CN110794490A - Design and preparation method of medium-wave infrared antireflection film - Google Patents
Design and preparation method of medium-wave infrared antireflection film Download PDFInfo
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- G—PHYSICS
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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Abstract
The invention discloses a design and preparation method of a medium-wave infrared antireflection film, which comprises the following steps: designing a film system, cleaning a substrate, heating the substrate, and plating the film system. The substrate material is infrared window glass with the refractive index of 1-5, the refractive index of the high-refractive-index coating material is 1.5-3, the refractive index of the low-refractive-index coating material is 1-1.5, the FGa glass with the thickness of 5mm has a good transmission effect in the infrared band of 3.7-5um by adopting a double-sided coating mode under the specific process conditions of ion-assisted deposition, proper baking temperature and the like, and the average transmission rate is more than 92%. The invention can improve the optical efficiency of the intermediate infrared window and has obvious advantages in convenient infrared detection.
Description
Technical Field
The invention belongs to the field of vacuum coating, and relates to a design and a preparation method of a medium-wave infrared antireflection film.
Background
With the continuous development of infrared technology, the infrared window film has important functions in the field of national defense and military. In an infrared detection system, it is necessary to improve the transmittance in the infrared band and thus the sensitivity of an optical system.
Disclosure of Invention
The technical solution adopted by the invention is as follows:
in order to solve the problems, the invention provides a design and preparation method of a medium-wave infrared antireflection film, which comprises the following steps:
(1) designing a membrane system:
the two facial mask systems are all Sub/(a)iHbiL)m/Air,m≥1,i=1,2,…,m。
Wherein H represents a high refractive index coating material with a refractive index of 1.5-3, L represents a low refractive index coating material with a refractive index of 1-1.5, aiAnd biRespectively representing the optical thickness coefficient of each film, the value of which is related to the reference wavelength lambda, m is the period number, and is more than or equal to 0 (a)iλ)≤2000,0≤(biλ)≤12000;
(2) Cleaning a substrate: cleaning the surface of an element to be coated;
(3) heating a substrate: vacuum baking and heating the element to be coated;
(4) ion beam cleaning: carrying out ion beam cleaning on an element to be coated;
(5) plating a first surface film system: according to the film system structure in the step (1), sequentially plating each film layer on the first surface of the element to be plated with a film;
(6) plating a second facial film system: and (4) after the first surface film system is plated, taking out the element, and repeating the steps (1) to (4) to plate the film layers of the second surface in sequence.
The two-sided film system plated in the steps (5) and (6) has the following structure:
Sub/0.92L2.91H3.92L0.92H2.92L0.45H/Air;
wherein H represents a high-refractive-index coating material ZnS, and L represents a low-refractive-index coating material MgF2。
The two-sided film system plated in the steps (5) and (6) has the following structure:
Sub/0.92L0.86H0.73L1.08H4.61L0.54H/Air;
wherein H represents a high refractive index coating material Al2O3L represents MgF which is a low refractive index coating material2。
The film coating preparation comprises the following steps:
(a) and (3) ZnS film coating: putting ZnS film material into crucible or molybdenum boat, plating by electron beam evaporation or resistance heating method with background vacuum degree higher than 4 × 10-3Pa, deposition rate of
(b)MgF2Coating a film layer: MgF2The film material is placed in a crucible and plated by adopting an electron beam evaporation method, and the background vacuum degree is higher than 4 multiplied by 10-3Pa, deposition rate of
(c)Al2O3Coating a film layer: mixing Al2O3The film material is placed in a crucible and plated by adopting an electron beam evaporation method, and the background vacuum degree is higher than 4 multiplied by 10-3Pa, deposition rate of
The invention has the beneficial effects that:
different film systems are plated on the two side surfaces of an infrared window FGa glass substrate with the thickness of 5mm by film system design and process optimization means to realize the medium wave infrared anti-reflection of 3.7-5um, and the average transmittance is more than 92 percent.
Drawings
FIG. 1 is a schematic cross-sectional view of a 5mm thick FGa glass substrate of the invention showing a mid-wave infrared antireflection film system, wherein (1) is a front film system, (2) is a FGa substrate, and (3) is a back film system.
FIG. 2 is a theoretical spectral curve of a medium wave infrared antireflection film in example 1 of the present invention.
FIG. 3 is a measured spectral curve of a medium wave infrared antireflective film of example 1 of the present invention.
