CN104536064B - The produced with combination method of optics ultra-wideband antireflective film - Google Patents
The produced with combination method of optics ultra-wideband antireflective film Download PDFInfo
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- CN104536064B CN104536064B CN201510010517.3A CN201510010517A CN104536064B CN 104536064 B CN104536064 B CN 104536064B CN 201510010517 A CN201510010517 A CN 201510010517A CN 104536064 B CN104536064 B CN 104536064B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Surface Treatment Of Glass (AREA)
- Surface Treatment Of Optical Elements (AREA)
Abstract
Ultra-wideband antireflective membrane compound technology method, comprises vacuum evaporation film forming and collosol and gel film forming; Vacuum evaporation film-forming process: preparation, the indoor all relevant appliance of clean vacuum are also put into optical mirror slip and are added coating materials; Vacuumize; Preheating coating materials; Coating materials vapor deposition is arrived to described optical lens surface; Toast 60 minutes; Carry out magnesium fluoride layer evaporation; The evaporation that carries out alumina layer under same baking temperature, the thicknesses of layers of evaporation is 4 nanometers; Step (1)-(6) for vacuum evaporation film-forming process; Step (7)-be (10) collosol and gel film-forming process. The present invention has reduced the rete number of broadband anti-reflection film, has widened the bandwidth region of existing broadband anti-reflection film. By plated film aftertreatment technology, rete has good hydrophobicity and self-cleaning performance, has good environmental suitability. Adopt composite membrane-forming method of the present invention, can reach 98.5% at 300nm-1000nm wavelength band mean transmissivity.
Description
Technical field
The present invention relates to optical coating processing technique field, particularly relate to a kind of preparation method of broadband anti-reflection film.
Background technology
Anti-reflection film eyeglass is a kind of important optics, its application be deep into Aero-Space remote sensing, laser communications,Photovoltaic cell, the ground many scientific instrument fields such as instrument of looking in the distance. Analyze from structural design, broad-band transparence-increased film glass is opticsSubstrate and multilayer dielectric film combine, and conventionally use high, medium and low three kinds of different refractivity materials to take in order to increase through bandwidthBe mixed with multilayer film, that the most frequently used is Al2O3—ZrO2—MgF2Collocation, but this matching structure is more complicated and only can be coated withThe spectral bandwidth of limit.
The vacuum anti-reflection film coating process method generally adopting at present comprises following job step: after clean optical mirror slip, putEnter vacuum chamber and add the preparation of coating materials, to vacuum chamber vacuumize, vacuum reaches vacuum chamber preheating and film after requirementThe preheating of material, the plated film step by coating materials vapor deposition to optical lens surface.
Better performances that collosol and gel anti-reflection film process has that technology controlling and process is simple, film is anti-reflection and be suitable for large faceThe advantage of long-pending masking. Comprise sol solution preparation, ageing of solution, plated film and heat treated process. By the standby porous of this legal systemSiO2 film has the advantages such as structure is controlled, refractive index is adjustable, damage threshold is high, optical characteristics is good, with low cost, can obtainBroadband anti-reflection effect. But its anti-reflection performance has much room for improvement.
Summary of the invention
The problem that the present invention need to solve is for above-mentioned the deficiencies in the prior art, and provide a kind of ultra-wideband antireflective film andIts preparation method. The prepared anti-reflection optical thin film of method of the present invention sees through bandwidth, and transmitance is high; And there is film structureThe feature of simply, easily implementing.
In order to address the above problem, the technical solution used in the present invention is: a kind of ultra-wideband antireflective membrane compound technology method,Comprise two kinds of technical process of vacuum evaporation film forming and collosol and gel film forming, it is characterized in that, step is as follows,
Wherein vacuum evaporation film-forming technology process comprises following job step:
(1). preparation, the indoor all relevant appliance of clean vacuum are also put into optical mirror slip and are added coating materials;
(2). vacuumize, described vacuum chamber is vacuumized;
(3). under the baking temperature of 300 degrees Celsius constant 60 minutes;
(4). carry out magnesium fluoride layer evaporation, the thicknesses of layers of evaporation is 83 nanometers;
(5). under same baking temperature, carry out the evaporation of alumina layer, the thicknesses of layers of evaporation is 4 nanometers;
(6). after optical mirror slip is naturally cooling, will further carry out collosol and gel film-forming technology process;
Wherein, collosol and gel film-forming technology process comprises following job step:
(7). produce base catalysis colloidal sol;
(8). the cleaning processing of the optical mirror slip after vacuum evaporation;
(9). lifting film forming on dipping coating machine;
(10). the dry and post processing of glued membrane.
