CN108424537B - Ultraviolet curing film with adjustable refractive index and preparation method thereof - Google Patents
Ultraviolet curing film with adjustable refractive index and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 claims abstract description 13
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 11
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 125000005395 methacrylic acid group Chemical group 0.000 claims abstract description 7
- 238000001338 self-assembly Methods 0.000 claims abstract description 6
- 230000001678 irradiating effect Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims 1
- 238000006068 polycondensation reaction Methods 0.000 description 6
- 230000003301 hydrolyzing effect Effects 0.000 description 5
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 239000005350 fused silica glass Substances 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- AHGFXGSMYLFWEC-UHFFFAOYSA-N [SiH4].CC(=C)C(O)=O Chemical compound [SiH4].CC(=C)C(O)=O AHGFXGSMYLFWEC-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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Abstract
The invention provides a refractive index adjustableThe ultraviolet curing film and the preparation method thereof comprise the following steps: mixing ethyl orthosilicate, deionized water and an organic solvent, reacting at 8-12 ℃ for 12-24h to prepare oligomer, aging at 45-55 ℃ for 48-72h, and preparing SiO by self-assembly of oligomer clusters2A porous ball; (2) mixing methacrylic silane, deionized water and an organic solvent, reacting at 110-130 ℃ for 6-8h to obtain an oligomer, and adding a photoinitiator to prepare an ultraviolet-curable sol; (3) mixing SiO2Mixing the porous balls and the ultraviolet-curable sol to prepare a film to be cured; (4) and irradiating the film to be cured under ultraviolet rays to prepare the ultraviolet curing film with the adjustable refractive index. The film prepared by the invention has wider refractive index regulation range and high laser damage resistance, and can realize high-energy laser output of a strong laser device.
Description
Technical Field
The invention belongs to the technical field of optical materials, and particularly relates to an ultraviolet curing film with an adjustable refractive index and a preparation method thereof.
Background
The refractive index adjustable film can realize ultrahigh transmittance (higher than 99.5%) aiming at electromagnetic waves with different wavelengths, and has huge application requirements in the fields of intense laser devices, solar cells and the like. The preparation of the film can be rapidly realized by adopting an ultraviolet curing mode, and the preparation efficiency is greatly improved.
SiO2The antireflection film is an optical material with wide application, and has good optical characteristics, mechanical properties and chemical stability. SiO produced by PVD methods2Although the antireflection film system can realize refractive index regulation, the antireflection film system cannot meet the high-energy transmission requirement in a strong laser device; the sol-gel film with adjustable refractive index prepared by the template method has the risk of structural collapse (when the template agent is removed).
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the ultraviolet curing film with the adjustable refractive index and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
an ultraviolet curing film with adjustable refractive index is prepared by the following steps:
(1) mixing ethyl orthosilicate, deionized water and an organic solvent uniformly according to a molar ratio of 0.8-1.2:2.5-3.5:8-12, reacting at 8-12 ℃ for 12-24h to obtain an oligomer, aging at 45-55 ℃ for 48-72h, and preparing SiO by self-assembly of the oligomer into clusters2A porous ball;
(2) uniformly mixing methacrylic silane, deionized water and an organic solvent according to a molar ratio of 0.8-1.2:4-6:8-12, reacting at 110-130 ℃ for 6-8h to obtain an oligomer, adding a photoinitiator accounting for 3-5% of the total mass of the system, and uniformly stirring to obtain an ultraviolet-curable sol;
(3) mixing SiO2The porous ball and the ultraviolet curable sol are mixed according to the mass ratio of 10-30:1, mixing, coating the mixture on a substrate by adopting a rotary coating method, and homogenizing at the rotating speed of 800-;
(4) the film to be cured obtained in the step (3) is at 1.5-2.5W/cm2The ultraviolet curing film with the adjustable refractive index is prepared by irradiating for 110-130 seconds under the ultraviolet irradiation intensity.
Further, the organic solvent in step (1) and step (2) is at least one of ethanol, decane and acetone.
