CN106980228A - A kind of method that durability micro-nano structure is prepared on bend glass - Google Patents
A kind of method that durability micro-nano structure is prepared on bend glass Download PDFInfo
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- CN106980228A CN106980228A CN201710276220.0A CN201710276220A CN106980228A CN 106980228 A CN106980228 A CN 106980228A CN 201710276220 A CN201710276220 A CN 201710276220A CN 106980228 A CN106980228 A CN 106980228A
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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 kind of method that durability micro-nano structure is prepared on bend glass, it is related to micro processing field, it is solved prepares the difficult technical problem of micro-nano structure on bend glass, and no longer needs that micro-nano structure is delivered in substrate by ion beam etching technology.The present invention method be：The PDMS soft templates with micro-nano structure are first made, its structureless one side is attached in spill substrate of glass and spin coating sol gel film；Convex substrate of glass is placed in the PDMS soft templates after gluing again, both are overall to expose under ultraviolet lighting；Then both are integrally placed on hot plate at 100 DEG C and heated 1 hour, solidify sol gel film；Finally removed from heating plate and be cooled to room temperature, separation convex substrate of glass and PDMS soft templates have just prepared the micro-nano structure of durability in convex substrate of glass.The present invention is applied to microfabrication, field of micro-Na manufacture etc..
Description
Technical field
The present invention relates to micro-nano technology field, and in particular to the method that durability micro-nano structure is prepared on bend glass.
Background technology
It is most useful that laser writing technology in the existing method that micro-nano technology is carried out on curved surface.This method, which is utilized, to swash
Light focus spot is scanned on curved surface so that the photoresist being coated on curved surface is exposed to obtain required figure.Its
Advantage is can to obtain arbitrary graphic, the need for shortcoming is that process is extremely slowly not suitable for heavy caliber high-volume processing,
And prepared structure and without durability, need other following process means by ion beam etching technology etc. to transmit structure
Onto substrate.Other methods include laser-holographic interferometry, decalcomania transfer etc., and these methods respectively have advantage and disadvantage, are limited quite
It is many.
Soft lithography is a series of Elastic forming boards (typical material is PDMS) used with micro-nano pattern as seal
Carry out the general name of the method for microfabrication.Because Elastic forming board used in the technology has good flexibility, therefore it can apply
In the preparation of micro-nano structure on curved substrate.Soft lithography operates very simply simultaneously, is easier in the future to industrialization
Direction is developed.
Up to the present, micro-nano is prepared on bend glass using the photosensitive sol gel film of soft lithography and synthesis
The method of structure, there is not yet open report.
The content of the invention
Asked to capture in micro processing field the technology for being difficult to prepare durability micro-nano structure in bend glass substrate
Topic, bend glass is realized the invention provides one kind using soft lithography and new photosensitive collosol and gel hybrid glass material
The method that durability micro-nano structure is simply prepared in substrate.
The technical scheme is that：
A kind of method that durability micro-nano structure is prepared on bend glass, comprises the following steps：
（1）The photosensitive collosol and gel hybrid glass material of synthesizing new, synthesis step is as follows：By methacrylic acid -3- (trimethoxies
Silicon substrate) propyl ester (3-trimethoxysilyl propyl methacrylate) and isopropyl alcohol and water press 0.04:0.048:
0.053 mixed in molar ratio, the oxide sol for making it hydrolyze to form silicon；Metallorganic tetra isopropyl titanium and acetylacetone,2,4-pentanedione are existed
According to 1 in nitrogen environment:Titanyl compound colloidal sol is made in 4 mol ratio, and after standing 30 minutes, configured two kinds of solution are pressed
According to special ratios（Make and substrate of glass refractive index identical sol gel film）Mixed, by adjusting mixed solution
Ratio shared by middle titanium oxide sol can make the collosol and gel hybrid glass material of different refractivity（Ranges of indices of refraction is big
About between 1.46-2.95）, it is allowed to identical with the refractive index of bend glass used；Solution after mixing is placed in magnetic stirring apparatus
Upper stirring, can be used after 24 hours, in order that SiO2/TiO2Mixed sols-gel rubber material has light sensitive characteristic, adds light and draws
Sending out agent includes 3%（By weight）Bis (2,4,6-trimethylbenzoyl) phosphine oxide and 1%（By weight）
1-hydroxycyclohexyl phenylketone, being stood after stirring can be had for 30 minutes after filtration evaporates
The photosensitive sol gel film of certain viscosity；
（2）The preparation of durability micro-nano structure on bend glass, particularly, the first step use the mother matrix with micro-nano structure
（Plane curved surface, can make by oneself and also can purchase）PDMS soft templates are replicated, and by structureless one in the PDMS soft templates being made
Face is attached to the photosensitive sol-gel glasses material that in concave curvatures substrate of glass and rotary coating is synthesized；Second step, by convex
Bend glass substrate is placed on the PDMS soft templates of concave curvatures substrate of glass, and will both overall progress under ultraviolet lighting
Exposure, due to the addition of light trigger in sol gel film, so collosol and gel can be produced admittedly after ultraviolet light
Connection reaction；3rd step, both are integrally placed on hot plate and heated 1 hour at 100 DEG C, sol gel film is fully cured；
4th step, whole device is removed from hot plate and room temperature is cooled to, then by convex surface substrate of glass and PDMS soft templates
Separation, has now just prepared the micro-nano structure of durability in convex surface substrate of glass.
