CN101434614A - Compound for manufacturing anti-reflection film and method for manufacturing anti-reflection film - Google Patents

Compound for manufacturing anti-reflection film and method for manufacturing anti-reflection film Download PDF

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Publication number
CN101434614A
CN101434614A CNA200710170356XA CN200710170356A CN101434614A CN 101434614 A CN101434614 A CN 101434614A CN A200710170356X A CNA200710170356X A CN A200710170356XA CN 200710170356 A CN200710170356 A CN 200710170356A CN 101434614 A CN101434614 A CN 101434614A
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China
Prior art keywords
reflection film
solution
compound
ethylene glycol
straight chain
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CNA200710170356XA
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Chinese (zh)
Inventor
翁畅健
陈庆松
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BenQ Materials Corp
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Daxon Technology Inc
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Priority to CNA200710170356XA priority Critical patent/CN101434614A/en
Publication of CN101434614A publication Critical patent/CN101434614A/en
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Abstract

The invention discloses a compound used for preparing an anti-reflection film, and a preparation method of the anti-reflection film. The compound has the structure of Si(OR)3-O-[Si(OR)2-O]n-Si(OR)3. In the formula, R is selected from C3H9-, C2H5- or CH3-, and n is an integral number from 1 to 15. The method includes the following steps: preparation of a first solution, a collosol-gelatum reaction is carried out to a mixed solution of the compound, a fluorinated siloxane-based monomer, a catalyst and a solvent; coating of the first solution on the surfacel; and drying process to form the anti-reflection film. The fluorinated siloxane-based monomer has the structure of CF3(CF2)mCH2CH2-Si(OX)3, and in the formula, X is selected from C3H9-, C2H5- or CH3- and m is an integral number from 0 to 10. The film has the physical properties of comparatively low light reflectivity as well as relatively high attrition resistance and hardness.

