CN110698673B - Frequency doubling element matching film of high-mechanical-strength strong laser device and preparation method thereof - Google Patents
Frequency doubling element matching film of high-mechanical-strength strong laser device and preparation method thereof Download PDFInfo
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- CN110698673B CN110698673B CN201911031025.7A CN201911031025A CN110698673B CN 110698673 B CN110698673 B CN 110698673B CN 201911031025 A CN201911031025 A CN 201911031025A CN 110698673 B CN110698673 B CN 110698673B
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Abstract
The invention discloses a frequency doubling element matching film of a high-mechanical-strength strong laser device and a preparation method thereof, belonging to the technical field of optical materials. Which comprises the following steps: mixing methyl triethoxysilane, ethyl orthosilicate, deionized water and an organic solvent, and stirring for reaction under heating to obtain an oligomer sol; mixing the oligomer sol with an organic solvent to prepare a coating sol; coating the coating sol on a substrate to prepare a film to be cured; and carrying out heat treatment on the film to be cured to obtain the matched film. The matching film prepared by the invention has higher curing strength and higher height and better mechanical property.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to a frequency doubling element matching film of a high-mechanical-strength laser device and a preparation method thereof.
Background
Optical elements in the intense laser device need to be coated with a special antireflection film layer to realize high-energy transmission of laser, wherein the emergent surface of the frequency doubling element needs to simultaneously realize high antireflection aiming at 527nm and 1053 nm. To realize high anti-reflection and frequency doubling of dual wavelengthTwo layers of films with specific refractive indexes and film thicknesses, namely a matching film and an antireflection film, are respectively prepared on the emergent surface of the element. SiO 22The antireflection film is an optical material with wide application, has good optical characteristics, laser damage resistance and chemical stability, and is a preferred material for preparing strong laser films.
The matching film prepared by the current universal single siloxane polycondensation method has longer post-treatment time and lower mechanical property of the film, and limits the manufacturing efficiency and the service life of frequency doubling elements of strong laser devices.
Disclosure of Invention
The invention aims to provide a frequency doubling element matching film of a high-mechanical-strength strong laser device and a preparation method thereof, and aims to solve the problems that the post-treatment time of a matching film layer prepared by the existing single siloxane polycondensation method is long, and the mechanical property of the film layer is low.
The technical scheme for solving the technical problems is as follows:
a preparation method of a frequency doubling element matching film of a high-mechanical-strength strong laser device comprises the following steps:
(1) mixing methyl triethoxysilane, ethyl orthosilicate, deionized water and an organic solvent, and stirring for reaction under heating to obtain an oligomer sol;
(2) mixing the oligomer sol with an organic solvent to prepare a coating sol;
(3) coating the coating sol on a substrate to prepare a film to be cured;
(4) and carrying out heat treatment on the film to be cured to obtain the matched film.
Further, in a preferred embodiment of the present invention, the molar ratio of methyltriethoxysilane, ethyl orthosilicate, deionized water and organic solvent in the step (1) is 1: (0.1-1): (2-6): 2.
further, in a preferred embodiment of the present invention, the organic solvent in the step (1) is one or more of ethanol, methanol and acetone.
Further, in a preferred embodiment of the present invention, the reaction conditions in the step (1) are as follows: reacting for 30-50h at 80-100 ℃.
Further, in a preferred embodiment of the present invention, in the step (2), the mass ratio of the oligomer sol to the organic solvent is 1: (1-3).
Further, in a preferred embodiment of the present invention, the organic solvent in the step (2) is one or more of butanol, heptane and decane.
Further, in a preferred embodiment of the present invention, the step (3) specifically comprises the following steps: coating the coating sol on a KDP substrate by adopting a rotary coating method, and homogenizing for 40-80s at the rotating speed of 700 r/min.
Further, in a preferred embodiment of the present invention, the heat treatment step in the step (4): the treatment is carried out for 1-3h at the temperature of 120-140 ℃.