Wherein, the operation of producing base catalysis colloidal sol (7) of described step is: will analyze pure level raw material tetraethyl orthosilicate(TEOS), deionized water, ammoniacal liquor and absolute ethyl alcohol n (TEOS) in molar ratio: n (H2O)：n(NH3)：n(C2H5OH)=1：2:0.6:34 mix; Under room temperature magnetic agitation condition, add container, continue to stir 3 hours after liquid feeding, 40 degrees Celsius closeEnvelope ageing obtains required base catalysis colloidal sol for 10 days.
Described step film forming step is (9): will be fixed to and lift coating machine folder through the clean optical mirror slip of processing of ultrasonic waveOn tool, the rate of pulling is 5-10cm/min.
The operation dry and post processing of described step glued membrane is (10): wet film is put into pregnancy again after drying in clean roomIn the organic solvent of base two silicon amine: hexane=1:2, soak 1h, taking-up is dried after drying under 450 degrees celsius.
Owing to having adopted such scheme, the present invention compared with prior art has following beneficial effect: 1, the present invention's preparationAnti-reflection optical thin film see through bandwidth, transmitance is high; 2, the present invention has film structure feature simple, that easily implement. , logicalCross the complex method that adopts vacuum evaporation and collosol and gel, reduced the rete number of broadband anti-reflection film, widened existing broadband and increasedThe bandwidth region of permeable membrane. By plated film aftertreatment technology, rete has good hydrophobicity and self-cleaning performance, has good ringBorder adaptability. Adopting traditional sol-gel method, is 97% at 300nm-1000nm wavelength band mean transmissivity; Adopt thisThe composite membrane-forming method of invention, can reach 98.5% at 300nm-1000nm wavelength band mean transmissivity.
Brief description of the drawings
Fig. 1 is the transmittance curve of compound ultra-wideband antireflective film in 300nm-1100nm wavelength band;
The anti-reflection curve of the broadband anti-reflection film that Fig. 2 vacuum deposition method is coated with.
Detailed description of the invention
Embodiment 1, the preparation method of broadband anti-reflection film. This anti-reflection film process of preparing is specific as follows:
1, preparation: clean vacuum chamber, coating clamp etc., in electron gun crucible, put into respectively magnesium fluoride and aluminium oxideCoating materials, optical mirror slip is put into vacuum chamber after cleaning totally and is fastened door for vacuum chamber.
2, vacuumize and optical mirror slip heating step: start vavuum pump and vacuumize and be warming up to gradually 300 degrees Celsius, heat upStep and constant temperature time determine according to the size of optical mirror slip and shape.
3, vacuum coating step: first carry out magnesium fluoride layer evaporation, the rete of evaporation under the baking temperature of 300 degrees CelsiusThickness is 83 nanometers, and then carries out the evaporation of alumina layer at same temperature, and the thicknesses of layers of evaporation is 4 nanometers.
4, adopt the film forming step of base catalysis colloidal sol: preprepared base catalysis colloidal sol is put into dipping and lift coating machineColloidal sol pond in, will be fixed to and lift on coating machine fixture through the optical mirror slip of the clean vacuum evaporation of processing of ultrasonic wave,Carry out sol-gal process film forming, the rate of pulling is 5-10cm/min.
5, the dry and post-processing step of glued membrane: wet film is put into hmds again after drying in clean room: hexane=In the organic solvent of 1:2, soak 1h, object is the hydrophilic radical hydroxyl in order to replace film surface with hydrophobic grouping, and taking-up is driedAfter under 450 degrees celsius, dry.
