CN114351098A - Broadband high-transmittance single-layer AlF3Preparation method of antireflection film - Google Patents
Broadband high-transmittance single-layer AlF3Preparation method of antireflection film Download PDFInfo
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- CN114351098A CN114351098A CN202011089057.5A CN202011089057A CN114351098A CN 114351098 A CN114351098 A CN 114351098A CN 202011089057 A CN202011089057 A CN 202011089057A CN 114351098 A CN114351098 A CN 114351098A
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Abstract
The invention belongs to the technical field of optical films and discloses an AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps: SF6/Ar2Setting a gas flow ratio, setting sputtering working pressure and setting radio frequency power supply power; the invention uses AlF3As a target, Ar2As working gas, SF6As the reaction gas, the gas is sufficiently mixed by using a gas path mixing device of the instrument, and SF is adjusted during sputtering6/Ar2Gas flow ratio, improved deposited AlF3Problems of F-starved defects in films by adjusting operating pressure and radio frequencyPower of power supply makes AlF3The stoichiometric ratio of the film F to the film Al is close to the normal stoichiometric ratio of 3 to 1, the refractive index of the film is reduced, and the transmittance of the coated glass is improved. AlF prepared by adopting the technical scheme3The antireflection film can be applied to optical devices, and is simple in preparation process and low in cost.
Description
Technical Field
The invention belongs to the technical field of optical films, and particularly relates to high-purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3A method of antireflection coating.
Background
Solar cells can convert inexhaustible light energy into electrical energy, and are often used as components of satellites, launch vehicles, terrestrial solar generators, and the like. And the glass cover plate is used as a solar cellThe solar cell module is directly contacted with the external environment, plays roles of wind prevention, rain prevention, dust prevention and the like, and can directly influence the transmittance of sunlight so as to influence the photoelectric conversion efficiency of the cell. Therefore, cover glasses for photovoltaic devices should have a higher transmittance in the solar radiation spectrum to convert more incident light into photocurrent. However, due to the difference in refractive index between air and the glass substrate, there is fresnel reflection loss of incident light at the surface of the glass substrate, which may reduce the photoelectric conversion efficiency of the solar cell. For example, when quartz glass is used as a cover sheet of a solar cell, since the refractive indices of air and glass are different, the average transmittance of the glass is 93.2%, and there is a reflection loss of 6.8% of incident light on the surface of the glass substrate, which limits the photoelectric conversion efficiency of the solar cell. According to the principle of light interference, one or more layers of optical films are plated on a glass substrate, so that the reflection loss of incident light can be reduced, the transmittance of light is increased, and the photoelectric conversion efficiency of the solar cell is further increased. Aluminum fluoride (AlF)3) Has a low refractive index, and is widely used as an antireflection film, a laser device, a space solar cell, an optical device, and the like. Preparation of AlF3There are many methods for antireflection film, including vacuum evaporation, sol-gel, magnetron sputtering, surface microstructure, acid etching, and the like. The film prepared by the magnetron sputtering method is compact, the binding force between the film and the substrate is strong, the operation process is simple, and the repeatability is good; however, it is difficult to control the deposition of films of normal stoichiometry when sputtering compound targets. And the magnetron sputtering method is used for preparing AlF3When the film is used, obvious F-poor defects can occur, and the optical performance of the film is seriously influenced.
Aiming at the technical problem, the invention provides an AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3A method of antireflection coating.
Disclosure of Invention
The invention aims to provide AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3Method of antireflection film, with SF6As a reaction gas, with Ar2As working gas, the gas is fully mixed by using a gas path mixing device of an instrument so as to overcome the defect of preparing AlF by a magnetron sputtering method3F-poor defects of the film, and the atomic ratio of F/Al is close to the ideal stoichiometric ratio of 3: 1 by adjusting the working gas pressure and the sputtering power, so that the prepared AlF3The transmittance of the film coated glass is improved by 1-3 percentage points, and the preparation method is simple and easy to control.
With AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) as a reaction gas, the total gas flow rate at the time of sputtering was set to 40sccm to 80sccm, and SF was added6/Ar2The gas flow ratio is set to be 0.1-20%;
(2) setting the working pressure of the reaction chamber: setting the working pressure of the reaction chamber to 0.1Pa-6.0Pa
(3) Setting the power of a radio frequency power supply: the power sputtering power is set to be 30W-400W;
the invention adjusts SF in sputtering6/Ar2Gas flow ratio, improved deposited AlF3F-poor defect in the film, and AlF is enabled by adjusting the power of the radio frequency power supply and the working pressure of the reaction chamber3The stoichiometric ratio of the film F to the film Al is close to the normal stoichiometric ratio of 3 to 1, the refractive index of the film is reduced, and the transmittance of the coated glass is improved.