The frequency doubling element matching film of the high-mechanical-strength laser device is prepared by the preparation method of the frequency doubling element matching film of the high-mechanical-strength laser device.
The invention has the following beneficial effects:
1. the invention adopts methyl triethoxysilane as raw material and ethyl orthosilicate as coupling agent. The ethyl orthosilicate has four active functional groups, and more than three active functional groups of the methyl triethoxysilane, so the ethyl orthosilicate has better chemical activity than the methyl triethoxysilane, and the introduction of the ethyl orthosilicate can accelerate the whole condensation reaction process and prepare oligomer sol more efficiently. In addition, because the ethyl orthosilicate has multi-active functional groups, the probability of cross-linking reaction in the condensation process is increased without adding a catalyst, the cross-linking degree among oligomers is improved, and the internal combination is enhanced under the condition of still keeping the form of short-chain oligomers, so that the mechanical strength of the film layer is improved, and the matched film with higher curing strength and higher height and better mechanical property is obtained.
2. In the preparation method, under the premise of not adding a catalyst, the hydrolysis condensation reaction of methyltriethoxysilane containing multiple active groups, ethyl orthosilicate and water can be promoted at the temperature of 80-100 ℃, residual moisture and organic solvent in the reaction can be evaporated and removed, and the low polymer sol with higher purity can be obtained, so that the low polymer sol can be cured at lower temperature in a shorter time, and the preparation efficiency of the film layer can be improved.
3. In the preparation method, heat treatment is carried out at the temperature of 120-140 ℃, reaction raw materials and a coupling agent can be fully crosslinked and cured at the temperature, the crystal phase structure of KDP crystals cannot be damaged, the application of the method on a temperature-sensitive substrate can be influenced if the baking temperature is too high, and the film layer curing cannot be realized if the temperature is too low.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph showing the results of laser damage threshold at 1053nm for matching films prepared in examples 1-3 of the present invention and comparative examples 1-2;
FIG. 2 is a graph showing the change of hardness with time in the post-treatment process at the same temperature for the matching films obtained in examples 1 to 3 of the present invention and comparative examples 1 to 2.
Detailed Description
The principles and features of the present invention are described below in conjunction with the embodiments and the accompanying drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
the preparation method of the frequency doubling element matching film of the high-mechanical-strength strong laser device comprises the following steps:
(1) adding 30mol of methyltriethoxysilane, 3mol of ethyl orthosilicate and 60mol of methanol into a reaction kettle, heating to 80 ℃ in an oil bath, and then mixing the components according to a molar ratio of 1: 0.1: 2: 2, adding 60mol of deionized water, and stirring for reaction for 50 hours to obtain oligomer sol;
(2) mixing the oligomer sol and butanol according to a mass ratio of 1: 1, mixing and diluting to prepare coating sol;
(3) coating the coating sol on a KDP substrate by adopting a rotary coating method, and homogenizing for 40s at the rotating speed of 700 r/min;
(4) and carrying out heat treatment on the film to be cured at 140 ℃ for 3h to obtain a matched film.
The matching film prepared in this example was marked as # 1 matching film, and its laser damage threshold was tested. And calculating parameters required by the matched antireflection film by using software according to the refractive index of the 1# matching film, preparing the parameters on the matching film, and testing the residual reflectivity of the whole film system at 1053nm and 527 nm.
Example 2:
the preparation method of the frequency doubling element matching film of the high-mechanical-strength strong laser device comprises the following steps:
(1) adding 30mol of methyltriethoxysilane, 15mol of ethyl orthosilicate and 60mol of ethanol into a reaction kettle, heating to 90 ℃ in an oil bath, and then adding a solvent according to a molar ratio of 1: 0.5: 2: 4, adding 120mol of deionized water, and stirring for reacting for 40 hours to obtain oligomer sol;
(2) mixing the oligomer sol and heptane according to the mass ratio of 1:2, mixing and diluting to prepare coating sol;
(3) coating the coating sol on a KDP substrate by adopting a rotary coating method, and homogenizing for 60s at the rotating speed of 700 r/min;
(4) and carrying out heat treatment on the film to be cured at 120 ℃ for 2h to obtain a matched film.
