CN102976626A - Method of using sol-gel to prepare MgF2 antireflection film - Google Patents

Method of using sol-gel to prepare MgF2 antireflection film Download PDF

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Publication number
CN102976626A
CN102976626A CN2012104585320A CN201210458532A CN102976626A CN 102976626 A CN102976626 A CN 102976626A CN 2012104585320 A CN2012104585320 A CN 2012104585320A CN 201210458532 A CN201210458532 A CN 201210458532A CN 102976626 A CN102976626 A CN 102976626A
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gel
solution
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陈源清
张古强
童少利
孙希佳
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention discloses a method of using sol-gel to prepare an MgF2 antireflection film. The method of using the sol-gel to prepare the MgF2 antireflection film comprises dissolving magnesium chloride in solvent with a certain amount of hydrofluoric acid as reactant to form MgF2 sol which is stable in performance and good in film-forming property, then obtaining a gel thin film on glass and other substrates combined with a dip-coating method or a roller painting method with the obtained MgF2 sol, and drying the obtained gel thin film in air, carrying out heat treatment, and obtaining a MgF2 thin film with high transmittance. Low-price magnesium chloride and ethanol are used as starting materials, carry out chemical reaction with hydrofluoric acid to form nanosized magnesium fluoride particles and dissolve in the ethanol. Magnesium fluoride sol which is stable in performance and good in film-forming property is formed. After drying and simple heat treatment are carried out to the thin film obtained through a pulling method and a suspended coating method and the like, the magnesium fluoride thin film with the transmittance up to 98% can be prepared.