Further, the molar ratio of the ethyl orthosilicate, the deionized water and the organic solvent in the step (1) is 1:3: 10.
Further, in the step (1), the reaction is carried out for 18h at 10 ℃ and then aged for 60h at 50 ℃.
Further, the molar ratio of the methacrylic acid silane to the deionized water to the organic solvent in the step (2) is 1:5: 10. Further, in step (2), the reaction was carried out at 120 ℃ for 7 hours.
Further, the photoinitiator added in the step (2) is TPO, and the adding amount is 4% of the total mass of the system.
Further, SiO in step (3)2The mass ratio of the porous spheres to the ultraviolet curable sol was 30: 1.
Further, the ultraviolet irradiation intensity in the step (4) is 2W/cm2The irradiation time was 120 s.
The ultraviolet curing film with the adjustable refractive index and the preparation method thereof provided by the invention have the following beneficial effects:
(1) the film provided by the invention has a wider refractive index regulation range, the refractive index of the compact ultraviolet curing sol-gel film is 1.5, and the compact ultraviolet curing sol-gel film is prepared by SiO2After the porous spheres are filled, the porosity can be effectively introduced, and the refractive index of the film is continuously reduced to 1.36 by filling air.
(2) The film provided by the invention has high laser damage resistance, and due to the porous structure, the film can generate certain energy relaxation and release when being bombarded by strong laser, and compared with the film prepared by a PVD method, the film provided by the invention can better embody excellent laser damage resistance.
(3) The film provided by the invention can simultaneously realize the transmittance of 1053nm and 527nm higher than 99.5 percent, so that after the refractive index of the film is adjusted to a required value, the film is assisted with a layer of antireflection film to realize the ultrahigh transmittance of 1053nm and 527nm, and the high-energy laser output of a strong laser device can be realized.
Drawings
FIG. 1 shows the refractive index and SiO ratio of UV-cured films with tunable refractive index prepared in examples 1-32Proportional graph of porous ball.
FIG. 2 is a graph showing the results of laser damage threshold of UV-cured films with tunable refractive indices prepared in examples 1-3.
Detailed Description
Example 1
An ultraviolet curing film with adjustable refractive index is prepared by the following steps:
(1) uniformly mixing ethyl orthosilicate, deionized water and ethanol according to the molar ratio of 1:3:10, then reacting for 18 hours at 10 ℃ according to the principle of silane hydrolytic polycondensation reaction to obtain oligomer, continuing aging for 60 hours at 50 ℃, and preparing SiO by self-assembly cluster of the oligomer2A porous ball;
(2) uniformly mixing methacrylic silane, deionized water and ethanol according to the molar ratio of 1:5:10, then reacting for 7 hours at 120 ℃ according to the principle of silane hydrolytic polycondensation to obtain an oligomer, adding a photoinitiator TPO accounting for 4% of the total mass of a reaction system, and uniformly stirring to obtain an ultraviolet-curable sol;
(3) mixing UV-curable sol and SiO2The porous ball is prepared from the following components in a mass ratio of 1: 10, uniformly mixing, coating the mixture on a fused quartz substrate by adopting a rotary coating method, and preparing a film to be cured by adopting parameters of the rotating speed of 1000rpm and the glue homogenizing time of 2.5 min;
(4) the film to be solidified is at 2W/cm2Irradiating for 120s under the ultraviolet irradiation intensity to prepare the ultraviolet curing film with adjustable refractive index.
The above films were tested to obtain: the refractive index of the film layer is 1.47, and the hardness is 0.36 GPa.