The invention has the beneficial effects that the magnetron sputtering method is used for depositing the AlF on the glass substrate3Film by adjusting SF in sputtering6/Ar2Gas flow ratio, overcomes the defect of preparing AlF by a magnetron sputtering method3Adjusting the power of the radio frequency power supply and the working pressure of the reaction chamber to ensure that the AlF is caused by the F-poor defect of the film3The ratio of F to Al on the surface of the film is close to the normal stoichiometric ratio of 3 to 1, and AlF is in the wavelength range of 300-3The average transmittance of the coated glass reaches 94.06 percent, which is compared with the transmittance of the uncoated glass (93 percent)14%), an improvement of 0.92%. AlF prepared by adopting the technical scheme3The film has higher average transmittance (94.06%) in the wavelength range of 300-1100nm, and the light transmittance is remarkably improved.
Drawings
FIG. 1 is a drawing of examples of the present invention providing AlF prepared under each example3Refractive index profile of the film in the wavelength range of 300-1100 nm.
FIG. 2 is a schematic representation of AlF prepared under examples of the invention3The transmittance spectra of the coated glass and the uncoated glass in the wavelength range of 300-1100 nm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
With high purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) As a reaction gas, the total gas flow rate during sputtering was set to 40sccm, and SF was added6/Ar2The gas flow ratio was set to 0.1%;
(2) setting the working pressure of the reaction chamber: setting the working air pressure of the vacuum chamber to be 0.1 Pa;
(3) setting the power of a radio frequency power supply: the power sputtering power is set to be 30W;
example two
With high purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) As a reaction gas, the total gas flow rate at the time of sputtering was set to 50sccm, and SF was added6/Ar2The gas flow ratio is set to 5%;
(2) setting the working pressure of the reaction chamber: setting the working air pressure of the vacuum chamber to be 1.5 Pa;
(3) setting the power of a radio frequency power supply: the power sputtering power is set to be 100W;
EXAMPLE III
With high purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) As a reaction gas, the total gas flow rate during sputtering was set to 60sccm, and SF was added6/Ar2The gas flow ratio is set to 10%;
(2) setting the working pressure of the reaction chamber: setting the working air pressure of the vacuum chamber to be 3.0 Pa;
(3) setting the power of a radio frequency power supply: the power sputtering power is set to be 200W;
example four
With high purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3The preparation method of the antireflection film comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) As a reaction gas, the total gas flow rate during sputtering was set to 70sccm, and SF was added6/Ar2The gas flow ratio was set to 15%;
(2) setting the working pressure of the reaction chamber: setting the working air pressure of the vacuum chamber to be 4.5 Pa;
(3) setting the power of a radio frequency power supply: the power sputtering power is set to 300W;
EXAMPLE five
With high purity AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3Antireflection filmThe preparation method comprises the following steps:
(1)SF6/Ar2setting the gas flow ratio: with high purity Ar2(99.999%) as working gas, high purity SF6(99.999%) As a reaction gas, the total gas flow rate during sputtering was set to 80sccm, and SF was added6/Ar2The gas flow ratio was set to 20%;
(2) setting the working pressure of the reaction chamber: setting the working air pressure of the vacuum chamber to be 6.0 Pa;
(3) setting the power of a radio frequency power supply: the power sputtering power is set to 400W;
AlF prepared in the above example3The antireflection films are reported as example 1, example 2, example 3, example 4, example 5, respectively.
All AlFs as shown in FIG. 13The refractive index of the film decreases with increasing wavelength in the range of 300-1100 nm. Is shown in6As a reaction gas to the working gas Ar2In gas, and by changing working gas pressure and power sputtering power, AlF is enabled3Film refractive index reduction effective, AlF prepared in example 23The refractive index of the film varies in the range of 1.407-1.377.