Description

A kind of use sol-gel method prepares MgF 2The method of antireflective coating
Technical field
The invention belongs to the reflectance coating preparing technical field, relate to the sol-gel method technology of preparing of used for solar batteries anti-reflection film, specifically, is that a kind of use sol-gel method prepares MgF 2The method of antireflection film.
Background technology
Antireflective coating claims again anti-reflection film, and namely light-plated film on optical element surface is used for reducing the reflection of optical element surface, increases the transmitance of light, thereby improves the performance in operation wavelength or wave band.
For the research of antireflective coating, as far back as 1817, Joseph's fraunhofer adopted aciding to make first antireflection film.1886, Lip river moral Rayleigh found that the glass-reflected rate of tarnishing is lower than the glass of just polishing, and reason is to have formed a very thin skim on the glass surface, and its specific refractory power is lower than the specific refractory power of its base material.From the angle of film, the most significant progress is the Fabry-Perot interferometer that occurs in 1899, and it has become a kind of basic structure formation of Thin Film Filter.Twentieth century three, the forties, the multilayer film theory of antireflective coating and reflection enhancing coating system and interference monochromatic filter is arisen at the historic moment in succession.
Making rapid progress of science and technology, the emerging in large numbers and the continuous lifting of manufacture level and design level of novel material, the performance index of antireflective coating have had greatly lifting, are widely used in every field.Development along with solar cell, the design of antireflection film has become the key factor of solar cell design, because light makes light loss up to more than 30% in the reflection of silicon face, if plate suitable film at silicon face, utilize the film interference principle that reflection of light is greatly reduced, thereby improve short-circuit photocurrent density and the photoelectric transformation efficiency of solar cell.The reflection that is coated with the silicon solar cell of antireflection film significantly reduces, and effciency of energy transfer has improved 49%.Someone has prepared two-layer TiO at silicon solar cell 2And SiO 2Antireflection film, the average reflectance of solar cell are 7.9%, and the reflectivity of not filming is 37.4%, and it is about 47% that the absorption of solar cell has increased, and measurable battery efficiency is increased to 17.4% from 12.1%, has namely improved 44%.
Along with expanding economy, increasing high building is rised sheer from level ground.Glass curtain wall integrates decorates ventilation and lighting, has been subject to liking of construction unit, but has also brought negative effect one light pollution simultaneously.And at these coating antireflection films on glass, then can effectively reduce this light pollution.Moreover, windshield, windowpane, shop glass, showcase etc. have such requirement.Liquid-crystal display has become the mainstream technology in the indicating meter revolution, but it still has many weak points aspect practical present: angle of visibility is little, be subjected to ambient light effects strong, when the visual angle surpasses a certain scope, that image just thickens is unclear, contrast gradient reduces.The application of antireflective coating helps the optimization of liquid-crystal display performance.In optical communication, faint reflected light also can detect the transmission of optical signal and produce material impact.
In a word, antireflection film is at solar cell, glass curtain wall, and optical mirror slip, the every field such as Display projector technology have this to use widely.At present, the main raw for the preparation of antireflection film has SiO 2, TiO 2, MgF 2, silicon nitride etc.SiO 2, TiO 2Be a kind of oxide compound, corrosion resistance nature is high, is reasonable antireflection film by people's understanding.So far, although this antireflection film has obtained scale operation, mainly be limited to SiO 2Film, process is complicated, and cost is high, and a lot of technology have to be overcome.And MgF 2Have lower specific refraction, and stable performance, be a kind of good anti-reflection film.But MgF 2Preparation difficulty, the film of this respect is seldom arranged up to now.
The technology of preparation film is a lot, comprises the sol-gel method of chemistry, spray heating decomposition, chemical Vapor deposition process, the in addition magnetron sputtering method of physics.In these methods, sol-gel method is more cheap, the method for solution scale operation, and the gained film has porousness.And the porous antireflection film has lower specific refraction, can reduce the reflectivity of film.Therefore, sol-gel method has very large advantage aspect the preparation antireflection film.
But sol-gel method generally prepares oxide material, fluoride materials few people film.What this patent was reported is exactly to use preparation of sol-gel MgF 2Antireflection film, the gained film will be at optics, solar cell, cladding glass, following high-clear display, the aspects such as shadow casting technique field have important application.
Summary of the invention
The purpose of this invention is to provide a kind of use sol-gel method and prepare MgF 2The method of antireflection film has been avoided expensive alkoxide and trifluoroacetic use, has reduced the pollution to environment, has reduced preparation cost.
