CN106980228B - Method for preparing durable micro-nano structure on curved glass - Google Patents
Method for preparing durable micro-nano structure on curved glass Download PDFInfo
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- CN106980228B CN106980228B CN201710276220.0A CN201710276220A CN106980228B CN 106980228 B CN106980228 B CN 106980228B CN 201710276220 A CN201710276220 A CN 201710276220A CN 106980228 B CN106980228 B CN 106980228B
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/002—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor using materials containing microcapsules; Preparing or processing such materials, e.g. by pressure; Devices or apparatus specially designed therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for preparing a durable micro-nano structure on curved glass, relates to the field of micro-machining, and solves the technical problem that the micro-nano structure is difficult to prepare on the curved glass, and the micro-nano structure is not required to be transferred to a substrate through an ion beam etching technology. The method comprises the following steps: firstly, preparing a PDMS soft template with a micro-nano structure, adhering one surface without the structure to a concave glass substrate, and spin-coating a sol-gel material; then placing the convex glass substrate on the PDMS soft template after gluing, and exposing the whole of the convex glass substrate and the PDMS soft template under ultraviolet illumination; then the two are integrally placed on a hot plate and heated for 1 hour at the temperature of 100 ℃ to solidify the sol-gel material; and finally, taking down the glass substrate from the heating plate and cooling the glass substrate to room temperature, and separating the convex glass substrate from the PDMS soft template to prepare the durable micro-nano structure on the convex glass substrate. The invention is suitable for the fields of micro-machining, micro-nano manufacturing and the like.
Description
Technical Field
The invention relates to the field of micro-nano processing, in particular to a method for preparing a durable micro-nano structure on curved glass.
Background
The most effective method in the existing method for carrying out micro-nano processing on the curved surface is a laser direct writing technology. The method utilizes laser focal spots to scan on a curved surface, so that photoresist coated on the curved surface is exposed to obtain a required pattern. The method has the advantages that any pattern can be obtained, the defects that the processing process is extremely slow and is not suitable for the requirement of large-caliber large-batch processing, the prepared structure does not have durability, and the structure needs to be transferred to a substrate through other subsequent processing means such as an ion beam etching technology. Other methods include laser holographic interferometry, decal transfer methods, and the like, each of which has advantages and disadvantages, and is limited in number.
The soft lithography technology is a generic name of a series of methods for performing microfabrication using an elastic template (typically, PDMS) with micro-nano patterns as a stamp. The elastic template used by the technology has good flexibility, so that the method can be applied to the preparation of micro-nano structures on the curved substrate. Meanwhile, the soft lithography technology is very simple to operate and is easier to develop towards the direction of industrialization in the future.
So far, no public report is found on a method for preparing a micro-nano structure on curved glass by utilizing a soft lithography technology and a synthesized photosensitive sol-gel material.
Disclosure of Invention
In order to solve the technical problem that the durable micro-nano structure is difficult to prepare on the curved glass substrate in the field of micro-machining, the invention provides a method for simply preparing the durable micro-nano structure on the curved glass substrate by using a soft lithography technology and a novel photosensitive sol-gel mixed glass material.
The technical scheme of the invention is as follows:
the method for preparing the durable micro-nano structure on the curved glass is characterized by comprising the following steps of:
s1: synthesizing a novel photosensitive sol-gel mixed glass material, wherein the synthesizing steps are as follows:
s11: mixing 3- (trimethoxysilyl) propyl methacrylate (3-trimethoxysilyl propyl methacrylate) with isopropanol and water at a molar ratio of 0.04:0.048:0.053, and hydrolyzing to form a first solution;
s12: preparing a second solution from a metal organic substance titanium tetraisopropoxide and acetylacetone in a nitrogen environment according to a molar ratio of 1: 4;
s13: standing for 30 minutes, mixing the prepared two solutions according to a specific ratio, and preparing the sol-gel mixed glass material with different refractive indexes by adjusting the proportion of the second solution in the mixed solution, wherein the refractive index range is 1.46-2.95, so that the refractive index of the sol-gel mixed glass material is the same as that of the used curved glass;
s14: the mixed solution is placed on a magnetic stirrer to be stirred for 24 hours and then can be used, in order to ensure that SiO is generated2/TiO2The mixed sol-gel material has photosensitive property, and the added photoinitiator comprises 3 percent (by weight ratio) bis (2,4, 6-trimethylphenylketone) phosphine oxide and 1 percent (by weight ratio) 1-hydroxyethylphenylketone;
s15: stirring uniformly, standing for 30 minutes, and filtering and distilling to obtain a photosensitive sol-gel material with certain viscosity;
s2: the preparation of the durable micro-nano structure on the curved glass comprises the following steps:
s21: copying a PDMS soft template by using a master mask with a micro-nano structure, adhering the surface without the structure of the prepared PDMS soft template to a concave curved glass substrate, and rotationally coating the synthesized photosensitive sol-gel glass material;
s22: placing the convex curved glass substrate on a PDMS soft template of the concave curved glass substrate, and exposing the two integrally under ultraviolet irradiation;
s23: putting the two on a hot plate, and heating for 1 hour at 100 ℃ to completely cure the sol-gel material;
s24: and taking down the whole device from the hot plate, cooling to room temperature, separating the convex curved glass substrate from the PDMS soft template, and preparing the durable micro-nano structure on the convex curved glass substrate.
