CN109575331A - A kind of small-bore optical imagery grade Kapton preparation method - Google Patents
A kind of small-bore optical imagery grade Kapton preparation method Download PDFInfo
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- CN109575331A CN109575331A CN201811464794.1A CN201811464794A CN109575331A CN 109575331 A CN109575331 A CN 109575331A CN 201811464794 A CN201811464794 A CN 201811464794A CN 109575331 A CN109575331 A CN 109575331A
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- optical imagery
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
The present invention provides a kind of small-bore optical imagery grade Kapton preparation methods, reduce wavefront error to improve film gauge uniformity, reach most basic image quality requirement, pass through multiple spin coating, until obtaining the Kapton of required thickness, the film transmission wavefront λ of λ, RMS≤1/30 of PV≤1/4 meets basic image quality requirement.The beneficial technical effect of the present invention: it is expected to reduce and external gap, raising thin-film component manufacture craft level extends the practical application area of China's thin-film component, especially transparent optical film diffraction imaging system field.
Description
Technical field
The present invention relates to diffraction optical element technical field, in particular to a kind of small-bore optical imagery grade polyimides is thin
Membrane preparation method.
Background technique
To space remote sensing system, more stringent requirements are proposed for the development of modernized war form.Geo-synchronous orbit satellite tool
There is high-timeliness, continue the advantages such as detectivity, is suitble to the demand of future military development.In order to improve geo-synchronous orbit satellite
Resolution ratio over the ground needs to develop heavy caliber space telescope system.Diffraction imaging system is small with density, face type tolerance is big, spreads out
The features such as high-efficient, optional material is more are penetrated, are one of the most potential solutions of heavy caliber space telescope system.
As the base material of binary optical elements, the thickness uniformity of thin-film material directly affects its wavefront error, sternly
Ghost image rings image quality, restricts the practical application of China's thin-film component.The image quality of thin-film component is improved, must just be mentioned
High film thickness uniformity.According to Rayleigh criterion, in order to reach most basic image quality requirement, film wavefront error pv value must be controlled
System is in 1/4 wavelength.Foreign countries at present can be by control errors before membrane wave in 1/4 wavelength, but carry out strict skill to China
Art block.In the open report of other domestic research groups, seldom sees and make internal disorder or usurp about grinding for film thickness error control.High quality it is thin
Membrane preparation technology only rests in external some advanced manufacturers and research institution's hand.In order to reduce the gap with foreign countries, improve thin
Membrane component manufacture craft is horizontal, and especially raising film gauge uniformity reduces wavefront error, is badly in need of progress related process and gropes
And breakthrough.
Summary of the invention
Reduce wavefront error to improve film gauge uniformity, reach most basic image quality requirement, the present invention mentions
A kind of low cost, high duplication, the wavefront error being simple and efficient has been supplied to meet the small-bore of image quality requirement less than 1/4 wavelength
Optical imagery grade Kapton preparation method.
Technical scheme is as follows: by the certain density polyamic acid solution of spin coating on quartz substrate, relying on
Extra solution is thrown away substrate itself by centrifugal force, and thin film is left on substrate, is subsequently transferred to carry out in heating plate
Preliminary drying removes solvent, finally carries out high temperature imidization and completes a circulation, spin coating-preliminary drying-imidization step is repeated, until obtaining
The Kapton of required thickness realizes that a kind of wavefront error meets the small-bore light of image quality requirement less than 1/4 wavelength
It studies as grade Kapton preparation method.Specific step is as follows:
Step 1: quartz substrate being fixed on suction piece platform by vacuum or mechanical system；
Step 2: preparing polyamic acid solution, and control in certain viscosity；
Step 3: a period of time on the appropriate solution levelling to the quartz substrate in step 1 in step 2, will be stood to solution
Infiltrate entire quartz substrate；
Step 4: extra solution is thrown away substrate itself by centrifugal force by the spin coating certain time under suitable revolving speed,
And thin film is left on substrate；
Step 5: the wet film in step 4 being transferred in heating plate and carries out preliminary drying removing solvent, until obtaining not any
The polyamic acid gel dry film of mobility；
Step 6: putting baking oven into together with quartz substrate and carry out the processing of high temperature hot imidization；
Step 7: if it is desired, repeating step 3 to step 6, until obtaining the Kapton of required thickness；
Step 8: film being stripped down from substrate finally, wavefront error is obtained less than 1/4 wavelength and meets image quality
It is required that small-bore optical imagery grade Kapton.
