CN110117375A - A kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type - Google Patents
A kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type Download PDFInfo
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- CN110117375A CN110117375A CN201910424939.3A CN201910424939A CN110117375A CN 110117375 A CN110117375 A CN 110117375A CN 201910424939 A CN201910424939 A CN 201910424939A CN 110117375 A CN110117375 A CN 110117375A
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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 invention discloses a kind of thickness successively to be successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type, by the polyamic acid glue for being cast low concentration on the quartz base plate with certain optical surface type of level leveling, any external force is not applied, make glue upper surface by the automatic levelling of capillary effect of itself surface tension and edge peripheral frame, and in the subsequent uniform removing process of vacuum, guarantee the absolute and horizontality of quartz base plate, realize that a kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type.Film can be applied to the fields such as transparent optical film reflecting mirror, film condenser, flexible thin-film solar cell, optical antenna, be with a wide range of applications.
Description
Technical field
The invention belongs to optical film technology field, in particular to a kind of thickness successively successively decreases by outer diameter to the center of circle, upper table
Face is in the polyimides method for preparing optical thin film of dimple type, by being cast disposable film forming, is a kind of low cost, is simple and efficient
Pre-formed film preparation method.
Background technique
With space optics, the development of space communication and earth observation technology, as space telescope, radar, antenna, energy
The primary optics measured collector, amplify imaging system, the high-resolution of reflecting mirror, the requirement of big visual field are increasingly
It is high.For a long time, conventional mirror does base base, major defect using the rigid material of the form stables such as glass, metal, crystal
It is that surface density is big, difficulty of processing is big, the manufacturing cycle is long, at high cost, it is difficult to suitable for super large caliber optical system to reflecting mirror
It is required that.
As material science recent decades are fast-developing, the appearance of high-performance polyimide film is so that flexible membrane base reflects
Mirror is possibly realized in space application.Compared with the large caliber reflecting mirror of traditional material, fexible film reflecting mirror has fairly obvious
The advantages of: surface density is small, and flexibility can open up/and it is foldable, the cost of material is low, the period is short, forming freedom degree is big etc., rocket fortune can be solved
Carry the limitation to limited bulk, quality.Membrane-base reflecting mirror is one kind using flexible polymer film as base base, with external force control plane shape
The external force such as reflecting mirror, such as electrostatic force, gas pressure the deformation and maintenance of face type are carried out to film.But there are surface precision compared with
Difference, the technological difficulties such as profile control is more difficult, control structure is complicated, the serious membrane-base reflecting mirror that restricts are led in large-aperture optical component
The popularization and utilization in domain.
The polyimides light that the invention mainly relates to a kind of thickness successively to be successively decreased by outer diameter to the center of circle, upper surface is in dimple type
Learn method for manufacturing thin film, disposably formed a film by the tape casting, the pre-formed film of thickness-tapered is prepared, be it is a kind of it is low at
Originally, the method that repeatability is high, is simple and efficient.
Summary of the invention
The polyamic acid glue that the present invention passes through the curtain coating low concentration on the quartz base plate with certain face type of level leveling
Liquid does not apply any external force, and glue upper surface is made to rely on the automatic levelling of capillary effect of itself mobility and edge peripheral frame,
And during subsequent vacuum desolvation agent, guarantee the absolute and horizontality of quartz base plate, realize a kind of thickness by
Outer diameter successively successively decreases to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type.
Technical scheme is as follows: a kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the poly- of dimple type
Acid imide method for preparing optical thin film, by being cast the poly- of low concentration on the quartz base plate with certain face type of level leveling
Amic acid glue does not apply any external force, makes glue upper surface by the surface tension of itself and the capillary effect of edge peripheral frame
Automatic levelling is answered, and in the subsequent uniform removing process of vacuum, guarantees the absolute and horizontality of quartz base plate,
Realize a kind of thickness successively successively decreased by outer diameter to the center of circle, upper surface be in dimple type polyimides method for preparing optical thin film.
Wherein, it is disposably formed a film using the tape casting, gained Kapton thickness >=20 μm, film effective aperture >=Ф
200mm。
Wherein, round fused quartz real estate type: upper surface PV Zhi≤1/10 λ, RMS≤1/50 λ；Lower surface Zhi≤1/4 PV
The λ of λ, RMS≤1/20；Quartz base plate bore >=Φ 250mm.
Wherein, peripheral frame is using aluminium frame, polytetrafluoroethylene (PTFE) frame, carbon fibre composite frame or epoxy glue frame.
Wherein, marble leveling platform flatness is 00 grade or more, three of them levelling foot is accurate adjustable up and down.
Wherein, the electrolevel precision for level leveling is 1 μm/m.
Wherein, the solid content that polyamic acid after diluent mixing is added is 2%-3%, gelatin viscosity 100-1000cps, dilute
Releasing agent is N,N-dimethylformamide.