Beneficial effects of the present invention：The present invention, which is solved, to be prepared the difficult technology of micro-nano structure in bend glass substrate and asks
Topic, it is most important that will no longer be required to tie by ion beam etching technology after the micro-nano structure solidification prepared by such a method
Structure is delivered in substrate, and collosol and gel hybrid glass material itself the refractive index continuously adjustabe after solidification（1.46~2.95）,
With the property similar to glass, it can adhere to each other with substrate of glass well, with high stability.Therefore originally
Invention disclosure satisfy that the durability application requirement that micro-nano structure is prepared on curved substrate, and cost needed for the invention is extremely low and operates
Simple possible.
Brief description of the drawings
Fig. 1 prepares durability micro-nano structure process chart on bend glass
In figure：1st, photoresist, 2, flat glass substrate, 3, PDMS soft templates, 4, concave curvatures substrate of glass, 5, new photosensitive molten
Sol-gel materials, 6, convex surface substrate of glass.
Embodiment
Embodiment：A kind of method that durability micro-nano structure is prepared on bend glass, is completed by following steps：
Step 1: the photosensitive collosol and gel hybrid glass material of synthesizing new.By methacrylic acid -3- (trimethoxy silicon substrate) propyl ester
(3-trimethoxysilyl propyl methacrylate) presses 0.04 with isopropyl alcohol and water:0.048:0.053 mol ratio is mixed
Close, the oxide sol for making it hydrolyze to form silicon.In order that SiO2/TiO2Mixed sols-gel rubber material has light sensitive characteristic, plus
Enter light trigger.During can make different refractivity by adjusting the ratio in mixed solution shared by titanium oxide sol
Collosol and gel hybrid glass material（Ranges of indices of refraction is about between 1.46-2.95）, it is allowed to the refraction with bend glass used
Rate is identical.
Step 2: using soft lithography and the new photosensitive sol-gel glasses material of synthesis in bend glass substrate
Prepare durability micro-nano structure.The first step, replicates PDMS soft templates, and will be made using the mother matrix with micro-nano structure
Structureless one side is attached to the photosensitive collosol and gel that in concave curvatures substrate of glass and rotary coating is synthesized in PDMS soft templates
Glass material；Second step, convex surface substrate of glass is placed on the PDMS soft templates of concave curvatures substrate of glass, and by two
Person is integrally exposed under ultraviolet lighting.3rd step, both are integrally placed on hot plate and heated 1 hour at 100 DEG C, is made molten
Sol-gel materials are fully cured.4th step, whole device is removed from hot plate and room temperature is cooled to, then by convex surface glass
Glass substrate is separated with PDMS soft templates, and the micro-nano structure of durability has now just been prepared in convex surface substrate of glass.
The oxide of the silicon used in new photosensitive collosol and gel hybrid glass material in present embodiment described in step one
The configuration mol ratio of the various materials of colloidal sol can use but be not limited solely to 0.04:0.048:0.053.
New photosensitive collosol and gel hybrid glass material in present embodiment described in step one has to be irradiated by specific light
The property connected firmly afterwards；The light trigger added during preparation includes but are not limited to 3%（By weight）bis(2,4,
6-trimethylbenzoyl) phosphine oxide and 1%（By weight）1-hydroxycyclohexyl
phenylketone。
The material of the Flexible formwork assembly used in soft lithography in present embodiment described in step 2 is polydimethylsiloxane,
Referred to as：PDMS, the PDMS is mixed by monomer molecule and polymerizer；The volume ratio of the monomer molecule and polymerizer is
10 ∶ 1。
Ultraviolet photoetching energy in present embodiment described in step 2 can be adjusted according to actual conditions.
Both are integrally placed on hot plate the heating 1 at 100 DEG C small by the 3rd step in present embodiment described in step 2
When, its acid extraction can be adjusted according to actual conditions.
Described above is only embodiments of the present invention, it is noted that for those skilled in the art, do not taken off
On the premise of from present inventive concept, some improvement can also be made, for example, improve the preparation side of new photosensitive sol gel film
Method improves the specific implementation details that micro-nano structure is prepared in mean camber substrate of the present invention, and these improvement also should be regarded as the present invention
Protection domain in.
