薄膜无需真空设备，成膜面积大，制备工艺比溶胶凝胶法简单方便。The invention adopts a metal organic deposition (MOD) method to prepare corresponding precursor liquids according to different film requirements, so as to grow high-quality optical films with continuously adjustable optical constants. The preparation process is simpler and more convenient than the sol-gel method.
本发明通过改变前驱液成分、薄膜沉积条件和热处理条件，实现光学常数连续可调，使得滤光膜的膜系结构可以大大简化，缩短工艺时间和成本。By changing the composition of the precursor liquid, the film deposition conditions and the heat treatment conditions, the invention realizes the continuous adjustment of the optical constant, so that the film structure of the filter film can be greatly simplified, and the process time and cost can be shortened.
附图说明Description of drawings
图1为本发明制备薄膜的流程图。Fig. 1 is the flow chart of the preparation of thin film of the present invention.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
一种光学常数连续可调的薄膜生长方法，如图1所示，包括：A thin film growth method with continuously tunable optical constants, as shown in Figure 1, includes:
S1.对基底进行表面处理，并根据所制作的光学薄膜类型制备相应的前驱液；S1. Perform surface treatment on the substrate, and prepare the corresponding precursor liquid according to the type of optical film produced;
S2.根据制备的前驱液，在表面处理后的基底上吸附生长一层均匀的液膜；S2. According to the prepared precursor liquid, a layer of uniform liquid film is adsorbed and grown on the surface-treated substrate;
S3.将步骤S2得到的样品放置在300-400℃的炉管中低温热处理；S3. The sample obtained in step S2 is placed in a furnace tube at 300-400°C for low temperature heat treatment;
S4.低温热处理完成后判断光学薄膜厚度是否达到需求，若是则执行步骤S5，否则返回步骤S2；S4. After the low temperature heat treatment is completed, determine whether the thickness of the optical film meets the requirement, if so, execute step S5, otherwise return to step S2;
S5.低温热处理完成后，将炉管温度升至800-1300℃进行高温热处理；S5. After the low temperature heat treatment is completed, the temperature of the furnace tube is raised to 800-1300°C for high temperature heat treatment;
S6.高温热处理完成后，得到指定厚度的高质量光学薄膜。S6. After the high-temperature heat treatment is completed, a high-quality optical film with a specified thickness is obtained.
优选地，采用的基底包括K9玻璃、石英玻璃、硅片或功能器件等；Preferably, the adopted substrate includes K9 glass, quartz glass, silicon wafer or functional device, etc.;
优选地，在步骤S1之前，制备前驱液，前驱液包括金属有机盐、增稠剂、溶剂，金属有机盐中金属原子的浓度范围是0.1-1.2摩尔，金属原子的浓度根据金属有机盐的溶解度进行调整。Preferably, before step S1, a precursor solution is prepared, the precursor solution includes a metal organic salt, a thickener and a solvent, the concentration range of metal atoms in the metal organic salt is 0.1-1.2 mol, and the concentration of metal atoms is based on the solubility of the metal organic salt. make adjustments.
具体地，金属有机盐中金属原子的种类包括钛、硅、钽、铌等；Specifically, the types of metal atoms in the metal organic salt include titanium, silicon, tantalum, niobium, etc.;
优选地，步骤S1中可以采用三次超声对基底进行表面处理，基底依次在丙酮、乙醇、去离子水中进行超声操作，三次超声操作的时间为5-10分钟。Preferably, in step S1, three ultrasonic waves can be used to perform surface treatment on the substrate, and the substrate is subjected to ultrasonic operations in acetone, ethanol, and deionized water in sequence, and the time of the three ultrasonic operations is 5-10 minutes.
在一实施例中，制备光学常数连续可调的高质量TiO2光学薄膜的过程包括：In one embodiment, the process of preparing a high-quality TiO 2 optical film with continuously tunable optical constants includes:
101、采用K9玻璃或石英玻璃作为基底，101. Use K9 glass or quartz glass as the substrate,
102、将基底放入丙酮中进行超声，超声完成后取出并放入乙醇中进行超声，乙醇超声完成后取出并放入去离子水中进行超声；102. Put the substrate into acetone for ultrasonication, take out after the ultrasonication is completed and put it into ethanol for ultrasonication, and after the ethanol ultrasonication is completed, take it out and put it into deionized water for ultrasonication;
103、在步骤102中得到的基底上吸附生长一层均匀的液膜；103. Adsorb and grow a uniform liquid film on the substrate obtained in step 102;
104、将步骤103得到的样品放置在300-400℃的炉管中低温热处理；104. The sample obtained in step 103 is placed in a furnace tube at 300-400°C for low temperature heat treatment;
105、低温热处理完成后，将炉管温度升至800-1300℃进行高温热处理；105. After the low temperature heat treatment is completed, the temperature of the furnace tube is raised to 800-1300°C for high temperature heat treatment;
106、高温热处理完成后，得到光学常数连续可调节的光学薄膜。106. After the high temperature heat treatment is completed, an optical film with continuously adjustable optical constants is obtained.
