CN116360031A - Hydrogel optical fiber with graded refractive index and preparation method thereof - Google Patents
Hydrogel optical fiber with graded refractive index and preparation method thereof Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/028—Optical fibres with cladding with or without a coating with core or cladding having graded refractive index
- G02B6/0281—Graded index region forming part of the central core segment, e.g. alpha profile, triangular, trapezoidal core
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C64/20—Apparatus for additive manufacturing; Details thereof or accessories therefor
- B29C64/205—Means for applying layers
- B29C64/209—Heads; Nozzles
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- G—PHYSICS
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
- G02B1/045—Light guides
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02033—Core or cladding made from organic material, e.g. polymeric material
- G02B6/02038—Core or cladding made from organic material, e.g. polymeric material with core or cladding having graded refractive index
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Abstract
本发明公开了一种折射率渐变型水凝胶光纤及其制备方法，以水凝胶材料为基质，其折射率分布具有从纤轴逐渐减小至包层的特征，该特征可以调控光模场半径、分布、数量以及导波方式等。利用数字光场投影3D打印方法制备本发明，通过数字化控制投影光场光强的渐变分布来调制水凝胶光纤的折射率渐变分布，并且能够保证水凝胶光纤的线性制备，实现水凝胶光纤的高效能导波传输。该水凝胶光纤横截面折射率渐变分布的特征可以使光场以一种“自聚焦”的形式始终向纤轴会聚，并且光学传输能力、抗色散能力以及抗环境干扰能力更强，同时由于水凝胶材料具有较好的生物相容性与柔韧度，在光治疗、脑机传输和细胞检测等领域具有巨大的应用潜力。
The invention discloses a graded refractive index hydrogel optical fiber and a preparation method thereof. The hydrogel material is used as a matrix, and its refractive index distribution has the characteristics of gradually decreasing from the fiber axis to the cladding, which can regulate the optical mode Field radius, distribution, quantity and wave guiding method, etc. The present invention is prepared by using the digital light field projection 3D printing method, and the gradient distribution of the refractive index of the hydrogel optical fiber is modulated by digitally controlling the gradient distribution of the light intensity of the projected light field, and the linear preparation of the hydrogel optical fiber can be guaranteed to realize the hydrogel High-efficiency guided wave transmission of optical fibers. The characteristics of the graded distribution of refractive index in the cross-section of the hydrogel optical fiber can make the light field always converge to the fiber axis in a "self-focusing" form, and the optical transmission ability, anti-dispersion ability and anti-environmental interference ability are stronger, and at the same time due to Hydrogel materials have good biocompatibility and flexibility, and have great application potential in the fields of phototherapy, brain-computer transmission and cell detection.
Description
技术领域technical field
本发明属于新型光波导器件领域，具体涉及一种折射率渐变型水凝胶光纤及其制备方法称。The invention belongs to the field of novel optical waveguide devices, and in particular relates to a graded-index hydrogel optical fiber and a preparation method thereof.
背景技术Background technique
水凝胶光纤是一种生物相容性好、延展性强和刺激响应灵敏的生物友好型光波导，在光治疗、脑机传输等领域都具有巨大的应用潜力。但是，由于水凝胶材料自身的吸收和散射特性，水凝胶光纤具有较高的光学传输损耗。并且作为植入式器件所使用时，水凝胶光纤也会面临接触高折射率组织液导致的光折射损耗以及活体运动导致的应力弯曲损耗，这些因素都会加剧水凝胶光纤的传输损耗。Hydrogel optical fiber is a kind of bio-friendly optical waveguide with good biocompatibility, strong ductility and sensitive stimulus response, which has great application potential in the fields of phototherapy, brain-computer transmission and so on. However, due to the absorption and scattering properties of the hydrogel material itself, the hydrogel optical fiber has a high optical transmission loss. And when used as an implantable device, the hydrogel optical fiber will also face the light refraction loss caused by contact with high refractive index tissue fluid and the stress bending loss caused by the movement of the living body. These factors will aggravate the transmission loss of the hydrogel optical fiber.