The invention has the beneficial effects that:
the invention solves the technical problem that the micro-nano structure is difficult to prepare on a curved glass substrate, and most importantly, the micro-nano structure prepared by the method does not need to be transferred to the substrate by an ion beam etching technology after being cured, and the refractive index of the cured sol-gel mixed glass material is continuously adjustable (1.46-2.95), so that the material has the property similar to glass, can be well adhered with the glass substrate, and has extremely high stability. Therefore, the method can meet the requirement of durability application for preparing the micro-nano structure on the curved substrate, and is extremely low in cost and simple and feasible in operation.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below.
FIG. 1 is a process flow diagram for preparing a durable micro-nano structure on curved glass
In the figure: 1. the photosensitive coating comprises a photoresist, 2, a plane glass substrate, 3, a PDMS soft template, 4, a concave curved surface glass substrate, 5, a novel photosensitive sol-gel material and 6, a convex curved surface glass substrate.
Detailed Description
The specific implementation mode is as follows: as shown in fig. 1, a method for preparing a durable micro-nano structure on curved glass comprises the following steps:
s1: synthesizing a novel photosensitive sol-gel mixed glass material, wherein the synthesizing steps are as follows:
s11: mixing 3- (trimethoxysilyl) propyl methacrylate (3-trimethoxysilyl propyl methacrylate) with isopropanol and water at a molar ratio of 0.04:0.048:0.053, and hydrolyzing to form a first solution;
s12: preparing a second solution from a metal organic substance titanium tetraisopropoxide and acetylacetone in a nitrogen environment according to a molar ratio of 1: 4;
s13: standing for 30 minutes, mixing the prepared two solutions according to a specific ratio, and preparing the sol-gel mixed glass material with different refractive indexes by adjusting the proportion of the second solution in the mixed solution, wherein the refractive index range is 1.46-2.95, so that the refractive index of the sol-gel mixed glass material is the same as that of the used curved glass;
s14: the mixed solution is placed on a magnetic stirrer to be stirred for 24 hours and then can be used, in order to ensure that SiO is generated2/TiO2The mixed sol-gel material has photosensitive property, and the added photoinitiator comprises 3 percent (by weight ratio) bis (2,4, 6-trimethylphenylketone) phosphine oxide and 1 percent (by weight ratio) 1-hydroxyethylphenylketone;
s15: stirring uniformly, standing for 30 minutes, and filtering and distilling to obtain a photosensitive sol-gel material with certain viscosity;
s2: the preparation of the durable micro-nano structure on the curved glass comprises the following steps:
s21: copying a PDMS soft template by using a master mask with a micro-nano structure, adhering the surface without the structure of the prepared PDMS soft template to a concave curved glass substrate, and rotationally coating the synthesized photosensitive sol-gel glass material;
s22: placing the convex curved glass substrate on a PDMS soft template of the concave curved glass substrate, and exposing the two integrally under ultraviolet irradiation;
s23: putting the two on a hot plate, and heating for 1 hour at 100 ℃ to completely cure the sol-gel material;
s24: and taking down the whole device from the hot plate, cooling to room temperature, separating the convex curved glass substrate from the PDMS soft template, and preparing the durable micro-nano structure on the convex curved glass substrate.
The molar ratio of the materials in the first solution used in the novel photosensitive sol-gel mixed glass material described in step S11 in this embodiment can be, but is not limited to, 0.04:0.048: 0.053.
In this embodiment, the novel photosensitive sol-gel hybrid glass material described in step S14 has a property of being firmly bonded after being irradiated with specific light; the photoinitiator added during the preparation process includes but is not limited to 3% (by weight) bis (2,4, 6-trimethybenzol) phosphine oxide and 1% (by weight) 1-hydroxycyclohexylphenylketone.
In this embodiment, the flexible template used in the soft lithography technique described in step S21 is polydimethylsilane, which is abbreviated as: PDMS, wherein the PDMS is formed by mixing monomer molecules and a polymerization agent; the volume ratio of the monomer molecules to the polymerizer is 10: 1.
The uv exposure energy in step S22 in this embodiment can be adjusted according to actual conditions.
In step S23 in the present embodiment, both are placed on a hot plate and heated at 100 ℃ for 1 hour, and the heating temperature and time can be adjusted according to the actual situation.
The foregoing is only an embodiment of the present invention, and it should be noted that, for those skilled in the art, without departing from the concept of the present invention, several modifications may be made, such as improving the preparation method of the novel photosensitive sol-gel material or improving the details of the specific implementation of the micro-nano structure on the curved substrate in the present invention, and these modifications should be considered to be within the scope of the present invention.