Example 2
An ultraviolet curing film with adjustable refractive index is prepared by the following steps:
(1) uniformly mixing ethyl orthosilicate, deionized water and acetone according to a molar ratio of 0.8:2.5:8, then reacting for 24 hours at 8 ℃ according to a silane hydrolytic polycondensation reaction principle to obtain an oligomer, aging for 72 hours at 45 ℃, and preparing SiO by self-assembly of the oligomer2A porous ball;
(2) uniformly mixing methacrylic silane, deionized water and acetone according to a molar ratio of 0.8:4:8, then reacting for 8 hours at 110 ℃ according to a silane hydrolysis polycondensation reaction principle to obtain an oligomer, adding a photoinitiator TPO accounting for 5% of the total mass of a reaction system, and uniformly stirring to obtain an ultraviolet curable sol;
(3) mixing UV-curable sol and SiO2The porous ball is prepared from the following components in a mass ratio of 1: 20, uniformly mixing, coating the mixture on a fused quartz substrate by adopting a rotary coating method, and preparing a film to be cured by adopting parameters of the rotating speed of 800rpm and the glue homogenizing time of 3 min;
(4) the film to be cured is at 1.5W/cm2Irradiating for 130s under the ultraviolet irradiation intensity to prepare the ultraviolet curing film with adjustable refractive index.
The above films were tested to obtain: the refractive index of the film layer is 1.41, and the hardness is 0.35 GPa.
Example 3
An ultraviolet curing film with adjustable refractive index is prepared by the following steps:
(1) uniformly mixing ethyl orthosilicate, deionized water and decane according to the mol ratio of 1.2:3.5:12, then reacting for 12 hours at the temperature of 12 ℃ according to the principle of silane hydrolytic polycondensation reaction to obtain oligomer, aging for 48 hours at the temperature of 55 ℃, and preparing SiO by self-assembly clustering of the oligomer2A porous ball;
(2) uniformly mixing methacrylic silane, deionized water and decane according to the molar ratio of 1.2:6:12, then reacting for 6 hours at 130 ℃ according to the principle of silane hydrolytic polycondensation reaction to obtain an oligomer, adding a photoinitiator TPO accounting for 3% of the total mass of the reaction system, and uniformly stirring to obtain the ultraviolet curable sol;
(3) mixing UV-curable sol and SiO2The porous ball is prepared from the following components in a mass ratio of 1: 30, coating the mixture on a fused quartz substrate by adopting a rotary coating method after the mixture is uniformly mixed, and preparing a film to be cured by adopting parameters of the rotating speed of 1200rpm and the glue homogenizing time of 2 min;
(4) the film to be cured is at 2.5W/cm2Irradiating for 110s under the ultraviolet irradiation intensity to prepare the ultraviolet curing film with adjustable refractive index.
The above films were tested to obtain: the refractive index of the film layer is 1.36, and the hardness is 0.32 GPa.
Refractive index and SiO of the UV-curable films with tunable refractive indices prepared in examples 1-3 above2The proportional relationship of the porous spheres is shown in fig. 1, and the laser damage threshold results are shown in fig. 2.
As can be seen from FIG. 1, SiO2When the content of the porous spheres is different, the refractive indexes of the films are different, and the refractive index of the film is along with that of SiO2The filling amount of the porous ball is increased and reduced when the UV-curable sol and the SiO2The porous ball is prepared from the following components in a mass ratio of 1: 30, the film refractive index dropped to 1.36.
As can be seen from FIG. 2, the laser damage thresholds of the films obtained in examples 1 to 3 were 58.1J/cm, respectively2@1053nm (5nsequiv) (i.e., 1. omega., 5ns equiv), 56.0J/cm2@1053nm (5ns equiv) (i.e., 1. omega., 5ns equiv), 55.2J/cm2@1053nm (5ns equiv) (i.e., 1. omega., 5ns equiv) and 50.9J/cm2@527nm (5ns equiv) (i.e., 2 ω, 5 nseequiv), 55.4J/cm2@527nm (5ns equiv) (i.e., 2 ω, 5ns equiv), 52.3J/cm2@527nm (5ns equiv) (i.e., 2 ω, 5ns equiv).