Technical scheme of the present invention is that a kind of use sol-gel method prepares MgF 2The method of antireflection film at first, is made reactant with a certain amount of hydrofluoric acid and magnesium chloride is dissolved in the MgF that has formed stable performance and good film-forming property in the solvent 2Colloidal sol; Then use the MgF for preparing 2Colloidal sol in the substrates such as glass, makes gel film in conjunction with dip-coating method or rolling method; Subsequently that the gel film that obtains is dry under air, and heat-treat, get final product the MgF of high permeability 2Film.
Specifically implement according to following steps:
1) preparation of fluorine-containing colloidal sol:
Magnesium chloride is dissolved in the solvent solution, make mol ratio magnesium chloride: solvent=1:(20~100), obtain solution A, with hydrofluoric acid dissolution in solvent solution, so that mol ratio hydrofluoric acid: solvent=1:(15~40), obtain solution B, then solution B is dropwise joined in the solution A that is stirring, after two kinds of solution of solution A and solution B mixed, return stirring was after 12~36 hours under 40 ℃~200 ℃ temperature, obtain magnesium fluoride colloidal sol
The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: solvent=1:(2.0~2.2): (50~180);
2) preparation of gel film and drying:
With the magnesium fluoride colloidal sol of step 1) preparation, in conjunction with dip-coating method, spin coating method or roller painting, make the magnesium fluoride gel film at glass, quartz or silicon substrate, subsequently the film that obtains was descended dry 5~10 minutes at 80~100 ℃, vapor away unnecessary solvent, obtain the gel dry film;
3) film thermal is processed:
With step 2) the gel dry film that makes puts into retort furnace, 300 ℃~550 ℃ temperature lower calcinations 5~50 minutes, and get final product,
If increase the thickness of film, but repeating step 2) and step 3) step several times.
Characteristics of the present invention also are,
Solvent described in the step 1) is ethanol or methyl alcohol.
Magnesium chloride described in the step 1) can substitute with magnesium acetate or magnesium hydroxide.
Step 3) is at air, N 2Or carry out under the Ar gas atmosphere.
Beneficial effect of the present invention is that it is starting raw material that the method adopts cheap magnesium chloride and ethanol, by carrying out chemical reaction in hydrofluoric acid, forms the magnesium fluoride particle of nanometer, is dissolved in the ethanol.Formed the magnesium fluoride colloidal sol of stable performance and good film-forming property.By lift, be coated with etc. that method is dried resulting film and brief heat treating after, can prepare transmitance up to 98% magnesium fluoride film.
Description of drawings
Fig. 1 is that the present invention uses sol-gel method to prepare MgF 2The preparation flow figure of colloidal sol in the method for antireflection film;
Fig. 2 is the MgF of method preparation of the present invention 2The antireflection film optical lens is crossed curve.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The invention provides a kind of use sol-gel method and prepare MgF 2The method of antireflection film is divided into the preparation of preparation, gel film of colloidal sol and drying, film thermal is processed three processes.At first, make reactant with a certain amount of hydrofluoric acid and magnesium chloride is dissolved in the MgF that has formed stable performance and good film-forming property in the ethanol 2Colloidal sol; Then use the colloidal sol of preparing, in the substrates such as glass, make gel film in conjunction with dip-coating method or rolling method; Subsequently that the gel film that obtains is dry under air, heat-treat under the certain temperature, get final product the MgF of high permeability 2Film.
Specifically implement according to following steps:
1) preparation of fluorine-containing colloidal sol, as shown in Figure 1:
Magnesium chloride is dissolved in the solvent solution, make mol ratio magnesium chloride: solvent=1:(20~100), obtain solution A after stirring clarification, with hydrofluoric acid dissolution in solvent solution, so that mol ratio hydrofluoric acid: solvent=1:(15~40), obtain solution B after stirring clarification, then solution B is dropwise joined in the solution A that is stirring, make that the mol ratio of Mg and HF is 1:2-2.2 in the mixed solution, after two kinds of solution of solution A and solution B mix, return stirring obtained magnesium fluoride colloidal sol after 12~36 hours under 40 ℃~200 ℃ temperature
The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: solvent=1:(2.0~2.2): (50~180), and wherein solvent is ethanol or methyl alcohol;
Wherein magnesium chloride can substitute with magnesium acetate or magnesium hydroxide.
2) preparation of gel film and drying:
With the magnesium fluoride colloidal sol of step 1) preparation, in conjunction with dip-coating method, spin coating method or roller painting, make the magnesium fluoride gel film at glass, quartz or silicon substrate, subsequently the film that obtains was descended dry 5~10 minutes at 80~100 ℃, vapor away unnecessary solvent, obtain the gel dry film;
3) film thermal is processed:
With step 2) the gel dry film that makes puts into retort furnace, at air, N 2Or under the Ar gas atmosphere, 300 ℃~550 ℃ temperature lower calcinations 5~50 minutes, and get final product,
If increase the thickness of film, but repeating step 2) and step 3) step several times.
Fig. 2 is the MgF of method preparation of the present invention 2The antireflection film optical lens is crossed curve.As shown in FIG., the transmitance of 550nm place sample has reached 98.2%, and transmitance has exceeded 7-9% than simple glass, compares SiO 2Antireflective coating has exceeded 4-5%.