The beneficial effects of the present invention are: the present invention provides a kind of low cost, high duplication, the wavefront mistakes being simple and efficient
Difference meets the small-bore optical imagery grade Kapton preparation method of image quality requirement less than 1/4 wavelength, is expected to reduce
With external gap, thin-film component manufacture craft level is improved, the practical application area of China's thin-film component is extended.
Detailed description of the invention
Fig. 1 is optical grade polyimide film material interferometer test result figure (transmitted wave prepared by the embodiment of the present invention 1
Preceding figure)；
Fig. 2 is optical grade polyimide film material interferometer test result figure (interference item prepared by the embodiment of the present invention 1
Line figure)；
Fig. 3 is optical grade polyimide film material interferometer test result figure prepared by the embodiment of the present invention 2, wherein
Fig. 3 (a) is transmission wavefront figure, and Fig. 3 (b) is interference fringe picture；
Fig. 4 is optical grade polyimide film material interferometer test result figure prepared by the embodiment of the present invention 3, wherein
Fig. 4 (a) is transmission wavefront figure, and Fig. 4 (b) is interference fringe picture；
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical solution in the embodiment of the present invention is explicitly described, it is clear that described embodiment is the present invention
A part of the embodiment, instead of all the embodiments.
Embodiment 1
It uses n,N-dimethylacetamide solvent to prepare solid content as 10% polyamic acid solution, will be fitted after vacuum defoamation
It measures on solution levelling to quartz substrate, starts spin coating, subsequent preliminary drying after standing a period of time to the entire quartz substrate of solution impregnation
And imidization, complete a circulation.Three circulations are repeated, film is stripped down from substrate finally, is obtained with a thickness of 19 μ
The Kapton of m, bore 90mm.Film obtained is tested with interferometer, as a result as shown in Figure 1.Fig. 1 is that the present invention is real
The optical grade polyimide film material interferometer test result figure (transmission wavefront figure) of the preparation of example 1 is applied, Fig. 2 is that the present invention is implemented
Optical grade polyimide film material interferometer test result figure (interference fringe picture) prepared by example 1；PV value: 0.176 λ=
111nm, root mean square RMS:0.026 λ=16nm；Test wavelength λ=632.8nm.
Embodiment 2
It uses n,N-dimethylacetamide solvent to prepare solid content as 13% polyamic acid solution, will be fitted after vacuum defoamation
It measures on solution levelling to quartz substrate, starts spin coating, subsequent preliminary drying after standing a period of time to the entire quartz substrate of solution impregnation
And imidization, complete a circulation.Two circulations are repeated, film is stripped down from substrate finally, is obtained with a thickness of 15 μ
The Kapton of m, bore 90mm.Film obtained is tested with interferometer, as a result as shown in Figure 3.Fig. 3 is that the present invention is real
Apply the optical grade polyimide film material interferometer test result figure of the preparation of example 2, wherein Fig. 3 (a): transmission wavefront figure, Fig. 3
(b): interference fringe picture；PV value: 0.214 λ=135nm, root mean square RMS:0.022 λ=14nm；Test wavelength λ=632.8nm.
Embodiment 3
It uses n,N-dimethylacetamide solvent to prepare solid content as 15% polyamic acid solution, will be fitted after vacuum defoamation
It measures on solution levelling to quartz substrate, starts spin coating, subsequent preliminary drying after standing a period of time to the entire quartz substrate of solution impregnation
And imidization, complete a circulation.Two circulations are repeated, film is stripped down from substrate finally, is obtained with a thickness of 24 μ
The Kapton of m, bore 90mm.Film obtained is tested with interferometer, as a result as shown in Figure 4.Fig. 4 present invention is implemented
Optical grade polyimide film material interferometer test result figure prepared by example 3, wherein Fig. 4 (a): transmission wavefront figure, Fig. 4
(b): interference fringe picture；PV value: 0.241 λ=153nm, root mean square RMS:0.028 λ=18nm；Test wavelength λ=632.8nm.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the present invention, all to be said using the present invention
Equivalent structure or equivalent flow shift made by bright book and accompanying drawing content is applied directly or indirectly in other relevant technology necks
Domain similarly includes within the scope of the present invention.