优选地，对基底进行超声处理之前，采用乙酰丙酮钛、聚乙烯醇缩丁醛和丙酸制备前驱液，乙酰丙酮钛中的钛金属原子浓度为0.1-1.2摩尔，聚乙烯醇缩丁醛是增稠剂。Preferably, before the substrate is subjected to ultrasonic treatment, a precursor solution is prepared by using titanium acetylacetonate, polyvinyl butyral and propionic acid, the concentration of titanium metal atoms in the titanium acetylacetonate is 0.1-1.2 mol, and the polyvinyl butyral is 0.1-1.2 moles. thickener.
优选地，通过调节前驱液的浓度、升温速率来改变氧化钛薄膜TiO2的孔隙率，当增稠剂的比例增大、升温速率越大，最终氧化钛薄膜TiO2的孔隙率越大，折射率越低，从而达到光学常数连续可调的高质量TiO2光学薄膜制备。Preferably, the porosity of the titanium oxide thin film TiO2 is changed by adjusting the concentration of the precursor solution and the heating rate. When the ratio of the thickener increases and the heating rate increases, the final porosity of the titanium oxide thin film TiO2 increases, and the refractive index increases. The lower the rate, the preparation of high-quality TiO 2 optical thin films with continuously tunable optical constants can be achieved.
优选地，基底依次在丙酮、乙醇、去离子水中进行超声操作，超声时间范围均为5-10分钟。Preferably, the substrate is subjected to ultrasonic operation in acetone, ethanol, and deionized water in sequence, and the ultrasonic time range is 5-10 minutes.
优选地，采用旋涂法、喷涂法、提拉法、丝网印刷、刮刀涂布法等方式在基底上吸附生长一层均匀的液膜。Preferably, a uniform liquid film is grown on the substrate by means of spin coating, spray coating, pulling method, screen printing, doctor blade coating and the like.
在另一实施例中，将吸附生长一层均匀液膜的基底放置在300-400℃的炉管中低温热处理5-15分钟，低温热处理过程中将溶剂挥发掉，并进行初步的有机分解。In another embodiment, the substrate on which a uniform liquid film is grown by adsorption is placed in a furnace tube at 300-400° C. for low-temperature heat treatment for 5-15 minutes. During the low-temperature heat treatment, the solvent is volatilized, and preliminary organic decomposition is performed.
优选地，在基底吸附生长液膜后进行低温热处理，低温热处理完成后再次在基底吸附生长液膜，通过液膜生长和低温热处理的循环操作对光学薄膜的厚度进行调节。Preferably, low temperature heat treatment is performed after the substrate absorbs and grows the liquid film, and after the low temperature heat treatment is completed, the liquid film is adsorbed and grown on the substrate again, and the thickness of the optical film is adjusted through the cyclic operation of the liquid film growth and the low temperature heat treatment.
优选地，低温热处理后，将炉管的温度提升至800-1300℃，对低温热处理后的物体进行高温热处理，高温热处理时间为45-90分钟。Preferably, after the low temperature heat treatment, the temperature of the furnace tube is raised to 800-1300° C., and the object after the low temperature heat treatment is subjected to a high temperature heat treatment, and the high temperature heat treatment time is 45-90 minutes.
在光学薄膜的制作过程中，通过前驱液成分的改变、薄膜沉积条件的改变，以及热处理条件的改变实现了光学常数的连续可调，在不同的工艺条件下调节膜层的光学常数，从而制备出所需的高质量的光学薄膜。In the production process of optical thin films, the continuous adjustment of optical constants is realized by changing the composition of the precursor liquid, the changes of film deposition conditions, and the changes of heat treatment conditions, and the optical constants of the films can be adjusted under different process conditions. produce the required high-quality optical films.
具体地，通过改变低温热处理的温度区间来调节所制备的光学薄膜的膜层的光学常数。Specifically, the optical constant of the film layer of the prepared optical film is adjusted by changing the temperature range of the low-temperature heat treatment.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, and substitutions can be made in these embodiments without departing from the principle and spirit of the invention and modifications, the scope of the present invention is defined by the appended claims and their equivalents.
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