The preparation method of the magnesium fluoride film of method preparation of the present invention, adopting cheap small molecules metal chlorate or acetate is starting raw material, do not relate to expensive macromole metal carboxylate or metal alkoxide, adopted the common organic solutions such as ethanol to make solvent, greatly reduce cost; The fluohydric acid content and the magnesium ion that add in the colloidal sol just in time react completely, and have eliminated the existence of other F ions, thereby the free F ion that contains in the gained solution is considerably less, has reduced environmental pollution.Even colloidal sol is rotten, after discharging, can be to environment yet.
Prepare magnesium fluoride film technique with other chemical methods and compare, avoided using expensive alkoxide.In the solution preparation process, avoided trifluoroacetic use.Moreover, the film preparation cycle also shortens greatly, and film preparation efficient improves greatly, is applicable to following big area, large-scale, mass production antireflection film.
Embodiment 1:
Be dissolved in the ethanol with magnesium hydroxide, obtain clear soln A after the stirring.The ratio of magnesium hydroxide and ethanol is in the A solution: magnesium hydroxide: ethanol=1:20.Then with 55% hydrofluoric acid dissolution in an amount of ethanol, obtain solution B.Hydrofluoric acid in the solution B: ethanol=1:15.A solution is stirred, add gradually B solution while then stir A solution.When in A, the B mixing solutions during Mg:HF=1:2, stop the interpolation of B solution.Then with the A of gained, B mixing solutions 80 ℃ of lower return stirrings 24 hours, obtain MgF 2Colloidal sol.The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium hydroxide: hydrofluoric acid: ethanol=1:2.0:50.
Utilize prepared MgF 2Colloidal sol at ambient temperature, lifts by dipping, roller coat, or be coated with method, lift in substrate of glass and apply one deck MgF 2Gel-film.Subsequently, the gel-film that obtains is incubated 5 minutes under 80 ℃ of conditions, subsequently at air conditions, 400 ℃ are incubated 15 minutes down.Repeatedly after above-mentioned plated film-drying-thermal treatment 3 times, namely obtain MgF 2Anti-reflection film, transmitance can reach 98.1%.
Embodiment 2:
Magnesium acetate is dissolved in the ethanol, obtains clear soln A after the stirring.The ratio of magnesium acetate and ethanol is in the A solution: magnesium acetate: ethanol=1:100.Then with 55% hydrofluoric acid dissolution in an amount of ethanol, obtain solution B.Hydrofluoric acid in the solution B: ethanol=1:40.A solution is stirred, add gradually B solution while then stir A solution.When in A, the B mixing solutions during Mg:HF=1:2, stop the interpolation of B solution.Then with the A of gained, B mixing solutions 40 ℃ of lower return stirrings 36 hours, obtain MgF 2Colloidal sol.The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: ethanol=1:2.0:180.
Utilize prepared MgF 2Colloidal sol at ambient temperature, lifts by dipping, roller coat, or be coated with method, lift in substrate of glass and apply one deck MgF 2Gel-film.Subsequently, the gel-film that obtains is incubated 7 minutes under 100 ℃ of conditions, under air, 550 ℃ are incubated 5 minutes down subsequently.Repeatedly after above-mentioned plated film-drying-thermal treatment 4 times, namely obtain MgF 2Anti-reflection film, transmitance can reach 98.5%.
Embodiment 3:
Magnesium acetate is dissolved in the methyl alcohol, obtains clear soln A after the stirring.The ratio of magnesium acetate and methyl alcohol is in the A solution: magnesium acetate: methyl alcohol=1:30.Then with 55% hydrofluoric acid dissolution in an amount of methyl alcohol, obtain solution B.Hydrofluoric acid in the solution B: methyl alcohol=1:20.A solution is stirred, add gradually B solution while then stir A solution.When in A, the B mixing solutions during Mg:HF=1:2.2, stop the interpolation of B solution.Then with the A of gained, B mixing solutions 120 ℃ of lower return stirrings 36 hours, obtain MgF 2Colloidal sol.The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: methyl alcohol=1:2.2:74.
Utilize prepared MgF 2Colloidal sol at ambient temperature, lifts by dipping, roller coat, or be coated with method, lift in substrate of glass and apply one deck MgF 2Gel-film.Subsequently, the gel-film that obtains is incubated 5 minutes under 90 ℃ of conditions, subsequently at N 2In, 300 ℃ are incubated 50 minutes down.Repeatedly after above-mentioned plated film-drying-thermal treatment 3 times, namely obtain MgF 2Anti-reflection film, transmitance can reach 98.2%.
Embodiment 4:
Magnesium acetate is dissolved in the methyl alcohol, obtains clear soln A after the stirring.The ratio of magnesium acetate and methyl alcohol is in the A solution: magnesium acetate: methyl alcohol=1:30.Then with 55% hydrofluoric acid dissolution in an amount of methyl alcohol, obtain solution B.Hydrofluoric acid in the solution B: methyl alcohol=1:40.A solution is stirred, add gradually B solution while then stir A solution.When in A, the B mixing solutions during Mg:HF=1:2.1, stop the interpolation of B solution.Then with the A of gained, B mixing solutions 200 ℃ of lower return stirrings 12 hours, obtain MgF 2Colloidal sol.The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: methyl alcohol=1:2.1:84.
Utilize prepared MgF 2Colloidal sol at ambient temperature, lifts by dipping, roller coat, or be coated with method, lift in substrate of glass and apply one deck MgF 2Gel-film.Subsequently, the gel-film that obtains is incubated 10 minutes under 100 ℃ of conditions, subsequently in Ar gas condition, 400 ℃ are incubated 5 minutes down.Repeatedly after above-mentioned plated film-drying-thermal treatment 4 times, namely obtain MgF 2Anti-reflection film, transmitance can reach 98.5%.