发明内容Contents of the invention
本发明提出了一种折射率渐变型水凝胶光纤及其制备方法，折射率渐变型水凝胶光纤具有优越的光学传输效率以及较低的介质接触损耗和应力弯曲损耗的特点，解决了水凝胶光纤传输损耗高的问题。其制备方法保证了水凝胶光纤良好的线性、均匀性以及连续性，解决了传统制备方法精度低以及成型方式复杂的问题。The invention proposes a graded-index hydrogel optical fiber and a preparation method thereof. The graded-index hydrogel optical fiber has the characteristics of superior optical transmission efficiency and lower dielectric contact loss and stress bending loss, and solves the problem of water The problem of high transmission loss of gel fiber. The preparation method ensures the good linearity, uniformity and continuity of the hydrogel optical fiber, and solves the problems of low precision and complicated molding methods of the traditional preparation method.
实现本发明的技术解决方案为：一种折射率渐变型水凝胶光纤，由水凝胶材料制备，所述水凝胶光纤中的折射率分布是从折射率为n1的纤轴逐渐减小至折射率为n2的包层，其折射率渐变形式n(R)由下式描述：The technical solution for realizing the present invention is: a graded-index hydrogel optical fiber, which is prepared from a hydrogel material, and the refractive index distribution in the hydrogel optical fiber gradually decreases from the fiber axis with a refractive index n 1 The graded form n(R) of the cladding with a refractive index as small as n 2 is described by:
式中，d为纤芯半径；R为距纤轴的径向长度；纤芯折射率与包层折射率的相对差Δ＝(n1-n2)/n2；k为渐变分布系数。In the formula, d is the radius of the core; R is the radial length from the fiber axis; the relative difference between the refractive index of the core and the cladding Δ=(n 1 -n 2 )/n 2 ; k is the gradient distribution coefficient.
一种折射率渐变型水凝胶光纤的制备方法，采用带有数字光场调制的投影3D打印方法制备折射率渐变型水凝胶光纤，步骤如下：A method for preparing a graded-index hydrogel optical fiber, using a projection 3D printing method with digital light field modulation to prepare a graded-index hydrogel optical fiber, the steps are as follows:
第一步：将石英光纤从底部穿入打印槽，打印槽自然形成密封结构，再向打印槽内倒入用于打印折射率渐变型水凝胶光纤的预制液，并静置消除液体晃动；调整石英光纤的位置使预制液液面与石英光纤的打印基底齐平，石英光纤的另一端固定在平移台上。Step 1: Insert the silica fiber into the printing tank from the bottom, the printing tank naturally forms a sealed structure, then pour the prefabricated liquid for printing the graded refractive index hydrogel optical fiber into the printing tank, and let it stand to eliminate the liquid shaking; Adjust the position of the silica fiber so that the liquid level of the preform is flush with the printing substrate of the silica fiber, and the other end of the silica fiber is fixed on the translation stage.
第二步：根据目标水凝胶光纤的折射率渐变分布类型，将对应的数字化光场光强渐变分布的投影图案投影到预制液与空气的交界面上，在气液交界处开始发生同比例光固化交联反应。Step 2: According to the refractive index gradient distribution type of the target hydrogel optical fiber, project the projection pattern of the corresponding digitized light field light intensity gradient distribution onto the interface between the prefabricated liquid and the air, and the same ratio begins to occur at the gas-liquid interface. Photocuring crosslinking reaction.
第三步：平移台匀速拉着石英光纤向下运动，保持同比例光固化交联反应在气液交界处持续发生，从而得到轴向连续且均匀的水凝胶光纤。Step 3: The translation stage pulls the silica fiber downward at a constant speed, and keeps the photocuring cross-linking reaction in the same proportion to continue to occur at the gas-liquid interface, thereby obtaining a continuous and uniform hydrogel fiber in the axial direction.
第四步：打印合适的长度后，停止打印，将制备出的水凝胶光纤从打印槽取出，浸泡在去离子水中，析出吸光剂以及其他未反应残液。Step 4: After printing a suitable length, stop printing, take out the prepared hydrogel optical fiber from the printing tank, soak it in deionized water, and precipitate light absorbing agent and other unreacted residual liquid.
