CN115555235B - Preparation method of silicon dioxide antireflection film - Google Patents
Preparation method of silicon dioxide antireflection film Download PDFInfo
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Abstract
The invention discloses a preparation method of a silicon dioxide antireflection film, which comprises the following steps: multilayer SiO is prepared by sol-gel pulling film coating method 2 Film and method for producing the sameWherein the underlayer film A is acid catalyzed SiO 2 Sol and base catalyzed SiO 2 The upper film B is prepared by mixing sol and is SiO treated with HMDS 2 The sol is prepared, and the strong anti-reflection effect in a wide spectral range is realized through sequential multilayer superposition of A/B/A/B/A/B … A/B. Multilayer SiO prepared by the invention 2 The antireflection film has central wavelengths of 351nm, 527nm, 1053nm and 1064nm>98% transmittance, reflectance<2%; high laser damage threshold, its value is greater than or equal to 20J/cm ‑2 The method comprises the steps of carrying out a first treatment on the surface of the Good hydrophobicity and environmental stability, and the water contact angle is more than or equal to 125 degrees. Such a multilayer SiO 2 The anti-reflection film is superior to the traditional single-layer SiO in the relevant performance and application range 2 The antireflection film has more advantages and can be widely applied to various optical systems, such as a large pulse energy type laser, a high average power type laser, an optical lens or a window, and a Faraday rotator.
Description
Technical Field
The invention belongs to the technical field of optical material preparation, and particularly relates to a preparation method of a silicon dioxide antireflection film.
Background
In high power laser systems, there are many optical elements, and due to the drastic change in refractive index between air and the element interface, the laser light will be reflected strongly at the element interface, and this light reflection will not only disturb the judgment of the target chamber, damage the optical elements in the optical system, but also reduce the output of laser energy. In some special laser light path systems, the generated 1053nm fundamental beam needs to be converted into 351nm triple-frequency laser by a series of frequency conversion crystals, and during the frequency conversion process, some optical elements will bear four laser beams with wavelengths of 351nm, 527nm, 1053nm and 1064nm at the same time. Although the surface of the element is coated with a layer of silicon dioxide (SiO 2 ) The antireflection film can make the refractive index between element interfaces change smoothly, reduce light reflection and increase light transmission so as to reduce damage to the element, but single-layer SiO 2 The antireflection film can only provide effective antireflection at a single wavelength, and is difficult to meet the high transmittance requirements of optical elements in most laser systems for multiple wavelengths and wide bands. At this time, a single unit is reusedSiO of (2) 2 The antireflection film is difficult to meet the requirements of most optical elements on high light transmittance and low damage, and due to single SiO 2 The anti-reflection film has larger specific surface area and an open pore structure, has stronger hydrophilicity, and is easy to adsorb water and organic molecules in the environment, thereby leading to SiO 2 The environmental stability of the antireflection film is poor. These defects will damage the optical components in the system, significantly reduce the output of laser energy, reduce the useful life and accuracy of the components. Therefore, it is required to prepare SiO which has excellent anti-reflection effect at four wavelengths, good hydrophobicity and good environmental stability 2 An antireflection film.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for preparing a silica anti-reflection film, comprising: multilayer SiO is prepared by sol-gel pulling film coating method 2 A film, wherein the underlayer film A is an acid catalyzed SiO 2 Sol and base catalyzed SiO 2 The upper film B is prepared by mixing sol and is SiO treated with HMDS 2 The sol is prepared, and the strong anti-reflection effect in a wide spectrum range is realized through the sequential multilayer superposition of A/B/A/B.