Claims (1)
1. A method for preparing a durable micro-nano structure on curved glass is characterized by comprising the following steps:
s1: synthesis of SiO2/TiO2The photosensitive sol-gel glass material comprises the following synthetic steps:
s11: mixing 3- (trimethoxysilyl) propyl methacrylate, isopropanol and water according to a molar ratio of 0.04:0.048:0.053, and hydrolyzing to form a first solution;
s12: preparing a second solution from a metal organic substance titanium tetraisopropoxide and acetylacetone in a nitrogen environment according to a molar ratio of 1: 4;
s13: standing for 30 minutes, mixing the prepared first solution and the second solution, and preparing SiO with different refractive indexes by adjusting the proportion of the second solution in the mixed solution2/TiO2The sol-gel glass material has a refractive index ranging from 1.46 to 2.95, so that the refractive index of the sol-gel glass material is the same as that of the used curved glass;
s14: placing the mixed solution on a magnetic stirrer to stir for 24 hours, and adding a photoinitiator to enable SiO to be generated2/TiO2The sol-gel glass material has photosensitive characteristics, and the photoinitiator comprises 3 weight percent of bis (2,4,6-trimethylbenzoyl) phosphine oxide and 1 weight percent of 1-hydroxycyclohexyl benzophenone;
s15: stirring evenly, standing for 30 minutes, filtering and distilling to obtain SiO2/TiO2A photosensitive sol-gel glass material;
s2: the preparation of the durable micro-nano structure on the curved glass comprises the following steps:
s21: copying a PDMS soft template by using a master plate with a micro-nano structure, adhering the surface without the structure on the prepared PDMS soft template to the concave curved surface glass substrate, and rotationally coating the SiO obtained in the step S12/TiO2A photosensitive sol-gel glass material;
s22: placing the convex curved glass substrate on a PDMS soft template of the concave curved glass substrate, and exposing the two integrally under ultraviolet irradiation;
s23: the two are put on a hot plate and heated for 1 hour at 100 ℃,make SiO2/TiO2The photosensitive sol-gel glass material is completely cured;
s24: and taking the two whole bodies off a hot plate, cooling to room temperature, separating the convex curved glass substrate from the PDMS soft template, and preparing the durable micro-nano structure on the convex curved glass substrate.
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| CN108628092A (en) * | 2018-05-16 | 2018-10-09 | 深圳市华星光电技术有限公司 | The production method for transferring the production method and transfer method, color membrane substrates of template |
| CN110760896A (en) * | 2018-07-26 | 2020-02-07 | 苏州苏大维格科技集团股份有限公司 | Crease-resistant electroforming process for working plate |
| CN109990977B (en) * | 2019-03-29 | 2020-11-24 | 中国科学院近代物理研究所 | Refractive index matching fluid |
| CN112782795B (en) * | 2021-01-29 | 2022-06-07 | 鲁东大学 | Method for preparing submicron grating with half period |
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| CN1269769A (en) * | 1997-07-29 | 2000-10-11 | 物理光学公司 | Monolithic glass light shaping diffuser and method for its producing |
| CN1785683A (en) * | 2004-12-10 | 2006-06-14 | 中国科学院兰州化学物理研究所 | Preparation method of patterned titanium dioxide micro structure |
| CN101339364A (en) * | 2008-08-13 | 2009-01-07 | 中国科学院上海光学精密机械研究所 | Method for manufacturing microlens array by soft mode impressing |
| CN101587297A (en) * | 2009-07-07 | 2009-11-25 | 西安交通大学 | Preparation for titanium dioxide based organic-inorganic composite film and method for preparing micro-optic device by adopting film |
| CN103576450A (en) * | 2013-11-07 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Method for preparing nanoscale thickness thin film and structure on curved surface substrate |
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| US8445889B2 (en) * | 2008-02-22 | 2013-05-21 | Nanyang Technological University | Method of patterning of nanostructures |
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| CN1269769A (en) * | 1997-07-29 | 2000-10-11 | 物理光学公司 | Monolithic glass light shaping diffuser and method for its producing |
| CN1785683A (en) * | 2004-12-10 | 2006-06-14 | 中国科学院兰州化学物理研究所 | Preparation method of patterned titanium dioxide micro structure |
| CN101339364A (en) * | 2008-08-13 | 2009-01-07 | 中国科学院上海光学精密机械研究所 | Method for manufacturing microlens array by soft mode impressing |
| CN101587297A (en) * | 2009-07-07 | 2009-11-25 | 西安交通大学 | Preparation for titanium dioxide based organic-inorganic composite film and method for preparing micro-optic device by adopting film |
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Effective date of registration: 20210120 Address after: 1708, 17th floor, building 2, yard 26, Chengtong street, Shijingshan District, Beijing Patentee after: Beijing Linjiang Technology Co.,Ltd. Address before: Ludong University, 184 Shixue Road, Zhifu District, Yantai City, Shandong Province Patentee before: LUDONG University |