本发明与现有技术相比，其显著优点在于：Compared with the prior art, the present invention has significant advantages in that:
(1)折射率渐变型水凝胶光纤具有水凝胶材料良好的生物相容性与柔韧度。折射率渐变型水凝胶光纤的光大部分都在靠近纤轴的范围传播，与阶跃折射率水凝胶光纤相比，其光学传输效率、抗色散能力以及抗干扰能力都更为优异。(1) Graded-index hydrogel optical fiber has good biocompatibility and flexibility of hydrogel materials. Most of the light in the graded-index hydrogel fiber propagates close to the fiber axis. Compared with the step-index hydrogel fiber, its optical transmission efficiency, anti-dispersion ability and anti-interference ability are all better.
(2)本发明提出的折射率渐变型水凝胶光纤的制备方法，折射率调制方便且具有高还原度高保真度的成型效果。(2) The preparation method of the graded-refractive-index hydrogel optical fiber proposed by the present invention is convenient for modulating the refractive index and has a high reduction degree and high-fidelity molding effect.
附图说明Description of drawings
图1为本发明折射率渐变型水凝胶光纤的制备方法流程图。Fig. 1 is a flow chart of the preparation method of the graded-index hydrogel optical fiber of the present invention.
图2为用于制备本发明折射率渐变型水凝胶光纤的数字光场投影3D打印装置结构示意图。Fig. 2 is a schematic structural diagram of a digital light field projection 3D printing device for preparing a graded-index hydrogel optical fiber of the present invention.
图3为折射率渐变型水凝胶光纤端面示意图。Fig. 3 is a schematic diagram of an end face of a graded-index hydrogel optical fiber.
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的一部分实施例，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 following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
下面将结合本设计实例对具体实施方式、以及本次发明的技术难点、发明点进行进一步介绍。The specific implementation, technical difficulties and invention points of this invention will be further introduced below in conjunction with this design example.
结合图1～图3，一种折射率渐变型水凝胶光纤，由水凝胶材料制备，所述水凝胶光纤中的折射率分布是从折射率为n1的纤轴逐渐减小至折射率为n2的包层，其折射率渐变形式n(R)由下式描述：In combination with Figures 1 to 3, a graded-index hydrogel optical fiber is prepared from hydrogel materials, and the refractive index distribution in the hydrogel optical fiber gradually decreases from the fiber axis with a refractive index of n 1 to For a cladding layer with a refractive index n 2 , its graded refractive index form n(R) is described by the following formula:
式中，d为纤芯半径；R为距纤轴的径向长度；纤芯折射率与包层折射率的相对差Δ＝(n1-n2)/n2；k为渐变分布系数。In the formula, d is the radius of the core; R is the radial length from the fiber axis; the relative difference between the refractive index of the core and the cladding Δ=(n 1 -n 2 )/n 2 ; k is the gradient distribution coefficient.
结合图2，一种折射率渐变型水凝胶光纤的制备方法，采用带有数字光场调制的投影3D打印方法进行制备，步骤如下：Referring to Figure 2, a method for preparing a graded-index hydrogel optical fiber is prepared by using a projection 3D printing method with digital light field modulation, and the steps are as follows:
第一步：将石英光纤从底部穿入打印槽，打印槽自然形成密封结构，再向打印槽内倒入用于打印折射率渐变型水凝胶光纤的预制液，并静置消除液体晃动。调整石英光纤的位置使预制液液面与石英光纤的打印基底齐平，石英光纤的另一端固定在平移台上。Step 1: Insert the silica fiber into the printing tank from the bottom, and the printing tank will naturally form a sealed structure, then pour the prefabricated liquid for printing the graded refractive index hydrogel optical fiber into the printing tank, and let it stand to eliminate the liquid sloshing. Adjust the position of the silica fiber so that the liquid level of the preform is flush with the printing substrate of the silica fiber, and the other end of the silica fiber is fixed on the translation stage.