Preferably, the method specifically comprises the following steps:
step one, preparing base catalyzed SiO 2 The sol comprises the following specific steps: mixing proper amount of ethyl orthosilicate, absolute ethyl alcohol and ammonia water to obtain a solution, sealing the solution in a reactor, stirring for a certain time at a certain temperature, standing and aging for a certain time at room temperature to obtain alkali-catalyzed SiO 2 Sol, named sol C;
step two, preparing acid-catalyzed SiO 2 The sol comprises the following specific steps: mixing proper amount of ethyl orthosilicate, absolute ethyl alcohol and deionized water uniformly, wherein the deionized water contains a certain amount of concentrated hydrochloric acid to obtain a reaction liquid, sealing the reaction liquid in a reactor, and stirring at a certain temperatureStirring and reacting for a certain time, then placing the mixture at room temperature and aging for a certain time to obtain acid-catalyzed SiO 2 Sol, named sol D;
step three, preparing HMDS/TEOS sol, which comprises the following specific steps: mixing proper amounts of absolute ethyl alcohol, ammonia water, deionized water, hexamethyldisilazane and ethyl orthosilicate, adding the reagents into a reactor, stirring for a certain time at a certain temperature, standing and aging at room temperature, diluting sol by absolute ethyl alcohol for one time before coating to obtain HMDS/TEOS sol, and marking the HMDS/TEOS sol as sol B;
step four, reflux condensing sol C for a certain time to remove ammonia until the pH test paper has no obvious change; then mixing sol C and sol D according to a certain volume ratio to obtain acid-base composite sol, and marking the acid-base composite sol as sol A;
step five, before lifting and pulling the coating, sequentially ultrasonically cleaning the substrate by using ethanol and acetone solution, and blowing the substrate clean by using a blower; and depositing sol A on a pre-cleaned substrate at a specific lifting speed to serve as a bottom layer film A, plating sol B on the bottom layer film A to serve as an upper layer film B, fully immersing the substrate in the sol A or sol B during plating, maintaining for a period of time after full immersion, extracting, airing at room temperature, and drying in an oven to obtain the A/B double-layer silicon dioxide antireflection film.
Preferably, when preparing 2-6 layers of silicon dioxide antireflection film, the bottom layer film A and the upper layer film B are prepared according to the method of the fifth step, and then repeatedly overlapped according to the mode of A/B/A/B/A/B with the same pulling speed.
Preferably, in the first step, the volume ratio of the ethyl orthosilicate, the absolute ethyl alcohol and the ammonia water is 13:130:5, the stirring temperature is 40 ℃, the stirring time is 12 hours, and the aging time is 24 hours.
Preferably, in the second step, the volume ratio of the ethyl orthosilicate, the absolute ethyl alcohol, the deionized water and the concentrated hydrochloric acid is 11:110:4:0.02, the stirring temperature is 40 ℃, the stirring time is 12 hours, and the aging time is 24 hours.
Preferably, in the third step, the volume ratio of the absolute ethyl alcohol, the ammonia water, the deionized water, the hexamethyldisilazane and the tetraethoxysilane is 110:0.6:2.5:1:10, the stirring temperature is 40 ℃, the stirring time is 12 hours, and the aging time is 24 hours.
Preferably, in the fourth step, the reflux condensation time is 10h, and the mixing volume ratio of sol c to sol d is 1:4.
Preferably, in the fifth step, the pulling speed is 80mm/min, and the maintenance time after complete immersion is 5-10 s.
The application of the preparation method of the silicon dioxide antireflection film is used for transmitting broad spectrum light with center wavelengths of 351nm, 527nm, 1053nm and 1064nm respectively.
The invention at least comprises the following beneficial effects: the invention prepares a plurality of layers of SiO by a simple and high-efficiency sol-gel pulling coating method 2 The number of the thin film samples is 2-6. Wherein the bottom film A is acid catalyzed SiO 2 Sol and base catalyzed SiO 2 Sol preparation is prepared by mixing at a volume of 1:4, and the upper layer film B is SiO treated with HMDS 2 Preparing sol. The strong anti-reflection effect in a wide spectrum range is realized through superposition of A/B/A/B/A/B … multilayer films. Multilayer SiO 2 The antireflection film has central wavelengths of 351nm, 527nm, 1053nm and 1064nm>98% transmittance, reflectance<2%; high laser damage threshold, its value is greater than or equal to 20J/cm -2 The method comprises the steps of carrying out a first treatment on the surface of the Good hydrophobicity and environmental stability, and the water contact angle is more than or equal to 125 degrees. Such a multilayer SiO 2 The anti-reflection film is superior to the traditional single-layer SiO in the relevant performance and application range 2 The antireflection film has more advantages, and can be widely applied to various optical systems, such as a large pulse energy type laser, a high average power type laser, an optical lens or window, a Faraday rotator and the like.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a 2-layer SiO prepared as in example 1 2 Transmittance map of antireflection film;