As shown in FIG. 2, the monolayer AlF prepared under each example3The transmittance spectra of the coated glass and the uncoated glass in the wavelength range of 300-1100 nm. Example 1AlF3The transmittance of the coated glass in the wave band of 300-350nm is lower than that of the glass substrate, and the transmittance of the coated glass in the wave range of 350-1100nm is obviously higher than that of the uncoated glass; example 2AlF3The transmittance of the coated glass in a wave band of 300-380nm is lower than that of the glass substrate, the transmittance of the coated glass in a wave band of 380-1100nm is far higher than that of the uncoated glass, and the average transmittance has a maximum value of 94.06%; example 3 the transmittance of the coated glass at 300-. Examples 4 and 5 the transmittance of the coated glass in the range of 410-1100nm was higher than that of the uncoated glass. The order of the average transmittance from large to small corresponds to the coated glasses of examples 2, 1, 4, 5 and 3.
And literature (Antireflection coatings for de)ep ultrasound optics positioned by magnetrons sputtering from Al targets; AlF deposited using magnetron sputtering method reported by Optics Express Vol.19(2011) p.7507-7512)3Compared with the antireflection film, the AlF prepared by the technical scheme of the embodiment3The transmittance and the anti-reflection wave band of the anti-reflection film are improved.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. With AlF3Preparation of broadband high-transmittance AlF for target material by magnetron sputtering method3Method for antireflection coating, characterized in that it is carried out with high purity SF6(99.999%) as a reaction gas to high purity Ar2(99.999%) of working gas for preparing AlF by magnetron sputtering method3F-depletion defects of the film; selecting proper working pressure of the reaction chamber to enable the atomic ratio of F/Al to be close to the ideal stoichiometric ratio of 3: 1; and proper radio frequency power supply power is supplemented, so that the atomic ratio of F/Al further accords with the ideal stoichiometric ratio of 3: 1, the refractive index of the film is reduced, and the transmittance of the coated glass is improved.
2. The broadband high transmission AlF according to claim 13The preparation method of the antireflection film is characterized in that the SF6/Ar2Gas flow rate ratio of6/Ar2The flow rate ratio is 0.1-20%.
3. The broadband high transmission AlF according to claim 13The preparation method of the antireflection film is characterized in that the working pressure of the reaction chamber is 0.1Pa-6.0 Pa.
4. The broadband high transmission MgF of claim 12The preparation method of the antireflection film is characterized in that the radio frequency power supply has power of 30W-400W.
5. The broadband high transmission AlF according to claim 13The method for preparing the antireflection film is characterized in that SF is adjusted6/Ar2Flow ratio, reaction chamber working pressure, radio frequency power supply power, and prepared AlF3The atomic ratio of F/Al of the antireflection film reaches an ideal stoichiometric ratio of 3: 1, the lowest refractive index of the antireflection film reaches 1.377, and the problem of F deficiency defect is effectively inhibited. When the film is deposited on a glass substrate, a good antireflection effect can be realized, so that the light transmittance of the substrate in the wavelength range of 300-1100nm is increased by 1-3 percentage points.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09263936A (en) * | 1996-03-28 | 1997-10-07 | Olympus Optical Co Ltd | Production of thin film and thin film |
| JP2000178714A (en) * | 1998-12-15 | 2000-06-27 | Canon Inc | Formation of fluoride thin film, optical member having the thin film and sputtering device |
| US6217719B1 (en) * | 1998-05-22 | 2001-04-17 | Canon Kabushiki Kaisha | Process for thin film formation by sputtering |
| JP2004315834A (en) * | 2003-04-10 | 2004-11-11 | Sony Corp | Fluoride thin film manufacturing method |
| US20050023131A1 (en) * | 2003-08-01 | 2005-02-03 | Canon Kabushiki Kaisha | Method and apparatus for forming fluoride thin film |
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2020
- 2020-10-13 CN CN202011089057.5A patent/CN114351098A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09263936A (en) * | 1996-03-28 | 1997-10-07 | Olympus Optical Co Ltd | Production of thin film and thin film |
| US6217719B1 (en) * | 1998-05-22 | 2001-04-17 | Canon Kabushiki Kaisha | Process for thin film formation by sputtering |
| JP2000178714A (en) * | 1998-12-15 | 2000-06-27 | Canon Inc | Formation of fluoride thin film, optical member having the thin film and sputtering device |
| JP2004315834A (en) * | 2003-04-10 | 2004-11-11 | Sony Corp | Fluoride thin film manufacturing method |
| US20050023131A1 (en) * | 2003-08-01 | 2005-02-03 | Canon Kabushiki Kaisha | Method and apparatus for forming fluoride thin film |
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