The matching film prepared in this example was marked as # 2 matching film and its laser damage threshold was tested. And calculating parameters required by the matched antireflection film by using software according to the refractive index of the 2# matching film, preparing the parameters on the matching film, and testing the residual reflectivity of the whole film system at 1053nm and 527 nm.
Example 3:
the preparation method of the frequency doubling element matching film of the high-mechanical-strength strong laser device comprises the following steps:
(1) adding 30mol of methyltriethoxysilane, 30mol of ethyl orthosilicate and 60mol of acetone into a reaction kettle, heating the mixture to 100 ℃ in an oil bath, and then mixing the mixture according to a molar ratio of 1: 1: 2: 6, adding 180mol of deionized water, and stirring for reaction for 30 hours to obtain oligomer sol;
(2) and (3) mixing the oligomer sol and decane according to the mass ratio of 1: 3 mixing and diluting to prepare coating sol;
(3) coating the coating sol on a KDP substrate by adopting a rotary coating method, and homogenizing for 80s at the rotating speed of 700 r/min;
(4) and carrying out heat treatment on the film to be cured at 130 ℃ for 1h to prepare a matching film.
The matching film prepared in this example was marked as # 3 matching film and its laser damage threshold was tested. And calculating parameters required by the matched antireflection film by software according to the refractive index of the 3# matching film, preparing the parameters on the matching film, and testing the residual reflectivity of the whole film system at 1053nm and 527 nm.
Comparative example 1
In the preparation method of the matching film of the comparative example, no ethyl orthosilicate was added, and the preparation method was as follows:
(1) adding 30mol of methyltriethoxysilane and 60mol of ethanol into a reaction kettle, heating to 90 ℃ in an oil bath, adding 90mol of deionized water, and reacting for 50 hours to obtain oligomer sol;
(2) diluting the prepared oligomer sol with heptane according to the mass ratio of 1: 2;
(3) coating the film on a substrate by adopting a rotary coating method, and homogenizing the film for 60s at the rotating speed of 700r/min to obtain a film to be cured;
(4) and carrying out heat treatment on the film to be cured in a 120 ℃ oven for 5h to obtain the matching film.
The matching film prepared in this comparative example was marked as # 4 matching film, and the laser damage threshold thereof was tested. And calculating parameters required by the matched antireflection film by using software according to the refractive index of the 4# matching film, preparing the parameters on the matching film, and testing the residual reflectivity of the whole film system at 1053nm and 527 nm.
Comparative example 2
In the preparation method of the matching film of the comparative example, ethyl orthosilicate is added in the later stage of the synthesis reaction of methyl triethoxysilane and water, and the preparation method is as follows:
(1) 30mol of methyltriethoxysilane and 60mol of ethanol are added into a reaction kettle, oil bath heating is carried out to 90 ℃, and then 90mol of deionized water is added for reaction. After reacting for 45 hours, adding 3mol of ethyl orthosilicate, and continuing to react for 5 hours to obtain oligomer sol;
(2) mixing the prepared oligomer sol with heptane according to the mass ratio of 1:2, diluting;
(3) coating the film on a substrate by adopting a rotary coating method, and homogenizing the film for 60s at the rotating speed of 700r/min to obtain a film to be cured;
(4) and carrying out heat treatment on the film to be cured for 5 hours at 120 ℃ in an oven to obtain the matching film.
The matching film prepared in this comparative example was marked as # 5 matching film, and the laser damage threshold thereof was tested. And calculating parameters required by the matched antireflection film by using software according to the refractive index of the 5# matching film, preparing the parameters on the matching film, and testing the residual reflectivity of the whole film system at 1053nm and 527 nm.
The 1# -3# matching film of the example and the 4# -5# matching film of the comparative example were tested for laser damage threshold, and the results are shown in fig. 1.