FIG. 2 is a 2-layer SiO produced in accordance with example 1 2 Reflectance map of the antireflection film.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
The preparation method of the 2-layer silicon dioxide antireflection film provided by the embodiment comprises the following steps:
step one, preparing base catalyzed SiO 2 The sol comprises the following specific steps: mixing 13mL of tetraethoxysilane, 130mL of absolute ethyl alcohol and 5mL of ammonia water to obtain a solution, sealing the solution in a 250mL double-neck round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature to obtain base-catalyzed SiO 2 Sol, named sol C;
step two, preparing acid-catalyzed SiO 2 The sol comprises the following specific steps: mixing 11mL of tetraethoxysilane, 110mL of absolute ethyl alcohol and 4mL of deionized water uniformly, wherein the deionized water contains 0.02mL of concentrated hydrochloric acid to obtain a reaction liquid, sealing the reaction liquid in a 250mL round-bottom flask, stirring and reacting for 12h at 40 ℃, and then standing and aging for 24h at room temperature to obtain acid-catalyzed SiO 2 Sol, named sol D;
step three, preparing HMDS/TEOS sol, which comprises the following specific steps: mixing 110mL of absolute ethyl alcohol, 0.6mL of ammonia water, 2.5mL of deionized water, 1mL of Hexamethyldisilazane (HMDS) and 10mL of Tetraethoxysilane (TEOS), adding the reagents into a 250mL round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature, diluting the sol by one time with absolute ethyl alcohol before coating to obtain HMDS/TEOS sol, and marking the HMDS/TEOS sol as sol B;
step four, reflux condensing sol C for 10 hours to remove ammonia until the pH test paper has no obvious change; then mixing sol C and sol D according to a volume ratio of 1:4 to obtain acid-base composite sol, and marking the acid-base composite sol as sol A;
step five, before lifting and pulling the coating, sequentially ultrasonically cleaning the substrate by using ethanol and acetone solution, and blowing the substrate clean by using a blower; the substrate is completely immersed in sol A and maintained for 5 hours, and the sol A is deposited on the substrate which is cleaned in advance at a lifting speed of 80mm/min to be used as a bottom layer film A; and then completely immersing the substrate in sol B and maintaining for 5s, depositing the sol B on the bottom layer film A at a lifting speed of 80mm/min to serve as an upper layer film B, drying the substrate at room temperature after the sol B is lifted out, and drying the substrate in an oven to obtain the A/B2 layer silicon dioxide antireflection film.
Example 2
The preparation method of the 2-layer silicon dioxide antireflection film provided by the embodiment comprises the following steps:
step one, preparing base catalyzed SiO 2 The sol comprises the following specific steps: mixing 13mL of tetraethoxysilane, 130mL of absolute ethyl alcohol and 5mL of ammonia water to obtain a solution, sealing the solution in a 250mL double-neck round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature to obtain base-catalyzed SiO 2 Sol, named sol C;
step two, preparing acid-catalyzed SiO 2 The sol comprises the following specific steps: mixing 11mL of tetraethoxysilane, 110mL of absolute ethyl alcohol and 4mL of deionized water uniformly, wherein the deionized water contains 0.02mL of concentrated hydrochloric acid to obtain a reaction liquid, sealing the reaction liquid in a 250mL round-bottom flask, stirring and reacting for 12h at 40 ℃, and then standing and aging for 24h at room temperature to obtain acid-catalyzed SiO 2 Sol, named sol D;
step three, preparing HMDS/TEOS sol, which comprises the following specific steps: mixing 110mL of absolute ethyl alcohol, 0.6mL of ammonia water, 2.5mL of deionized water, 1mL of Hexamethyldisilazane (HMDS) and 10mL of Tetraethoxysilane (TEOS), adding the reagents into a 250mL round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature, diluting the sol by one time with absolute ethyl alcohol before coating to obtain HMDS/TEOS sol, and marking the HMDS/TEOS sol as sol B;
step four, reflux condensing sol C for 10 hours to remove ammonia until the pH test paper has no obvious change; then mixing sol C and sol D according to a volume ratio of 1:4 to obtain acid-base composite sol, and marking the acid-base composite sol as sol A;
step five, before lifting and pulling the coating, sequentially ultrasonically cleaning the substrate by using ethanol and acetone solution, and blowing the substrate clean by using a blower; the substrate is completely immersed in sol A and maintained for 10s, and the sol A is deposited on the substrate which is cleaned in advance at a lifting speed of 80mm/min to be used as a bottom layer film A; and then the substrate is completely immersed in the sol B and maintained for 10 seconds, the sol B is deposited on the bottom layer film A at a lifting speed of 80mm/min to serve as an upper layer film B, and after the sol B is pulled out, the substrate is dried at room temperature and then dried in an oven, so that the A/B2 silicon dioxide antireflection film is obtained.