FIG. 4 is a theoretical spectral curve of a medium wave infrared antireflection film in example 2 of the present invention.
FIG. 5 is a measured spectral curve of a medium wave infrared antireflective film of example 2 of the invention.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to the accompanying drawings, but the scope of the present invention should not be limited thereby.
Referring to fig. 1, the design and preparation method of the medium wave infrared antireflection film based on the surface of the infrared window FGa glass substrate with the thickness of 5mm mainly comprises the following steps:
(1) designing a membrane system:
the two facial mask systems are all Sub/(a)iHbiMciL)m/Air,m≥1,i=1,2,…,m。
Wherein H represents a high refractive index coating material with a refractive index of 1.5-3, L represents a low refractive index coating material with a refractive index of 1-1.5, aiAnd biRespectively representing the optical thickness coefficient of each film, the value of which is related to the reference wavelength lambda, m is the period number, and is more than or equal to 0 (a)iλ)≤2000,0≤(biλ)≤12000;
(2) Cleaning a substrate: cleaning the surface of an element to be coated;
(3) heating a substrate: vacuum baking and heating the element to be coated;
(4) ion beam cleaning: carrying out ion beam cleaning on an element to be coated;
(5) plating a first surface film system: according to the film system structure in the step (1), sequentially plating each film layer on the first surface of the element to be plated with a film;
(6) plating a second facial film system: and (4) after the first surface film system is plated, taking out the element, and repeating the steps (2) to (4) to plate the film layers of the second surface in sequence.
Example 1
(1) Determining the film system structure, wherein the two film system structures are as follows: sub/0.92L2.91H3.92L0.92 H2.92L0.45H/Air; wherein H represents a high-refractive-index coating material ZnS, and L represents a low-refractive-index coating material MgF2. FIG. 2 is a theoretical spectral curve of a medium wave infrared antireflective film designed according to this example.
(2) Cleaning a substrate: the substrate was wiped with absorbent gauze dipped in a 1:1 mixture of absolute ethanol and petroleum ether.
(3) The vacuum chamber was cleaned and the film charge was placed into the crucible.
(4) And (3) placing the cleaned substrate in a coating fixture, and then placing the coating fixture on a vacuum chamber workpiece frame.
(5) And (3) opening a vacuum system, opening the baking when the vacuum degree reaches 0.1Pa, setting the baking temperature to be 200 ℃, and opening the rotation, wherein the rotation voltage is 5V.
(6) Ion cleaning is carried out on the film plating element for 5min by using an ion source, the ion beam voltage is 150V, and the ion beam current is 6A;
(7) ZnS is plated by resistance evaporation at a deposition rate ofPlating MgF by electron beam evaporation2The deposition rate isAnd (3) sequentially plating the film layers on the first surface of the film element to be plated according to the intermediate film system in the step (1).
(8) Repeating the preparation work before the coating in the steps (1) to (6), and sequentially coating the film layers on the second surface of the element to be coated according to the coating process in the step (7).
(9) After the film coating is finished, the baking temperature is reduced to be close to the room temperature, the vacuum chamber is opened, and the film coating element is taken out.
(10) The transmittance of the coated element was measured using a fourier infrared spectrometer, and as shown in fig. 3, the mean transmittance of medium wave infrared 3.7-5um was 92.9%.
Example 2
(1) Determining the film system structure, wherein the two film system structures are as follows: sub/0.92 L0.86H0.73L1.08H4.61L0.54H/Air; wherein H represents a high refractive index coating material Al2O3L represents a low refractive index plateFilm material MgF2. FIG. 4 is a theoretical spectral curve of a medium wave infrared antireflective film designed according to this example.
(2) Cleaning a substrate: the substrate was wiped with absorbent gauze dipped in a 1:1 mixture of absolute ethanol and petroleum ether.
(3) The vacuum chamber was cleaned and the film charge was placed into the crucible.
(4) And (3) placing the cleaned substrate in a coating fixture, and then placing the coating fixture on a vacuum chamber workpiece frame.
(5) And (3) opening a vacuum system, opening the baking when the vacuum degree reaches 0.1Pa, setting the baking temperature to be 200 ℃, and opening the rotation, wherein the rotation voltage is 5V.