第二步：根据目标水凝胶光纤的折射率渐变分布类型，将对应的数字化光场光强渐变分布的投影图案投影到预制液与空气的交界面上，在气液交界处开始发生同比例光固化交联反应。Step 2: According to the refractive index gradient distribution type of the target hydrogel optical fiber, project the projection pattern of the corresponding digitized light field light intensity gradient distribution onto the interface between the prefabricated liquid and the air, and the same ratio begins to occur at the gas-liquid interface. Photocuring crosslinking reaction.
设计数字化光场光强渐变分布的投影图案具体如下，在保持打印速度不变的情况下，投影多张尺寸大小相同、光场光强不同的图案，打印出不同光场光强下的单纤芯水凝胶光纤，并测量单纤芯水凝胶光纤的折射率，从中找到光场光强与制备出的水凝胶折射率的关系，同时找到此种水凝胶折射率的调制区间。依据此关系，生成光场光强随径向递减的投影图案，光场光强分布与折射率渐变型水凝胶光纤横截面的折射率分布相对应。Design the projection pattern of the gradient distribution of digital light field light intensity as follows. While keeping the printing speed constant, project multiple patterns with the same size and different light field light intensities, and print out single-fiber images with different light field light intensities. Core hydrogel optical fiber, and measure the refractive index of single-core hydrogel optical fiber, find the relationship between the light field intensity and the refractive index of the prepared hydrogel, and find the modulation interval of the refractive index of this hydrogel. According to this relationship, a projection pattern in which the light intensity of the light field decreases with the radial direction is generated, and the light intensity distribution of the light field corresponds to the refractive index distribution of the cross-section of the graded-index hydrogel optical fiber.
第三步：平移台匀速拉着石英光纤向下运动，保持同比例光固化交联反应在气液交界处持续发生，从而得到轴向连续且均匀的水凝胶光纤。Step 3: The translation stage pulls the silica fiber downward at a constant speed, and keeps the photocuring cross-linking reaction in the same proportion to continue to occur at the gas-liquid interface, thereby obtaining a continuous and uniform hydrogel fiber in the axial direction.
第四步：打印合适的长度后，停止打印，将制备出的水凝胶光纤从打印槽取出，浸泡在去离子水中，析出吸光剂以及其他未反应残液。Step 4: After printing a suitable length, stop printing, take out the prepared hydrogel optical fiber from the printing tank, soak it in deionized water, and precipitate light absorbing agent and other unreacted residual liquid.
所述用于数字光场投影3D打印方法的预制液，其成分为：The prefabricated liquid for the digital light field projection 3D printing method has the following components:
1)20％～40％(w/V)的丙烯酰胺，为制备水凝胶光纤的单体，用于构建三维网状结构的骨架。1) 20%-40% (w/V) acrylamide, which is a monomer for preparing hydrogel optical fibers, and is used to construct the skeleton of a three-dimensional network structure.
2)5％～10％(w/V)的聚乙二醇二丙烯酸酯(700Da)，是制备水凝胶的一种高分子化合物，也用于构建三维网状结构的骨架。2) 5%-10% (w/V) polyethylene glycol diacrylate (700Da), which is a polymer compound for preparing hydrogel, and is also used to construct the skeleton of a three-dimensional network structure.
3)0.01％～0.03％(w/V)的苯基-2,4,6-三甲基苯甲酰基亚磷酸锂，为光引发剂，可在紫外光的照射下产生自由基、阳离子等，从而引发单体聚合生成线性大分子。3) 0.01%～0.03% (w/V) phenyl-2,4,6-trimethylbenzoyllithium phosphite, as a photoinitiator, can generate free radicals, cations, etc. under the irradiation of ultraviolet light , thus initiating the polymerization of monomers to form linear macromolecules.
4)1％～2％(w/V)的N,N’-亚甲基双丙烯酰胺，为交联剂，可在线性大分子之间产生化学键，使之相互连在一起，形成网状结构。4) 1% to 2% (w/V) N,N'-methylenebisacrylamide, as a cross-linking agent, can generate chemical bonds between linear macromolecules, so that they are connected to each other to form a network structure.