Example 3
The preparation method of the 6-layer silicon dioxide antireflection film provided by the embodiment comprises the following steps:
step one, preparing base catalyzed SiO 2 The sol comprises the following specific steps: mixing 13mL of tetraethoxysilane, 130mL of absolute ethyl alcohol and 5mL of ammonia water to obtain a solution, sealing the solution in a 250mL double-neck round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature to obtain base-catalyzed SiO 2 Sol, named sol C;
step two, preparing acid-catalyzed SiO 2 The sol comprises the following specific steps: mixing 11mL of tetraethoxysilane, 110mL of absolute ethyl alcohol and 4mL of deionized water uniformly, wherein the deionized water contains 0.02mL of concentrated hydrochloric acid to obtain a reaction liquid, sealing the reaction liquid in a 250mL round-bottom flask, stirring and reacting for 12h at 40 ℃, and then standing and aging for 24h at room temperature to obtain acid-catalyzed SiO 2 Sol, named sol D;
step three, preparing HMDS/TEOS sol, which comprises the following specific steps: mixing 110mL of absolute ethyl alcohol, 0.6mL of ammonia water, 2.5mL of deionized water, 1mL of Hexamethyldisilazane (HMDS) and 10mL of Tetraethoxysilane (TEOS), adding the reagents into a 250mL round-bottom flask, stirring for 12h at 40 ℃, then standing and aging for 24h at room temperature, diluting the sol by one time with absolute ethyl alcohol before coating to obtain HMDS/TEOS sol, and marking the HMDS/TEOS sol as sol B;
step four, reflux condensing sol C for 10 hours to remove ammonia until the pH test paper has no obvious change; then mixing sol C and sol D according to a volume ratio of 1:4 to obtain acid-base composite sol, and marking the acid-base composite sol as sol A;
step five, before lifting and pulling the coating, sequentially ultrasonically cleaning the substrate by using ethanol and acetone solution, and blowing the substrate clean by using a blower; the substrate is completely immersed in sol A and maintained for 5s, and the sol A is deposited on the substrate which is cleaned in advance at a lifting speed of 80mm/min to be used as a bottom layer film A; completely immersing the substrate in sol B for 5s, and depositing the sol B on the bottom film A at a lifting speed of 80mm/min to serve as an upper film B; then repeatedly superposing according to the sequence of A/B, lifting and plating a bottom layer film A on an upper layer film B, lifting and plating an upper layer film B on the bottom layer film A until the form of plating A/B/A/B/A/B6 layers of films, wherein the immersion time and lifting speed of each layer of film are the same as those of the embodiment 1; and (3) after the silicon dioxide antireflection film is extracted, airing at room temperature, and then drying in an oven to obtain the 6-layer silicon dioxide antireflection film.
The transmittance and the reflectance of the A/B double-layer silicon dioxide antireflection films prepared in the examples 1 and 2 to light with different wavelengths are respectively measured and compared with a K9 glass sheet purchased on the market to obtain the graph 1 and the graph 2, wherein the abscissa in the graph 1 is wavelength and the ordinate in the transmittance, and the abscissa in the graph 2 is wavelength and the ordinate in the reflectance; as can be seen from fig. 1 and 2, the a/B2 layer silica antireflection films prepared in example 1 and example 2 have a large light transmittance and a lower light reflectance in the wavelength range of 400 to 2000nm, compared to the K9 glass sheet.
Disclosed "hydrophobic SiO 2 Preparation of broadband antireflection film and its Performance study in the Studies of Master science, TEOS is used as SiO 2 Adding 4.8mL of deionized water, 196mL of absolute ethyl alcohol and 1.2mL of ammonia water into 20mL of tetraethoxysilane under alkaline conditions, uniformly mixing, and aging for 12d at room temperature to obtain the base-catalyzed SiO 2 Film, orUnder the acidic condition, adding 6.4mL of deionized water, 196mL of absolute ethyl alcohol and 0.03mL of hydrochloric acid into 20mL of tetraethoxysilane, uniformly mixing, and aging for 12d at room temperature to prepare the acid-catalyzed SiO 2 The result shows that the prepared alkali-catalyzed and acid-catalyzed SiO is prepared by the film 2 The film does not have the anti-reflection effect of broadband light, and the base catalysis SiO 2 The average anti-reflection rate of the film is 97.46%, and the acid catalysis SiO 2 The average anti-reflection rate of the film is 94.63 percent, and the anti-reflection effect of the film is lower than that of the A/B2 layer silicon dioxide anti-reflection film prepared by the invention (the A/B2 layer silicon dioxide anti-reflection film prepared by the preparation method provided by the invention has the central wavelengths of 351nm, 527nm, 1053nm and 1064nm>98% light transmittance).
