CN1102622C - Moistureproof antireflecting silica coating and its preparation - Google Patents

Moistureproof antireflecting silica coating and its preparation Download PDF

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Publication number
CN1102622C
CN1102622C CN98123529A CN98123529A CN1102622C CN 1102622 C CN1102622 C CN 1102622C CN 98123529 A CN98123529 A CN 98123529A CN 98123529 A CN98123529 A CN 98123529A CN 1102622 C CN1102622 C CN 1102622C
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China
Prior art keywords
coating
acid
mol ratio
dehydrated alcohol
water
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CN98123529A
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CN1250068A (en
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孙予罕
张晔
吴东
范文浩
徐耀
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

The present invention relates to a moistureproof antireflection SiO2 coating and a making method thereof. The coating is made from SiO2 and a certain amount of organic groups R'(R' can be straight-chain alkyl groups, alkenyl groups, phenyl groups, halothane groups, etc.) The making method comprises: Si(OR)4, R'xSi(OR)<4-x>(X is equal to 1, 2 or 3), absolute alcohol, water and an acid-base catalyst are mixed according to a certain proportion, aged and coated so as to obtain the coating. The coating has very high light transmission performance and hydrophobic property; the light transmission rate reaches 95 to 95.8%(the limiting value is 96%), and the contact angle is from 110 to 130 degrees.