Description

Be used to make the manufacture method of the compound and the anti-reflection film of anti-reflection film
Technical field
The present invention relates to a kind of manufacture method that is used to make compound and a kind of anti-reflection film of anti-reflection film, be used to make the luminous reflectance factor of the indicator screen film that can reduce optical module or display unit.
Background technology
Luminous reflectance factor is one of important factor that influences the screen display effect in the indicating meter of optical module or display unit.Lower luminous reflectance factor can improve display effect.Therefore, the many anti-reflection films that can use of the indicating meter of optical module or display unit are to reduce luminous reflectance factor.
Cause the major cause of luminous reflectance to be, when light wave is advanced through different media,, cause having part light to penetrate back the former medium from different medium interfaces because different media has different refractivity.
The known film that reduces luminous reflectance factor comprises fluoride film.Its principle is that the refractive index ratio base material of fluoride film is low, and the phase differential of the light that is reflected reaches 180 °, and the reflection ray at two interfaces reaches the purpose that reduces luminous reflectance owing to forming destruction interference.Fluoride film comprises and utilizes vapour deposition method to form, yet this method is difficult to utilize vapour deposition method to form uniform fluoride film when making the larger area substrate.
Disclose low reflectivity film No. 91136165 in the TaiWan, China patent with nanostructure.Its principle is to utilize at film surface to form structural changess such as carving line, and then specific refractory power is changed.Yet this method is comparatively loaded down with trivial details and cost is higher on technology.In addition, disclose in U.S. Pat 20060099407, modification makes and has after reactive terminal functional group on nanoparticle surface, makes low reflectivity film by the formed hole of the mutual storehouse of nanoparticle again.This film turbidity value (Haze) is higher, and causes loosely organizedly easily because of the structure mesoporosity is more, causes physical propertiess such as abrasion performance bad.
Open among clear 61-40845 and the special fair 6-98703 the Japanese Patent spy and to disclose the coating fluoroalkyl silanes or to have the method for the fluorinated polymer of ad hoc structure.Yet add excessive fluoric compound and often cause wetting effect difference and the bad shortcoming of thin film physics character.In the technology of another the low luminous reflectance factor film-forming method disclosed in the U.S. Pat 6472012, need pyroprocessing, be not suitable for being applied on the substrate as non-refractories such as Polarizers through 420 ℃.In U.S. Pat 6773121, disclose and carry out cryogenic sol gel reaction, to make anti-reflection film with monomers such as siloxanes sol-gel precursors monomer commonly used and fluorine silicon oxyalkyls.But the antireflection degree of this film is unsatisfactory.
Summary of the invention
Main purpose of the present invention is to provide a kind of compound that is used to make anti-reflection film, makes film have lower luminous reflectance factor.
Another main purpose of the present invention is to provide a kind of compound that is used to make anti-reflection film, makes film have the higher abrasion performance degree and the physical properties of hardness.
Another main purpose of the present invention is to provide a kind of manufacture method of anti-reflection film, makes film have lower luminous reflectance factor.
Another main purpose of the present invention is to provide a kind of manufacture method of anti-reflection film, makes film have the higher abrasion performance degree and the physical properties of hardness.
The compound that is used to make anti-reflection film of the present invention, it has Si (OR) 3-O-[Si (OR) 2-O] n-Si (OR) 3Structure, in the formula, R is selected from C 3H 9-, C 2H 5-or CH 3-, and n is 1 to 15 integer.Compound molecular weight is 400 to 2000.
The manufacture method step of anti-reflection film of the present invention comprises: prepare first solution, carry out sol gel reaction by the mixing solutions with above-claimed cpd, fluoro siloxanyl monomers, catalyzer and solvent and form; With first solution coat in the surface; And carry out drying process, to form anti-reflection film.The fluoro siloxanyl monomers has CF 3(CF 2) mCH 2CH 2-Si (OX) 3Structure, in the formula, X is selected from C 3H 9-, C 2H 5-or CH 3-, m is 0 to 10 integer.
Method further comprises: prepare second solution, carry out sol gel reaction by the mixing solutions with straight chain type siloxane oligomer, catalyzer and solvent and form; And replace first solution in the application step and coat the surface with the mixing solutions of first solution and second solution.Catalyzer comprises acidity or alkaline matter.
Description of drawings
Fig. 1 is the embodiment schema of the manufacture method of anti-reflection film of the present invention; And
Fig. 2 is the preferred embodiment schema of the manufacture method of anti-reflection film of the present invention.
Embodiment
The invention provides a kind of compound that is used to make anti-reflection film, and a kind of manufacture method of anti-reflection film.
Of the present inventionly be used to make the compound of anti-reflection film for having Si (OR) 3-O-[Si (OR) 2-O] n-Si (OR) 3The straight chain type siloxane oligomer of structure, in the formula, R is selected from C 3H 9-, C 2H 5-or CH 3-, and n is 1 to 15 integer.Compound molecular weight is 400 to 2000.In a preferred embodiment, above-mentioned straight chain type siloxane oligomer can become the compound compositions that is used to make anti-reflection film jointly with the fluoro siloxanyl monomers.Wherein, the fluoro siloxanyl monomers has CF 3(CF 2) mCH 2CH 2-Si (OX) 3Structure, in the formula, X is selected from C 3H 9-, C 2H 5-or CH 3-, and m is 0 to 10 integer.