As can be seen from FIG. 1, the laser damage thresholds of the films prepared in examples 1-3 at 1053nm were 57.26J/cm2(5ns equiv), 61.40J/cm2(5ns equiv) and 69.07J/cm2(5ns equiv), respectively, and the laser damage thresholds of the films prepared in comparative examples 1-2 at 1053nm were 47.26J/cm2(5ns equiv) and 53.94J/cm2(5ns equiv), respectively, which are higher than the requirement of 30J/cm2(5ns equiv), respectively, indicating that several film layers have excellent laser damage resistance.
As can be seen from fig. 2, the hardness of the frequency doubling element matching films prepared in examples 1 to 3 is 239.08MPa, 266.51MPa and 309.65MPa, the hardness of the frequency doubling element matching films prepared in comparative examples 1 to 2 is 44.23MPa and 41.79MPa, and the mechanical strength of the films prepared in examples 1 to 3 is significantly improved. The hardness of the film layer of the matching film prepared in the embodiment 1-3 basically does not change obviously after being subjected to post-treatment for 2 hours, which shows that the curing of the film layer is completed, while the hardness of the film layer prepared in the comparative example 1-2 is slowly increased within 5 hours, and the curing of the surface film layer is not complete, so that the efficiency of the film layer preparation method provided by the invention is obviously improved.
The parameters required by the anti-reflection film matched with the refractive indexes of the matching films of the embodiment and the comparison example are calculated by software, the matching films are prepared on the matching films, and the residual reflectivity of the whole film system at 1053nm and 527nm is tested, and the results are shown in table 1.
TABLE 1
The residual reflectances of the film systems obtained in examples 1 to 3 and those of the film systems obtained in comparative examples 1 to 2 were each less than 1%, indicating that the film layers had excellent antireflection effects at 1053nm and 527 nm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of a frequency doubling element matching film of a high-mechanical-strength strong laser device is characterized by comprising the following steps:
(1) mixing methyl triethoxysilane, ethyl orthosilicate, deionized water and an organic solvent, and stirring for reaction under heating to obtain an oligomer sol;
(2) mixing the oligomer sol with an organic solvent to prepare a coating sol;
(3) coating the coating sol on a substrate to prepare a film to be cured;
(4) carrying out heat treatment on the film to be cured to prepare the matching film;
wherein the molar ratio of the methyltriethoxysilane to the ethyl orthosilicate in the step (1) to the deionized water to the organic solvent is 1: (0.1-1): (2-6): 2; the reaction conditions in the step (1) are as follows: reacting for 30-50h at 80-100 ℃.
2. The method for preparing the matching film of the frequency doubling element of the high mechanical strength strong laser device according to claim 1, wherein the organic solvent in step (1) is one or more of ethanol, methanol and acetone.
3. The method for preparing the matching film of the frequency doubling element of the high mechanical strength strong laser device according to claim 1, wherein the mass ratio of the oligomer sol to the organic solvent in the step (2) is 1: (1-3).
4. The method for preparing the matching film of the frequency doubling element of a high mechanical strength laser device according to claim 3, wherein the organic solvent in the step (2) is one or more of butanol, heptane and decane.
5. The method for preparing the matching film of the frequency doubling element of the high mechanical strength laser device according to any one of claims 1 to 4, wherein the step (3) comprises the following steps: and coating the coating sol on a KDP substrate by adopting a rotary coating method, and homogenizing for 40-80s at the rotating speed of 700 r/min.
6. The method for preparing the matching film of the frequency doubling element of the high mechanical strength strong laser device according to claim 5, wherein the heat treatment step in the step (4): the treatment is carried out for 1-3h at the temperature of 120-140 ℃.
7. The matching film of frequency doubling element of high mechanical strength laser device prepared by the method for preparing the matching film of frequency doubling element of high mechanical strength laser device according to any one of claims 1 to 6.
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| US7695781B2 (en) * | 2004-02-16 | 2010-04-13 | Fujifilm Corporation | Antireflective film, polarizing plate including the same, image display unit including the same and method for producing antireflective film |
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