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (5)
1. The preparation method of the silicon dioxide antireflection film is characterized by comprising the following steps: multilayer SiO is prepared by sol-gel pulling film coating method 2 A film, wherein the underlayer film A is an acid catalyzed SiO 2 Sol and base catalyzed SiO 2 The upper film B is prepared by mixing sol and is SiO treated with HMDS 2 The sol is prepared, and the strong anti-reflection effect in a wide spectrum range is realized through the sequential 6-layer lamination of A/B/A/B; the method specifically comprises the following steps:
step one, preparing base catalyzed SiO 2 The sol comprises the following specific steps: mixing proper amount of ethyl orthosilicate, absolute ethyl alcohol and ammonia water to obtain a solution, sealing the solution in a reactor, and in a certain periodStirring for a certain time under the temperature condition, then placing at room temperature for aging for a certain time to obtain the base-catalyzed SiO 2 Sol, named sol C;
step two, preparing acid-catalyzed SiO 2 The sol comprises the following specific steps: mixing proper amount of ethyl orthosilicate, absolute ethyl alcohol and deionized water uniformly, wherein the deionized water contains a certain amount of concentrated hydrochloric acid to obtain a reaction liquid, sealing the reaction liquid in a reactor, stirring and reacting for a certain time under a certain temperature condition, and then standing and aging for a certain time under a room temperature condition to obtain acid-catalyzed SiO 2 Sol, named sol D;
step three, preparing HMDS/TEOS sol, which comprises the following specific steps: mixing proper amounts of absolute ethyl alcohol, ammonia water, deionized water, hexamethyldisilazane and ethyl orthosilicate, adding the reagents into a reactor, stirring for a certain time at a certain temperature, standing and aging at room temperature, diluting sol by absolute ethyl alcohol for one time before coating to obtain HMDS/TEOS sol, and marking the HMDS/TEOS sol as sol B;
step four, reflux condensing sol C for a certain time to remove ammonia until the pH test paper has no obvious change; then mixing sol C and sol D according to a certain volume ratio to obtain acid-base composite sol, and marking the acid-base composite sol as sol A;
step five, before lifting and pulling the coating, sequentially ultrasonically cleaning the substrate by using ethanol and acetone solution, and blowing the substrate clean by using a blower; depositing sol A on a pre-cleaned substrate at a specific lifting speed to serve as a bottom layer film A, plating sol B on the bottom layer film A to serve as an upper layer film B, fully immersing the substrate in the sol A or sol B, maintaining for a period of time after full immersion, extracting, airing at room temperature, and drying in an oven to obtain the A/B double-layer silicon dioxide antireflection film;
in the fourth step, the reflux condensing time is 10h, and the mixing volume ratio of sol C to sol D is 1:4;
when preparing the 6-layer silicon dioxide antireflection film, preparing a bottom film A and an upper film B according to the method of the step five, and repeatedly superposing the bottom film A and the upper film B in a mode of A/B/A/B/A/B at the same pulling speed;
in the third step, the volume ratio of the absolute ethyl alcohol, the ammonia water, the deionized water, the hexamethyldisilazane and the tetraethoxysilane is 110:0.6:2.5:1:10, the stirring temperature is 40 ℃, the stirring time is 12 hours, and the aging time is 24 hours.
2. The method of preparing an anti-reflection film according to claim 1, wherein in the first step, the volume ratio of ethyl orthosilicate, absolute ethyl alcohol and ammonia water is 13:130:5, the stirring temperature is 40 ℃, the stirring time is 12h, and the aging time is 24h.
3. The method of claim 1, wherein in the second step, the volume ratio of ethyl orthosilicate, absolute ethyl alcohol, deionized water and concentrated hydrochloric acid is 11:110:4:0.02, the stirring temperature is 40 ℃, the stirring time is 12h, and the aging time is 24h.
4. The method for preparing a silica anti-reflection film according to claim 1, wherein in the fifth step, the pulling speed is 80mm/min, and the maintenance time after complete immersion is 5-10 s.
5. Use of a method for producing a silica antireflection film as claimed in any one of claims 1 to 4 for transmitting broad spectrum light having center wavelengths of 351nm, 527nm, 1053nm, 1064nm, respectively.
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| CN108761581B (en) * | 2018-05-25 | 2020-05-12 | 中国工程物理研究院激光聚变研究中心 | SiO with adjustable refractive index2Preparation method of antireflection film |
| CN108623185B (en) * | 2018-05-25 | 2021-11-23 | 中国工程物理研究院激光聚变研究中心 | Double-layer composite SiO2Preparation method of antireflection film |
| CN113387596A (en) * | 2021-08-02 | 2021-09-14 | 凯盛晶华玻璃有限公司 | Wear-resistant super-hydrophobic photovoltaic glass and preparation method thereof |
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