(6) Ion cleaning is carried out on the film plating element for 5min by using an ion source, the ion beam voltage is 150V, and the ion beam current is 6A;
(7) al plating by electron beam evaporation2O3The deposition rate isPlating MgF by electron beam evaporation2The deposition rate isAnd (3) sequentially plating the film layers on the first surface of the film element to be plated according to the intermediate film system in the step (1).
(8) Repeating the preparation work before the coating in the steps (1) to (6), and sequentially coating the film layers on the second surface of the element to be coated according to the coating process in the step (7).
(9) After the film coating is finished, the baking temperature is reduced to be close to the room temperature, the vacuum chamber is opened, and the film coating element is taken out.
(10) The transmittance of the coated element was measured using a fourier infrared spectrometer, and as shown in fig. 5, the average transmittance of medium wave infrared 3.7-5um was 92.2%.
Claims (7)
1. A design and preparation method of a medium wave infrared antireflection film is characterized by comprising the following steps:
(1) designing a membrane system:
the two facial mask systems are all Sub/(a)iHbiL)m/Air,m≥1,i=1,2,…,m;
Wherein H represents a high refractive index coating material with a refractive index of 1.5-3, L represents a low refractive index coating material with a refractive index of 1-1.5, aiAnd biRespectively representing the optical thickness coefficient of each film, the value of which is related to the reference wavelength lambda, m is the period number, and is more than or equal to 0 (a)iλ)≤2000,0≤(biλ)≤12000;
(2) Cleaning a substrate: cleaning the surface of an element to be coated;
(3) heating a substrate: before coating, baking and heating the coated element to increase the temperature of the substrate;
(4) ion beam cleaning: carrying out ion beam cleaning on an element to be coated;
(5) plating a first surface film system: according to the film system structure in the step (1), sequentially plating each film layer on the first surface of the element to be plated with a film;
(6) plating a second facial film system: and (4) after the first surface film system is plated, taking out the element, and repeating the steps (2) to (4) to plate the film layers of the second surface in sequence.
2. The method of claim 1, wherein the substrate is an infrared window material, preferably FGa glass, sapphire, spinel, zinc sulfide, zinc selenide, magnesium fluoride, rutile, calcium fluoride, yttria, zirconia, silicon, or germanium; h is ZnS, ZnSe or YbF3、YF3、BaF2、HfO2、Ta2O5、Nb2O5、TiO2、Y2O3、ZrO2、Al2O3Or SiO; l is MgF2、CaF2Or SiO2。
3. The method for designing and preparing a medium wave infrared antireflection film according to claim 1, wherein in the step (1), the two face film systems have the following structures:
Sub/0.92L2.91H3.92L0.92H2.92L0.45H/Air;
wherein H represents a high refractive index coating material ZnS, L represents a low refractive index coating material MgF2。
4. The method for designing and preparing a medium wave infrared antireflection film according to claim 1, wherein in the step (1), the two face film systems have the following structures:
Sub/0.92L0.86H0.73L1.08H4.61L0.54H/Air;
wherein H represents a high refractive index coating material Al2O3L represents MgF which is a low refractive index coating material2。
5. The method for designing and manufacturing a medium wave infrared antireflection film according to claim 1, wherein in the step (2), the substrate is wiped with a mixture of absorbent gauze dipped with absolute ethanol and petroleum ether at an N:1 ratio, wherein N is preferably 1 to 3.
6. The method for designing and preparing a medium wave infrared antireflection film according to claim 1, wherein in the step (3), the element to be coated is baked and heated in a vacuum-pumping process, the baking temperature is 100 ℃ to 300 ℃, and the heat preservation is performed for 1 to 3 hours.
7. The method for designing and manufacturing a medium wave infrared antireflection film according to claim 1, wherein in the step (4), the ion source is used to perform ion cleaning on the film plating element for 1 to 15min, the ion beam voltage is 50 to 200V, and the ion beam current is 1 to 8A.
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CN111323862A (en) * | 2020-03-11 | 2020-06-23 | 上海翼捷工业安全设备股份有限公司 | Infrared filter for sunlight interference resistance flame detection and preparation method thereof |
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CN111812753A (en) * | 2020-06-01 | 2020-10-23 | 湖南大学 | Silicon substrate 3-6 μm infrared window sheet |
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CN113917573A (en) * | 2021-09-27 | 2022-01-11 | 中国建筑材料科学研究总院有限公司 | Amorphous infrared film system structure and preparation method thereof |
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