Comparative example
The PVD method is adopted to prepare the film, and specifically comprises the following steps: SiO with the purity of 99.99 percent is adopted2As a sputtering source target, the sputtering source target is used under a vacuum degree of 1X 10-4Pa, argon flow of 250sccm, substrate temperature of 400 ℃, bias voltage of 100V and sputtering time of 1 hour to prepare SiO with thickness of about 150nm 23 film samples with laser damage threshold of 32J/cm2@1053nm (5ns equiv) (i.e., 1. omega., 5ns equiv), 35J/cm2@1053nm (5ns equiv) (i.e., 1. omega., 5 nseequiv), 36J/cm2@1053nm (5ns equiv) (i.e., 1 ω, 5ns equiv) and 26J/cm2@527nm (5ns equiv) (i.e., 2 ω, 5ns equiv), 28J/cm2@527nm (5ns equiv) (i.e., 1 ω, 5ns equiv), 29J/cm2@527nm (5nsequiv) (i.e., 1 ω, 5ns equiv).
Compared with the film prepared by adopting a PVD method, the film prepared by the invention can better show excellent laser damage resistance.
Claims (10)
1. A preparation method of an ultraviolet curing film with adjustable refractive index is characterized by comprising the following steps:
(1) mixing ethyl orthosilicate, deionized water and an organic solvent uniformly according to a molar ratio of 0.8-1.2:2.5-3.5:8-12, reacting at 8-12 ℃ for 12-24h to obtain an oligomer, aging at 45-55 ℃ for 48-72h, and preparing SiO by self-assembly of the oligomer into clusters2A porous ball; the organic solvent is at least one of decane and acetone;
(2) uniformly mixing methacrylic silane, deionized water and an organic solvent according to a molar ratio of 0.8-1.2:4-6:8-12, reacting at 110-130 ℃ for 6-8h to obtain an oligomer, adding a photoinitiator accounting for 3-5% of the total mass of the system, and uniformly stirring to obtain an ultraviolet-curable sol;
(3) mixing SiO2Mixing the porous ball and the ultraviolet-curable sol according to the mass ratio of 10-30:1, coating the mixture on a substrate by adopting a rotary coating method, and homogenizing at the rotating speed of 800-;
(4) the film to be cured obtained in the step (3) is at 1.5-2.5W/cm2The ultraviolet curing film with the adjustable refractive index is prepared by irradiating for 110-130 seconds under the ultraviolet irradiation intensity.
2. The method for preparing the ultraviolet curing film with the adjustable refractive index according to claim 1, wherein the organic solvent in the step (2) is at least one of ethanol, decane and acetone.
3. The method for preparing the ultraviolet curing film with the adjustable refractive index according to claim 1, wherein the molar ratio of the ethyl orthosilicate, the deionized water and the organic solvent in the step (1) is 1:3: 10.
4. The method for preparing UV curable film with tunable refractive index according to claim 1, wherein in step (1), the reaction is performed at 10 ℃ for 18h, and then the aging is performed at 50 ℃ for 60 h.
5. The method for preparing the ultraviolet curing film with the adjustable refractive index as claimed in claim 1, wherein the molar ratio of the methacrylic silane, the deionized water and the organic solvent in the step (2) is 1:5: 10.
6. The method for preparing UV-curable film with adjustable refractive index according to claim 1, wherein the reaction in step (2) is carried out at 120 ℃ for 7 hours.
7. The method for preparing UV-curable film with adjustable refractive index according to claim 1, wherein the photoinitiator added in step (2) is TPO, and the addition amount is 4% of the total mass of the system.
8. The method for preparing UV-curable film with adjustable refractive index according to claim 1, wherein SiO in step (3)2The mass ratio of the porous spheres to the ultraviolet curable sol was 30: 1.
9. The method for preparing UV-curable film with adjustable refractive index according to claim 1, wherein the UV irradiation intensity in step (4) is 2W/cm2The irradiation time was 120 s.
10. The UV-curable film with adjustable refractive index prepared by the method according to any one of claims 1 to 9.
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| CN110734561B (en) * | 2019-10-28 | 2022-02-11 | 中国工程物理研究院激光聚变研究中心 | Frequency doubling element matching film of intense laser device and preparation method thereof |
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