Claims (5)
1. a kind of small-bore optical imagery grade Kapton preparation method, it is characterised in that: by being revolved on quartz substrate
Certain density polyamic acid solution is applied, extra solution is thrown away into substrate itself by centrifugal force, and leave one on substrate
Layer film is subsequently transferred to carry out preliminary drying removing solvent in heating plate, finally carries out high temperature imidization and complete a circulation, repeat
Spin coating-preliminary drying-imidization step, until obtaining the Kapton of required thickness, film transmission wavefront PV≤1/4 λ, RMS
≤ 1/30 λ meets image quality requirement.
2. small-bore optical imagery grade Kapton preparation method according to claim 1, it is characterised in that: quartz
Sizes of substrate >=Ф 100mm.
3. small-bore optical imagery grade Kapton preparation method according to claim 1, it is characterised in that: polyamides
The solid content of amino acid is 7%~15%.
4. small-bore optical imagery grade Kapton preparation method according to claim 1, it is characterised in that: use
The method of multiple spin coating superposition, until the Kapton of preparation required thickness, film thickness >=15 μm, film effective aperture
≥Ф90mm。
5. small-bore optical imagery grade Kapton preparation method according to any one of claims 1 to 4, feature
Be: the preparation method specifically includes the following steps:
Step 1: quartz substrate being fixed on suction piece platform by vacuum or mechanical system；
Step 2: preparing polyamic acid solution, and control in certain viscosity；
Step 3: a period of time on the appropriate solution levelling to the quartz substrate in step 1 in step 2, will be stood to solution impregnation
Entire quartz substrate；
Step 4: extra solution is thrown away substrate itself by centrifugal force by the spin coating certain time under suitable revolving speed, and
Thin film is left on substrate；
Step 5: the wet film in step 4 being transferred in heating plate and carries out preliminary drying removing solvent, until obtaining not no mobility
Polyamic acid gel dry film；
Step 6: putting baking oven into together with quartz substrate and carry out the processing of high temperature hot imidization；
Step 7: if it is desired, repeating step 3 to step 6, until obtaining the Kapton of required thickness；
Step 8: film being stripped down from substrate finally, wavefront error is obtained less than 1/4 wavelength and meets image quality requirement
Small-bore optical imagery grade Kapton.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811464794.1A CN109575331A (en) | 2018-12-03 | 2018-12-03 | A kind of small-bore optical imagery grade Kapton preparation method |
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| CN201811464794.1A CN109575331A (en) | 2018-12-03 | 2018-12-03 | A kind of small-bore optical imagery grade Kapton preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647180A (en) * | 2020-05-18 | 2020-09-11 | 中国科学院光电技术研究所 | Preparation method of large-aperture optical imaging polyimide film |
Citations (2)
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|---|---|---|---|---|
| CN102627780A (en) * | 2012-03-30 | 2012-08-08 | 北京化工大学 | Method for preparing submicron polyimide self-supporting film by adopting spin-coating method |
| CN105801856A (en) * | 2016-03-25 | 2016-07-27 | 中国科学院重庆绿色智能技术研究院 | Colorless transparent high-performance low-surface-roughness polyimide optical thin film material and preparation method thereof |
-
2018
- 2018-12-03 CN CN201811464794.1A patent/CN109575331A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627780A (en) * | 2012-03-30 | 2012-08-08 | 北京化工大学 | Method for preparing submicron polyimide self-supporting film by adopting spin-coating method |
| CN105801856A (en) * | 2016-03-25 | 2016-07-27 | 中国科学院重庆绿色智能技术研究院 | Colorless transparent high-performance low-surface-roughness polyimide optical thin film material and preparation method thereof |
Non-Patent Citations (4)
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| ZHIYU ZHANG: ""Hybrid-level Fresnel zone plate for diffraction efficiency enhancement"", 《OPTICS EXPRESS》 * |
| 曹国华 等: "《有机电致发光器件及载流子输运特性》", 30 November 2018 * |
| 李红军 等: ""薄膜沉积法制作菲涅耳透镜"", 《微细加工技术》 * |
| 王若秋 等: ""用于空间望远镜的大口径高衍射效率薄膜菲涅尔衍射元件"", 《红外与激光工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647180A (en) * | 2020-05-18 | 2020-09-11 | 中国科学院光电技术研究所 | Preparation method of large-aperture optical imaging polyimide film |
| CN111647180B (en) * | 2020-05-18 | 2022-10-21 | 中国科学院光电技术研究所 | Preparation method of large-aperture optical imaging polyimide film |
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Application publication date: 20190405 |