Claims (7)
1. a kind of method that durability micro-nano structure is prepared on bend glass, it is characterised in that comprise the following steps：
（1）The photosensitive collosol and gel hybrid glass material of synthesizing new, synthesis step is as follows：By methacrylic acid -3- (trimethoxies
Silicon substrate) propyl ester (3-trimethoxysilyl propyl methacrylate) and isopropyl alcohol and water press 0.04:0.048:
0.053 mixed in molar ratio, the oxide sol for making it hydrolyze to form silicon；Metallorganic tetra isopropyl titanium and acetylacetone,2,4-pentanedione are existed
According to 1 in nitrogen environment:Titanyl compound colloidal sol is made in 4 mol ratio, and after standing 30 minutes, configured two kinds of solution are pressed
According to special ratios（Make and substrate of glass refractive index identical sol gel film）Mixed, by adjusting mixed solution
Ratio shared by middle titanium oxide sol can make the collosol and gel hybrid glass material of different refractivity（Ranges of indices of refraction is big
About between 1.46-2.95）, it is allowed to identical with the refractive index of bend glass used；Solution after mixing is placed in magnetic stirring apparatus
Upper stirring, can be used after 24 hours, in order that SiO2/TiO2Mixed sols-gel rubber material has light sensitive characteristic, adds light and draws
Sending out agent includes 3%（By weight）Bis (2,4,6-trimethylbenzoyl) phosphine oxide and 1%（By weight）
1-hydroxycyclohexyl phenylketone, being stood after stirring can be had for 30 minutes after filtration evaporates
The photosensitive sol gel film of certain viscosity；
（2）The preparation of durability micro-nano structure on bend glass, particularly, the first step use the mother matrix with micro-nano structure
（Plane curved surface, can make by oneself and also can purchase）PDMS soft templates are replicated, and by structureless one in the PDMS soft templates being made
Face is attached to the photosensitive sol-gel glasses material that in concave curvatures substrate of glass and rotary coating is synthesized；Second step, by convex
Bend glass substrate is placed on the PDMS soft templates of concave curvatures substrate of glass, and will both overall progress under ultraviolet lighting
Exposure, due to the addition of light trigger in sol gel film, so collosol and gel can be produced admittedly after ultraviolet light
Connection reaction；3rd step, both are integrally placed on hot plate and heated 1 hour at 100 DEG C, sol gel film is fully cured；
4th step, whole device is removed from hot plate and room temperature is cooled to, then by convex surface substrate of glass and PDMS soft templates
Separation, has now just prepared the micro-nano structure of durability in convex surface substrate of glass；There is micro-nano structure durability to be
Because the collosol and gel mixing material after solidification has the property similar to glass, it can be sticked to substrate of glass well
Together, therefore with high stability；The size of the final micro-nano structure obtained on bend glass depends on being used
The size of micro-nano structure on mother matrix, and it is limited to the resolution ratio of PDMS material；Generally, PDMS templates minimum can be for preparation
Below 100nm micro-nano structure, and micro-nano structure size it is more big contribute to micro-nano structure on mean camber glass of the present invention into
Prepared by work(, the micro-nano structure that this method is used to prepare more than micro-meter scale has splendid effect.
2. the preparation method according to claims 1, it is characterised in that by methacrylic acid -3- (trimethoxy silicon substrate)
Propyl ester (3-trimethoxysilyl propyl methacrylate) presses 0.04 with isopropyl alcohol and water:0.048:0.053 mole
Than mixing, the oxide sol for making it hydrolyze to form silicon.
3. the preparation method according to claims 1, it is characterised in that by metallorganic tetra isopropyl titanium and levulinic
Ketone is in nitrogen environment according to 1:Titanyl compound colloidal sol is made in 4 mol ratio.
4. the preparation method according to claims 1, it is characterised in that by adjusting titanium oxide sol in mixed solution
Shared proportions go out the collosol and gel hybrid glass material of different refractivity（Ranges of indices of refraction about 1.46-2.95 it
Between）, it is allowed to identical with the refractive index of bend glass substrate used.
5. the preparation method according to claims 1, it is characterised in that in order that SiO2/TiO2Mixed sols-gel material
Material has light sensitive characteristic, and adding light trigger includes 3%（By weight）bis(2,4,6-trimethylbenzoyl)
Phosphine oxide and 1%（By weight）1-hydroxycyclohexyl phenylketone, obtain having certain glue
The photosensitive sol gel film of degree.
6. the preparation method according to claims 1, it is characterised in that using existing micro-nano structure mother matrix copy with
Micro-nano structure is the PDMS soft templates of complementary structure on mother matrix.
7. the preparation method according to claims 1, it is characterised in that utilize prepared PDMS soft template matching steps
（1）The new photosensitive collosol and gel hybrid glass material of middle synthesis, according to（2）In step prepared on bend glass it is durable
The micro-nano structure of property.
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| CN201710276220.0A CN106980228B (en) | 2017-04-25 | 2017-04-25 | Method for preparing durable micro-nano structure on curved glass |
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| CN201710276220.0A CN106980228B (en) | 2017-04-25 | 2017-04-25 | Method for preparing durable micro-nano structure on curved glass |
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Cited By (4)
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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 |
| CN109990977A (en) * | 2019-03-29 | 2019-07-09 | 中国科学院近代物理研究所 | A kind of index-matching fluid |
| 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 |
| CN112782795A (en) * | 2021-01-29 | 2021-05-11 | 鲁东大学 | Method for preparing submicron grating with half period |
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| CN112782795B (en) * | 2021-01-29 | 2022-06-07 | 鲁东大学 | Method for preparing submicron grating with half period |
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