Fig. 1 illustrates the embodiment schema of the manufacture method of anti-reflection film of the present invention.Step 3001 is undertaken forming after the sol gel reaction by the mixing solutions with above-mentioned straight chain type siloxane oligomer, above-mentioned fluoro siloxanyl monomers, catalyzer and solvent for preparing first solution.Above-mentioned catalyzer comprises acidity or alkaline matter.In a preferred embodiment, catalyzer select for use hydrogenchloride (hydrogen chloride, HCl).
Solvent is by Virahol (i-propyl alcohol), propyl carbinol (n-butanol), isopropylcarbinol (i-butanol), the trimethyl carbinol (t-butanol), methylethylketone (methyl ethyl ketone), mibk (methyl isobutyl ketone), ethylene glycol positive propyl ether (ethylene glycoln-propyl ether), ethylene glycol monomethyl ether (ethylene glycol monomethyl ether), ethylene glycol monoethyl ether (ethylene glycol monoethyl ether), diethylidene ethylene glycol monomethyl ether (diethylene glycol monomethyl ether), diethylidene ethylene glycol monoethyl ether (diethylene glycol monoethyl ether), select in propylidene ethylene glycol monomethyl ether (propylene glocol monoethyl ether) or its mixture.In a preferred embodiment, solvent is selected Virahol for use.
Step 3004 is in the surface with first solution coat.What in a preferred embodiment, the coating process of second solution used is that rod is coated with method.Yet in different embodiment, the coating process of second solution can use methods such as spin-coating method, dip coating or spraying method.
Step 3005 is for carrying out drying process, to form anti-reflection film.In a preferred embodiment, drying process uses the baking of circulation baking oven for heating.Yet in different embodiment, also can use drying processes such as natural air drying, vacuum-drying.Below illustrate manufacture method and each step of above-mentioned anti-reflection film.
Embodiment 1
Get tetraethyl silicate (ethyl silicate), 2 ten three fluoro-1 that restrain as fluoro siloxanyl monomers of 3 grams as the straight chain type siloxane oligomer, 1,2,2-tetrahydro-octyl group trimethoxy silane (tridecafluoro-1,1,2,2-tetrahydrooctyl) trimethoxysilan, 10 restrains Virahol and the 1.5 0.1N hydrogenchloride that restrain as catalyzer as solvent, stir 30 minutes at room temperature until reaching homogeneous phase fully, then carrying out sol gel reaction under 70 ℃ the temperature of reaction after 2 hours, reduce to room temperature, promptly form first solution.In a preferred embodiment, first solution can be further filters with the strainer of 0.45um, and refrigerates standby.
Get above-mentioned first solution of 1.5 grams, 3.5 gram isopropanol solvents and 0.5 gram ethylene glycol positive propyl ether solvent, in room temperature, stir after 10 minutes, with No. 4 rods, coat on the substrate surface with application rate 80mm/s, and place 100 ℃ circulation baking oven to toast 5 minutes, then took out afterwards in 20 hours, can obtain being attached to the anti-reflection film of substrate surface with 90 ℃ of constant temperature bakings.
Fig. 2 illustrates the preferred embodiments of the present invention schema, in a preferred embodiment, the manufacture method of anti-reflection film of the present invention further comprises: step 3002, promptly, prepare second solution, undertaken forming after the sol gel reaction by mixing solutions with straight chain type siloxane oligomer, catalyzer and solvent; And step 3003, that is, coat the surface with the mixing solutions of first solution and second solution.Below illustrate each step of different embodiment.
Embodiment 2
Get tetraethyl silicate, 2 ten three fluoro-1 that restrain as fluoro siloxanyl monomers of 3 grams as the straight chain type siloxane oligomer, 1,2,2-tetrahydro-octyl group trimethoxy silane, 10 restrains as the Virahol of solvent and the 1.5 0.1N hydrogenchloride that restrain as catalyzer, in room temperature, stir 30 minutes until reaching homogeneous phase fully, then, carrying out sol gel reaction under 70 ℃ the temperature of reaction after 2 hours, reduce to room temperature, promptly form first solution.In a preferred embodiment, first solution can be further filters with the strainer of 0.45um, and refrigerates standby.
Get 2 grams as the tetraethyl silicate of straight chain type siloxane oligomer, 10 grams as the Virahol of solvent and 2 grams as the 0.1N hydrogenchloride of catalyzer, in carrying out sol gel reaction under 80 ℃ the temperature of reaction after 2 hours, reduce to room temperature, promptly form second solution.In a preferred embodiment, second solution can be further filters with the strainer of 0.45um, and refrigerates standby.
Get above-mentioned first solution of 1.5 grams, above-mentioned second solution of 0.5 gram, 3.5 gram isopropanol solvents and 0.5 gram ethylene glycol positive propyl ether solvent, in room temperature, stir after 10 minutes, with No. 4 rods, coat on the substrate surface with application rate 80mm/s, and place 100 ℃ circulation baking oven to toast 5 minutes, then, took out afterwards in 20 hours with 90 ℃ of constant temperature bakings, can obtain being attached to the anti-reflection film of substrate surface.
The present invention is described by above-mentioned related embodiment, yet the foregoing description is only for implementing example of the present invention.Must be pointed out that the embodiment that has disclosed does not limit the scope of the invention.On the contrary, be contained in the modification of the spirit of claim and scope and be equal to be provided with and be included in the scope of the present invention.
Symbol description
3001 step 3002 steps
3003 step 3004 steps
3005 steps