Description

Moistureproof antireflecting silica coating and method for making thereof
The present invention relates to a kind of moistureproof antireflecting SiO 2Coating and method for making thereof.
Sol-gel (Sol-Gel) method prepares hydrophobic SiO 2It is commonplace that film is studied abroad, in the majority with Japanese Patent especially, no matter be which country research, generally all adopts organic and inorganic sila formed material as main raw material, by the hydrophobic SiO of the final acquisition of sol-gel approach 2Film.Is the sila formed material that raw material can obtain containing Si-C and Si-O key by the Sol-Gel method with Rn ' Si (OR) 4-n.One European patent (EP 0 513 727 A2) is with Si (OR) 4With the fluoroalkyl siloxanes be that feedstock production goes out hydrophobic SiO 2Coating, the contact angle of film and water can reach 110 °.But its light transmission is not good enough.Adopt the antireflective SiO of sol-gel method preparation 2Coating can make the single face transmitance near 96% (two-sided transmitance is near 100%).As above people [" optics journal ", 1997,17 (3), 338] such as sea light machine institute Tonga seedling is with Si (OC 2H 5) 4Be raw material, prepare SiO by the sol-gel approach 2Colloidal sol adopt crystal pulling method to prepare transmittance near 96% antireflection coatings, but the humidity resistance of coating is relatively poor, and the contact angle of itself and water is below 40 °.
The objective of the invention is to develop a kind of hydrophobicity and the good moistureproof antireflecting SiO of anti-reflection property tool 2Coating and preparation method.
Coating of the present invention is coated on the substrate of glass, and the glass of this coating has purposes very widely.
Moistureproof antireflecting coating of the present invention is characterized in that having in the coating organic group R ' of some amount.
Preparation method of the present invention is as follows:
(1) with Si (OR) 4, R ' xSi (OR) 4-x (x=1,2 or 3), dehydrated alcohol mixes;
(2) catalyst by proportion with dehydrated alcohol, water and acid or alkali mixes;
(3) solution with (1) and (2) mixes stirring 30-300 minute;
(4) at 0-70 ℃ of aging 20-73 days;
(5) adopt crystal pulling method, rotational method or the coating of meniscus method.
Aforesaid R can be methyl, ethyl etc.
Aforesaid R ' can be straight chained alkyl, thiazolinyl, phenyl or fluoroalkyl.
Aforesaid R ' xSi (OR) 4-x and Si (OR) 4Mol ratio between 0.1-10, be preferably between the 0.5-5; Dehydrated alcohol and Si (OR) 4Mol ratio can be between 1-100; Water and Si (OR) 4Mol ratio can between 1-10, be preferably between the 1-6.5; Acid catalyst can be an organic acid, also can be mineral acid, and with mineral acid the best, as nitric acid, hydrochloric acid, sulfuric acid etc., alkaline catalysts can be amine or mineral alkali.
Test shows, the transmittance of single face coating of the present invention almost reach the ultimate value 96% of eyeglass single face coating transmittance up to 95-95.8%.Simultaneously coating of the present invention has very good hydrophobic performance, and the contact angle of it and water is up to 110-130 °, and the contact angle of common coating is only about 40 °.
Embodiments of the invention and measuring method are as follows:
Embodiment 1
(1) with 10mlSi (OC 2H 5) 4, 8.92ml (CH 3) 2Si (OC 2H 5) 2Mix with the 50ml dehydrated alcohol, stir 15min;
(2) with 54.3ml dehydrated alcohol and 2.8mlH 2O, 0.045ml 5.5N NH 3H 2The O mixing;
(3) above-mentioned (1) is mixed with (2), continue to stir 30min;
(4) solution that gained is mixed places encloses container, and 60 ℃ were worn out 20 days, and promptly got hydridization SiO 2Sol filming liquid;
(5) adopt the rotary plating method, be about to colloidal sol and drip on the substrate of high speed rotating, the hydrophobic anti-reflection SiO that keeps 1min to obtain meeting the requirements 2Film.
Decide the contact angle θ of coating and water, the quality of coming the hydrophobic performance of characterization of membrane according to this with FACE contact angle instrumentation.With UV spectrophotometric determination transmitance Tc-λ curve.Characterize the quality of light transmission with Tc.The θ of present embodiment coating=114 °, Tc=95.0%, CH in the coating 3-existence can confirm by the IR collection of illustrative plates, at 1276cm -1Si-CH 3The flexural vibration of middle c h bond absorb and 778cm -1And 830cm -1The stretching vibration of Si-C key absorbs can illustrate CH 3-existence.In addition, the increase of the contact angle of film and water has also confirmed the existence of hydrophobic grouping in the coating.
Embodiment 2
(1) with 10mlSi (OC 2H 5) 4, 7.68ml (CH 3) 2Si (OC 2H 5) 2Mix with the 50ml dehydrated alcohol, stir 15min;
(2) with 54.3ml dehydrated alcohol and 1.57mlH 2O, 0.045ml 5.5N NH 3H 2The O mixing;
(3) above-mentioned (1) is mixed with (2), continue to stir 30min;
(4) the solution sealing that gained is mixed is preserved, and places 25 ℃ to wear out 32 days;
Other is with embodiment 1, and measurement result is θ=110 °, Tc=95.8%.
Embodiment 3
(1) with 10mlSi (OC 2H 5) 4, 7.68ml (CH 3) 2Si (OC 2H 5) 2Mix with the 50ml dehydrated alcohol, stir 15min;
(2) with 54.3ml dehydrated alcohol and 2.34mlH 2O, 0.085ml 5.5N NH 3H 2The O mixing;
(3) above-mentioned (1) is mixed with (2), continue to stir 30min;
(4) the solution sealing that gained is mixed is preserved, and places 25 ℃ to wear out 32 days;
Other is with embodiment 1, and measurement result is θ=123 °, Tc=95.3%.
Embodiment 4
(1) with 5mlSi (OC 2H 5) 4, 3.84ml (CH 3) 2Si (OC 2H 5) 2Mix with the 50ml dehydrated alcohol, stir 15min;
(2) with 54.3ml dehydrated alcohol and 1.19mlH 2O, 0.026ml 5.5N NH 3H 2The O mixing;
(3) above-mentioned (1) is mixed with (2), continue to stir 30min;
(4) the solution sealing that gained is mixed is preserved, and places 25 ℃ to wear out 72 days;
Other is with embodiment 1, and measurement result is θ=130 °, Tc=95.0%.