5)0.01％～0.05％(w/V)的柠檬黄，为光吸收剂，限制反应面以外的光交联反应，从而提高数字光场投影3D打印方法的轴向打印精度及分辨率。5) 0.01%-0.05% (w/V) tartrazine, which is a light absorber, limits the photocrosslinking reaction outside the reaction surface, thereby improving the axial printing accuracy and resolution of the digital light field projection 3D printing method.
6)47.92％～73.98％(w/V)的去离子水，用于上述试剂的溶解，使总体积为100％。6) 47.92%-73.98% (w/v) deionized water is used for dissolving the above reagents, making the total volume 100%.
预制液的实施例：Examples of preforms:
所述用于打印折射率渐变型水凝胶光纤的预制液，如利用体积百分比分别为30％(w/V)的丙烯酰胺、10％(w/V)的聚乙二醇二丙烯酸酯(700Da)、0.02％(w/V)的苯基-2,4,6-三甲基苯甲酰基亚磷酸锂、1.5％(w/V)的N,N’-亚甲基双丙烯酰胺、0.03％(w/V)的柠檬黄和58.45％(w/V)的去离子水。此配置出的预制液流动性较好，可以满足打印过程中的回流要求，同时将丙烯酰胺与聚乙二醇二丙烯酸酯复合，与只添加丙烯酰胺的预制液相比，增加了水凝胶折射率的调制范围，有利于渐变折射率水凝胶光纤的制备。The prefabricated solution for printing the graded-index hydrogel optical fiber, such as the use of acrylamide with a volume percentage of 30% (w/V) and polyethylene glycol diacrylate ( 700Da), 0.02% (w/V) of phenyl-2,4,6-trimethylbenzoyl lithium phosphite, 1.5% (w/V) of N,N'-methylenebisacrylamide, 0.03% (w/V) tartrazine and 58.45% (w/V) deionized water. The fluidity of the prefabricated liquid prepared by this configuration is better, which can meet the reflow requirements in the printing process. At the same time, acrylamide and polyethylene glycol diacrylate are compounded, and compared with the prefabricated liquid only added with acrylamide, the hydrogel The modulation range of the refractive index is beneficial to the preparation of the graded-index hydrogel optical fiber.
综上所述，本发明以水凝胶材料为基质，其折射率分布具有从纤轴逐渐减小至包层的特征，该特征可以调控光模场半径、分布、数量以及导波方式等。利用数字光场投影3D打印方法制备本发明，通过数字化控制投影光场光强的渐变分布来调制水凝胶光纤的折射率渐变分布，并且能够保证水凝胶光纤的线性制备，实现水凝胶光纤的高效能导波传输。该水凝胶光纤横截面折射率渐变分布的特征可以使光场以一种“自聚焦”的形式始终向纤轴会聚，并且光学传输能力、抗色散能力以及抗环境干扰能力更强，同时由于水凝胶材料具有较好的生物相容性与柔韧度，在光治疗、脑机传输和细胞检测等领域具有巨大的应用潜力。In summary, the present invention uses a hydrogel material as a matrix, and its refractive index distribution has the characteristics of gradually decreasing from the fiber axis to the cladding layer. This feature can regulate the radius, distribution, quantity, and waveguide mode of the optical mode field. The present invention is prepared by using the digital light field projection 3D printing method, and the gradient distribution of the refractive index of the hydrogel optical fiber is modulated by digitally controlling the gradient distribution of the light intensity of the projected light field, and the linear preparation of the hydrogel optical fiber can be guaranteed to realize the hydrogel High-efficiency guided wave transmission of optical fibers. The characteristics of the graded distribution of refractive index in the cross-section of the hydrogel optical fiber can make the light field always converge to the fiber axis in a "self-focusing" form, and the optical transmission ability, anti-dispersion ability and anti-environmental interference ability are stronger, and at the same time due to Hydrogel materials have good biocompatibility and flexibility, and have great application potential in the fields of phototherapy, brain-computer transmission and cell detection.
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| CN118181740B (en) * | 2024-04-09 | 2024-08-20 | 北京师范大学珠海校区 | Method for 3D printing of multi-material segmented side-emitting hydrogel optical fiber |
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