Wherein, the desolventizing by the way of vacuumizing at room temperature, vacuum pumping speed 0.5L/S-6L/S, vacuum plant cavity
Interior Zhen Kong Du≤150Pa.
Wherein, the top cover the center point of vacuum plant is connected by bellows with vacuum pump, and ball valve is equipped in pipeline, and
It is adjustable；
Horizontal stability is very good after the leveling of fused quartz substrate, and still maintains during entire vacuum desolvation agent
Stablize.
After leveling the quartz base plate level of optical surface, solvent is controlled by the way of vacuum desolvation agent and is uniformly delayed
Slow vaporization, and ensure that substrate keeps stability in entire subsequent process, thickness is prepared under the capillary effect of peripheral frame
Successively successively decreased by outer diameter to the center of circle, upper surface be in dimple type polyimides optical thin film, the specific steps are as follows:
Step 1: the round fused quartz substrate carry out level leveling being placed in vacuum plant in marble platform, and
Its outer increases round enclosing；
Step 2: preparing polyamic acid glue, be diluted to a certain concentration after completion of the reaction；
Step 3: will be on the glue levelling to the quartz base plate in step 1 in step 2；And stand a few hours；
Step 4: connecting vacuum pump and carry out vacuum except solvent, ball valve valve is opened to minimum, until obtaining no any stream
The polyamic acid gel dry film of dynamic property；
Step 5: putting the dry film in step 4 into baking oven together with quartz base plate and carry out the processing of high temperature hot imidization；
Step 6: directly film is stripped down from substrate, obtain thickness successively successively decreased by outer diameter to the center of circle, upper surface
In the polyimides optical thin film of dimple type.
The beneficial effects of the present invention are: the works such as surface processing polished cumbersome compared to traditional dimple type optical glass
Skill, the present invention are a kind of polyimides method for preparing optical thin film with dimple type being simple and efficient, and save post-processing, are saved
A large amount of manpower and material resources reduce cost of manufacture.
Detailed description of the invention
Fig. 1 is the flow diagram that present invention preparation has micro- concave film；
Fig. 2 is the polyimide film material interferometer test result figure of the embodiment of the present invention 1, wherein Fig. 2 (a) is
Penetrate wave front chart；Fig. 2 (b) is interference fringe picture；
Fig. 3 is the polyimide film material interferometer test result figure of the embodiment of the present invention 2, wherein Fig. 3 (a) is
Penetrate wave front chart；Fig. 3 (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
Polyamic acid solution is diluted to by 2%, gelatin viscosity 120cps, and vacuum using n,N-Dimethylformamide solvent
Deaeration, then glue is carefully poured into advance on the quartz base plate of horizontal leveling, use aluminium frame for enclosing, and standing 1h makes and his like
It is steady fixed.Vacuum plant is sealed, is then opened ball valve to minimum, it is pre- that connection vacuum pump carries out vacuum under 120Pa vacuum degree
Solvent 18h is removed, polyamic acid dry film is obtained and directly strips down film from substrate after the processing of vacuum hot-imide
Obtain surface be in dimple type Kapton, 22 μm of film thickness, bore Φ 220mm.Film obtained is interfered
Instrument test, as a result as shown in Figure 2.Fig. 2 is optical grade polyimide film material interferometer test prepared by the embodiment of the present invention 1
Result figure, Fig. 2 (a): transmission wavefront figure, Fig. 2 (b): interference fringe picture.
Embodiment 2
Polyamic acid solution is diluted to by 2.5%, gelatin viscosity 400cps using n,N-Dimethylformamide solvent, and true
Then glue is carefully poured into advance on the quartz base plate of horizontal leveling, uses polytetrafluoroethylene (PTFE) frame for enclosing by empty deaeration, quiet
It sets 2h and is allowed to levelling stabilization.Vacuum plant is sealed, then opens ball valve to minimum, connects vacuum pump under 130Pa vacuum degree
It carries out vacuum and removes solvent 16h in advance, obtain polyamic acid dry film, after the processing of vacuum hot-imide, directly by film from substrate
On strip down obtain surface be in dimple type Kapton, 25 μm of film thickness, bore Φ 210mm.It will be obtained
Film is tested with interferometer, as a result as shown in Figure 3.Fig. 3 is optical grade polyimide film material prepared by the embodiment of the present invention 2
Interferometer test result figure, Fig. 3 (a): transmission wavefront figure, Fig. 3 (b): interference fringe picture.
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 (10)
- The polyimides method for preparing optical thin film that 1. a kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in dimple type, It is characterized by: by the polyamic acid glue for being cast low concentration on the quartz base plate with certain face type of level leveling, Do not apply any external force, glue upper surface made to rely on the automatic levelling of capillary effect of itself surface tension and edge peripheral frame, And in the subsequent uniform removing process of vacuum, guarantees the absolute and horizontality of quartz base plate, realize a kind of thickness Degree is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type.