Claims (5)

1. one kind is used sol-gel method to prepare MgF 2The method of antireflection film is characterized in that, at first, makes reactant with a certain amount of hydrofluoric acid and magnesium chloride is dissolved in the MgF that has formed stable performance and good film-forming property in the solvent 2Colloidal sol; Then use the MgF for preparing 2Colloidal sol in the substrates such as glass, makes gel film in conjunction with dip-coating method or rolling method; Subsequently with the gel film that obtains through super-dry and thermal treatment, MgF that can high permeability 2Film.
2. method according to claim 1 is characterized in that, specifically implements according to following steps:
1) preparation of fluorine-containing colloidal sol:
Magnesium chloride is dissolved in the solvent solution, make mol ratio magnesium chloride: solvent=1:(20~100), obtain solution A, with hydrofluoric acid dissolution in solvent solution, so that mol ratio hydrofluoric acid: solvent=1:(15~40), obtain solution B, then solution B is dropwise joined in the solution A that is stirring, after two kinds of solution of solution A and solution B mixed, return stirring was after 12~36 hours under 40 ℃~200 ℃ temperature, obtain magnesium fluoride colloidal sol
The mol ratio of effective constituent is in the magnesium fluoride colloidal sol: magnesium chloride: hydrofluoric acid: solvent=1:(2.0~2.2): (50~180);
2) preparation of gel film and drying:
With the magnesium fluoride colloidal sol of step 1) preparation, in conjunction with dip-coating method, spin coating method or roller painting, make the magnesium fluoride gel film at glass, quartz or silicon substrate, subsequently the film that obtains was descended dry 5~10 minutes at 80~100 ℃, vapor away unnecessary solvent, obtain the gel dry film;
3) film thermal is processed:
With step 2) the gel dry film that makes puts into retort furnace, 300 ℃~550 ℃ temperature lower calcinations 5~50 minutes, and get final product,
If increase the thickness of film, but repeating step 2) and step 3) step several times.
3. method as described in claim 2 is characterized in that the solvent described in the step 1) is ethanol or methyl alcohol.
4. method as claimed in claim 2 is characterized in that, the magnesium chloride described in the step 1) can substitute with magnesium acetate or magnesium hydroxide.
5. method as claimed in claim 2 is characterized in that, step 3) is at air, N 2Or carry out under the Ar gas atmosphere.
CN2012104585320A 2012-11-14 2012-11-14 Method of using sol-gel to prepare MgF2 antireflection film Pending CN102976626A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109655942A (en) * 2018-12-19 2019-04-19 宁波甬安光科新材料科技有限公司 A kind of optical thin film, optical module and preparation method comprising the film
CN111018538A (en) * 2019-11-21 2020-04-17 天津津航技术物理研究所 Preparation method of oxynitride medium-wave infrared window material
CN115490436A (en) * 2022-09-23 2022-12-20 新福兴玻璃工业集团有限公司 Antireflection magnesium fluoride coated glass and online preparation method thereof
CN116004108A (en) * 2022-12-29 2023-04-25 宁波勤邦新材料科技有限公司 Transparent front plate base film and preparation method thereof
CN116925624A (en) * 2023-08-24 2023-10-24 湖南庆润新材料有限公司 Self-cleaning anti-reflection coating, coating and preparation method

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CN101846756A (en) * 2010-05-26 2010-09-29 湖南大学 MgF2/oxide composite membrane used for anti-reflection of glass surface

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109655942A (en) * 2018-12-19 2019-04-19 宁波甬安光科新材料科技有限公司 A kind of optical thin film, optical module and preparation method comprising the film
CN111018538A (en) * 2019-11-21 2020-04-17 天津津航技术物理研究所 Preparation method of oxynitride medium-wave infrared window material
CN115490436A (en) * 2022-09-23 2022-12-20 新福兴玻璃工业集团有限公司 Antireflection magnesium fluoride coated glass and online preparation method thereof
CN115490436B (en) * 2022-09-23 2024-02-02 新福兴玻璃工业集团有限公司 Anti-reflection magnesium fluoride coated glass and online preparation method thereof
CN116004108A (en) * 2022-12-29 2023-04-25 宁波勤邦新材料科技有限公司 Transparent front plate base film and preparation method thereof
CN116004108B (en) * 2022-12-29 2023-09-08 宁波勤邦新材料科技股份有限公司 Transparent front plate base film and preparation method thereof
CN116925624A (en) * 2023-08-24 2023-10-24 湖南庆润新材料有限公司 Self-cleaning anti-reflection coating, coating and preparation method
CN116925624B (en) * 2023-08-24 2024-02-23 湖南庆润新材料有限公司 Self-cleaning anti-reflection coating, coating and preparation method

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Application publication date: 20130320