Claims (8)

1. a compound that is used to make anti-reflection film has the structure shown in the following formula: Si (OR) 3-O-[Si (OR) 2-O] n-Si (OR) 3, wherein, R is selected from C 3H 9-, C 2H 5-or CH 3-; And n is 1 to 15 integer.
2. compound according to claim 1, the molecular weight of described compound are 400 to 2000.
3. compound composition that is used to make anti-reflection film, contain:
The straight chain type siloxane oligomer has the structure shown in the following formula: Si (OR) 3-O-[Si (OR) 2-O] n-Si (OR) 3, wherein, R is selected from C 3H 9-, C 2H 5-or CH 3-; And n is 1 to 15 integer; And
The fluoro siloxanyl monomers has the structure shown in the following formula: CF 3(CF 2) mCH 2CH 2-Si (OX) 3, wherein, X is selected from C 3H 9-, C 2H 5-or CH 3-;
And m is 0 to 10 integer.
4. compound composition according to claim 3, the molecular weight of wherein said straight chain type siloxane oligomer are 400 to 2000.
5. anti-reflection film manufacture method may further comprise the steps:
Prepare first solution, carry out sol gel reaction by mixing solutions and form straight chain type siloxane oligomer, fluoro siloxanyl monomers, catalyzer and solvent;
With described first solution coat in the surface; And
Carry out drying process, to form described anti-reflection film;
Wherein, described straight chain type siloxane oligomer has the structure shown in the following formula:
Si (OR) 3-O-[Si (OR) 2-O] n-Si (OR) 3, wherein, R is selected from C 3H 9-, C 2H 5-or CH 3-, n is 1 to 15 integer;
Described fluoro siloxanyl monomers has the structure shown in the following formula: CF 3(CF 2) mCH 2CH 2-Si (OX) 3, wherein, X is selected from C 3H 9-, C 2H 5-or CH 3-,
M is 0 to 10 integer.
6. method according to claim 5 further comprises:
Prepare second solution, undertaken forming after the sol gel reaction by mixing solutions with described straight chain type siloxane oligomer, described catalyzer and described solvent; And
Mixing solutions with described first solution and described second solution replaces described first solution in the described application step and coats described surface.
7. method according to claim 5, wherein said catalyzer comprises acidity or alkaline matter.
8. method according to claim 5, wherein said solvent is by selecting in Virahol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, methylethylketone, mibk, ethylene glycol positive propyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylidene ethylene glycol monomethyl ether, diethylidene ethylene glycol monoethyl ether, propylidene ethylene glycol monomethyl ether or its mixture.
CNA200710170356XA 2007-11-15 2007-11-15 Compound for manufacturing anti-reflection film and method for manufacturing anti-reflection film Pending CN101434614A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942584A (en) * 2012-08-07 2013-02-27 马可 Oligomer compound, hydrophobic composition, preparation method of the oligomer compound, and use of the oligomer compound and the hydrophobic composition
DE102016208586A1 (en) 2015-05-19 2016-11-24 Eternal Materials Co., Ltd. Coating composition for increasing light transmission and coating made therefrom

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942584A (en) * 2012-08-07 2013-02-27 马可 Oligomer compound, hydrophobic composition, preparation method of the oligomer compound, and use of the oligomer compound and the hydrophobic composition
CN102942584B (en) * 2012-08-07 2015-11-04 鹤山市顺鑫实业有限公司 Oligomer compound, hydrophobic composition and its preparation method and application
DE102016208586A1 (en) 2015-05-19 2016-11-24 Eternal Materials Co., Ltd. Coating composition for increasing light transmission and coating made therefrom
US11046867B2 (en) 2015-05-19 2021-06-29 Eternal Materials Co., Ltd. Coating composition for enhancing light transmittance and coating layer formed therefrom

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