- 2. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: it is disposably formed a film using the tape casting, gained Kapton thickness >=20 μ M, film effective aperture >=Ф 200mm.
- 3. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: round fused quartz real estate type: the upper surface λ of PV Zhi≤1/10, RMS≤1/50 λ；Lower surface PV Zhi≤1/4 λ, RMS≤1/20 λ；Quartz base plate bore >=Φ 250mm.
- 4. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: peripheral frame is using aluminium frame, polytetrafluoroethylene (PTFE) frame, carbon fibre composite frame Or epoxy glue frame.
- 5. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: it is 00 grade or more that marble, which levels platform flatness, three of them levelling foot is smart up and down It is really adjustable.
- 6. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: the electrolevel precision for level leveling is 1 μm/m.
- 7. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: the solid content that polyamic acid after diluent mixes is added is 2%-3%, glue Viscosity 100-1000cps, diluent are n,N-Dimethylformamide.
- 8. a kind of thickness according to claim 1 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: the desolventizing by the way of vacuumizing at room temperature, vacuum pumping speed 0.5L/S- 6L/S, Zhen Kong Du≤150Pa in vacuum plant cavity.
- 9. a kind of thickness according to claim 8 is successively successively decreased by outer diameter to the center of circle, upper surface is sub- in the polyamides of dimple type Amine method for preparing optical thin film, it is characterised in that: the top cover the center point of vacuum plant is connected by bellows with vacuum pump, pipeline In ball valve is installed, and it is adjustable；Horizontal stability is very good after the leveling of fused quartz substrate, and still maintains steady during entire vacuum desolvation agent It is fixed.
- 10. a kind of described in any item thickness are successively successively decreased by outer diameter to the center of circle according to claim 1~9, upper surface is in dimple The polyimides method for preparing optical thin film of type, it is characterised in that: the preparation method specifically includes the following steps:Step 1: the round fused quartz substrate carry out level leveling being placed in vacuum plant in marble platform, and outside it Along the round enclosing of increase；Step 2: preparing polyamic acid glue, be diluted to a certain concentration after completion of the reaction；Step 3: will be on the glue levelling to the quartz base plate in step 1 in step 2；And stand a few hours；Step 4: connecting vacuum pump and carry out vacuum except solvent, ball valve valve is opened to minimum, until obtaining no any mobility Polyamic acid gel dry film；Step 5: putting the dry film in step 4 into baking oven together with quartz base plate and carry out the processing of high temperature hot imidization；Step 6: film being stripped down from substrate directly, obtains that thickness is successively successively decreased by outer diameter to the center of circle, surface is in dimple The polyimides optical thin film of type.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910424939.3A CN110117375A (en) | 2019-05-21 | 2019-05-21 | A kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910424939.3A CN110117375A (en) | 2019-05-21 | 2019-05-21 | A kind of thickness is successively successively decreased by outer diameter to the center of circle, upper surface is in the polyimides method for preparing optical thin film of dimple type |
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| CN110117375A true CN110117375A (en) | 2019-08-13 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218077A (en) * | 1991-08-26 | 1993-06-08 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Diphenylmethane-containing dianhydride and polyimides prepared therefrom |
| CN101113205A (en) * | 2007-07-20 | 2008-01-30 | 东南大学 | Method for preparing copolymerization tyoe polyimide film containing fluorenes structure |
| CN103087449A (en) * | 2013-01-16 | 2013-05-08 | 南昌航空大学 | Preparation method of polymer nanometer composite material with high heat conduction, high dielectric and low loss |
| CN106916324A (en) * | 2017-03-14 | 2017-07-04 | 华南理工大学 | Preparation method with low-k and high-fracture toughness polyimide film |
-
2019
- 2019-05-21 CN CN201910424939.3A patent/CN110117375A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5218077A (en) * | 1991-08-26 | 1993-06-08 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Diphenylmethane-containing dianhydride and polyimides prepared therefrom |
| CN101113205A (en) * | 2007-07-20 | 2008-01-30 | 东南大学 | Method for preparing copolymerization tyoe polyimide film containing fluorenes structure |
| CN103087449A (en) * | 2013-01-16 | 2013-05-08 | 南昌航空大学 | Preparation method of polymer nanometer composite material with high heat conduction, high dielectric and low loss |
| CN106916324A (en) * | 2017-03-14 | 2017-07-04 | 华南理工大学 | Preparation method with low-k and high-fracture toughness polyimide film |
Non-Patent Citations (2)
| Title |
|---|
| 向伟编著: "《工程流体力学》", 28 February 2017, 西安电子科技大学出版社 * |
| 吴国光: ""聚酰亚胺薄膜的酰亚胺化方法"", 《信息记录材料》 * |
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Application publication date: 20190813 |