Claims (2)
1. a ultra-wideband antireflective membrane compound technology method, is characterized in that, comprises vacuum evaporation film forming and collosol and gel film formingTwo kinds of technical process;
Wherein vacuum evaporation film-forming technology process comprises following job step:
(1). preparation, the indoor all relevant appliance of clean vacuum are also put into optical mirror slip and are added coating materials;
(2). vacuumize, described vacuum chamber is vacuumized;
(3). under the baking temperature of 300 degrees Celsius constant 60 minutes;
(4). carry out magnesium fluoride layer evaporation, the thicknesses of layers of evaporation is 83 nanometers;
(5). under same baking temperature, carry out the evaporation of alumina layer, the thicknesses of layers of evaporation is 4 nanometers;
(6). after optical mirror slip is naturally cooling, will further carry out collosol and gel film-forming technology process;
Wherein, collosol and gel film-forming technology process comprises following job step:
. produce base catalysis colloidal sol;
. the cleaning processing of the optical mirror slip after vacuum evaporation;
. lifting film forming on dipping coating machine;
. the dry and post processing of glued membrane;
Described stepThe operation of producing base catalysis colloidal sol be:
To analyze pure level raw material tetraethyl orthosilicates (TEOS), deionized water, ammoniacal liquor and absolute ethyl alcohol n (TEOS) in molar ratio：n(H2O)：n(NH3)：n(C2H5OH)=1:2:0.6:34 mixes; Under room temperature magnetic agitation condition, add container, liquid feedingAfter continue stir 3 hours, 40 degrees Celsius sealing ageings within 10 days, obtain required base catalysis colloidal sol;
Described stepFilm forming step be:
To be fixed to and lift on coating machine fixture through the clean optical mirror slip of processing of ultrasonic wave, the rate of pulling be 5-10cm/min.
2. ultra-wideband antireflective membrane compound technology method according to claim 1, is characterized in that described stepGlued membraneDry and post-processing operation be:
Wet film is put into hmds: hexane=1:2 again organic solvent after drying in clean room soaks 1h, and taking-up is dried in the airAfter dry, under 450 degrees celsius, dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510010517.3A CN104536064B (en) | 2015-01-08 | 2015-01-08 | The produced with combination method of optics ultra-wideband antireflective film |
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| CN201510010517.3A CN104536064B (en) | 2015-01-08 | 2015-01-08 | The produced with combination method of optics ultra-wideband antireflective film |
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| CN104536064A CN104536064A (en) | 2015-04-22 |
| CN104536064B true CN104536064B (en) | 2016-05-18 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108070824A (en) * | 2016-11-17 | 2018-05-25 | 上海域申光电科技有限公司 | Reduce the film plating process of optical thin film internal stress |
| CN107703625B (en) * | 2017-09-27 | 2020-12-01 | 湖北东田光电材料科技有限公司 | Method for judging design correctness of each film layer of broadband antireflection film |
| CN110928012A (en) * | 2019-12-06 | 2020-03-27 | 深圳市康盛光电科技有限公司 | Anti-electric breakdown preparation method of ITO conductive film for light modulation film |
| CN115555235B (en) * | 2022-10-28 | 2023-07-18 | 西南科技大学 | Preparation method of silicon dioxide antireflection film |
| CN115893992B (en) * | 2022-11-02 | 2024-02-20 | 广德特旺光电材料有限公司 | Preparation method of silicon aluminum oxide ceramic evaporation material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CA2230552C (en) * | 1998-02-25 | 2002-12-31 | James Stilburn | Wide-band two layer antireflection coating for optical surfaces |
| CN101508191B (en) * | 2009-03-30 | 2012-06-27 | 天津美泰真空技术有限公司 | Anti-reflection film on polycarbonate/polymethylacrylate composite plate and preparation method thereof |
| JP2011164181A (en) * | 2010-02-05 | 2011-08-25 | Toppan Printing Co Ltd | Antireflective film |
| CN102153292B (en) * | 2010-12-27 | 2013-10-16 | 上海师范大学 | High-transmission nano silicon dioxide anti-reflection film and preparation method and application thereof |
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