Claims (6)

1. moistureproof antireflecting SiO 2Coating is characterized in that containing in this coating straight chained alkyl, thiazolinyl, phenyl or fluoroalkyl, and is prepared by following method:
(1) with Si (OR) 4, R ' xSi (OR) 4-x, dehydrated alcohol mixes;
(2) catalyst by proportion with dehydrated alcohol, water and acid or alkali mixes;
(3) solution with (1) and (2) mixes stirring 30-300 minute;
(4) at 0-70 ℃ of aging 20-73 days;
(5) adopt crystal pulling method, rotational method or the coating of meniscus method;
Wherein R ' is straight chained alkyl, thiazolinyl, phenyl or fluoroalkyl, and R is methyl, ethyl,
X=1,2 or 3
R ' xSi (OR) 4-x and Si (OR) 4Mol ratio between 0.1-10
Dehydrated alcohol and Si (OR) 4Mol ratio between 1-100
Water and Si (OR) 4Mol ratio between 1-10.
2. the preparation method of coating as claimed in claim 1 is characterized in that step is as follows:
(1) with Si (OR) 4, R ' xSi (OR) 4-x, dehydrated alcohol mixes;
(2) catalyst by proportion with dehydrated alcohol, water and acid or alkali mixes;
(3) solution with (1) and (2) mixes stirring 30-300 minute;
(4) at 0-70 ℃ of aging 20-73 days;
(5) adopt crystal pulling method, rotational method or the coating of meniscus method;
Wherein R ' is straight chained alkyl, thiazolinyl, phenyl or fluoroalkyl, and R is methyl, ethyl,
X=1,2 or 3
R ' xSi (OR) 4-x and Si (OR) 4Mol ratio between 0.1-10
Dehydrated alcohol and Si (OR) 4Mol ratio between 1-100
Water and Si (OR) 4Mol ratio between 1-10.
3. coating as claimed in claim 1 is characterized in that described R ' xSi (OR) 4-x and Si (OR) 4Mol ratio between 0.5-5.
4. coating as claimed in claim 1 is characterized in that described water and Si (OR) 4Mol ratio between 1-6.5.
5. as claim 1,3 or 4 described coatings, it is characterized in that described acid catalyst is organic acid or mineral acid; Alkaline catalysts is amine or mineral alkali.
6. coating as claimed in claim 5 is characterized in that described mineral acid is nitric acid, hydrochloric acid or sulfuric acid.
CN98123529A 1998-10-07 1998-10-07 Moistureproof antireflecting silica coating and its preparation Expired - Fee Related CN1102622C (en)

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Application Number Priority Date Filing Date Title
CN98123529A CN1102622C (en) 1998-10-07 1998-10-07 Moistureproof antireflecting silica coating and its preparation

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CN1102622C true CN1102622C (en) 2003-03-05

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Publication number Priority date Publication date Assignee Title
CN101422774B (en) * 2008-12-09 2011-04-27 东华大学 Preparation method of enamel surface coatings with hydrophobic effect
CN103757706B (en) * 2014-01-08 2016-01-20 同济大学 A kind of preparation method of nonlinear optical crystal surface antireflection protective film

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0513727A2 (en) * 1991-05-13 1992-11-19 Toyota Jidosha Kabushiki Kaisha Water repellent glass and process for producing the same
WO1994023315A1 (en) * 1993-04-05 1994-10-13 Commissariat A L'energie Atomique Method for producing thin films having optical and abrasion resistance properties

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0513727A2 (en) * 1991-05-13 1992-11-19 Toyota Jidosha Kabushiki Kaisha Water repellent glass and process for producing the same
WO1994023315A1 (en) * 1993-04-05 1994-10-13 Commissariat A L'energie Atomique Method for producing thin films having optical and abrasion resistance properties

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