CN111090134B - Chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared composite antireflection film - Google Patents
Chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared composite antireflection film Download PDFInfo
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- CN111090134B CN111090134B CN201911146650.6A CN201911146650A CN111090134B CN 111090134 B CN111090134 B CN 111090134B CN 201911146650 A CN201911146650 A CN 201911146650A CN 111090134 B CN111090134 B CN 111090134B
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- G—PHYSICS
- G02—OPTICS
- 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
Abstract
The invention relates toA chalcogenide glass substrate laser, medium wave infrared and long wave infrared three-spectral-band composite antireflection film and a preparation method thereof belong to the technical field of vacuum coating. The preparation method realizes the preparation of the 1.064 mu m, 3.7 mu m-4.8 mu m and 8 mu m-12 mu m three-spectral-range composite antireflection film on the chalcogenide glass substrate by means of film system design, transition layer screening, process optimization and the like. The two side film systems of the invention are symmetrical structures, and the basic forms of the film systems on the two sides are as follows: sub/. alpha.H (. beta.)iMγiL)mThe film coating comprises a film layer, a film layer and a film layer, wherein H, M, L represents a high refractive index film layer, a middle refractive index film layer and a low refractive index film layer respectively, and the film layers on the two sides have consistent stress, so that the surface shape quality and the mechanical property of the coated substrate are improved.
Description
Technical Field
The invention belongs to the technical field of vacuum coating, and particularly relates to a chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared three-spectral-band composite antireflection film and a preparation method thereof.
Background
In recent years, the common-caliber infrared composite detection technology is developed rapidly, is a new technical approach for realizing accurate detection, can realize wide-spectrum omnibearing detection, has higher analysis sensitivity and interference resistance compared with an infrared detector of a single system, and can meet the practical requirement of severe environment. The infrared antireflection film can effectively improve the optical performance of the infrared optical element and plays a vital role in an infrared optical system. The multi-spectral band composite infrared film technology is the only way to improve the spectral performance of the common-aperture optical system.
The chalcogenide glass has the advantages of wide transmission spectrum range, small temperature coefficient of refractive index, moldability, and the like, and has excellent athermal performance and excellent dispersion elimination performance. In recent years, use in infrared optical systems has become increasingly common. But the arsenic-selenium-germanium material has higher thermal expansion coefficient (12-20 multiplied by 10)-6K-1@ 20-200 deg.C), and is far higher than the thermal expansion coefficient of common coating material(e.g., Ge: 6.1X 10)-6K-1@20℃～200℃，ZnS： 6.6×10-6K-1@20 ℃ -200 ℃), the film layer thermal stress is easily overlarge in the cooling process of the substrate after the film coating is finished due to the difference between the expansion coefficients of the film layer and the substrate, and the problems of the chalcogenide glass optical element, such as the ultra-poor surface shape, even the film stripping and the like exist after the surface antireflection film is coated. At present, few researches on the preparation technology of the infrared antireflection film of chalcogenide glass are published, and no report is found about a laser-infrared multi-spectral antireflection film.
Disclosure of Invention
Technical problem to be solved
The technical problem to be solved by the invention is as follows: a chalcogenide glass substrate laser, medium-wave infrared and long-wave infrared three-band composite antireflection film and a preparation method thereof are designed, and the purposes of improving the environmental stability and the product qualification rate of the chalcogenide glass two-band antireflection film are achieved.
(II) technical scheme
In order to solve the technical problem, the invention provides a preparation method of a chalcogenide glass substrate low-residual-reflectivity antireflection film, which comprises the following steps of:
(1) cleaning a substrate: cleaning the surface of chalcogenide glass to be coated with a film by using a polishing powder dipping solution and a cleaning agent;
(2) heating a substrate: baking and heating the coated part before coating, and increasing the temperature of the substrate, wherein the baking temperature is 140-180 ℃, and the temperature is kept for 1-2 hours;
(3) pre-cleaning a substrate: pre-cleaning the coated parts for 5-10 min by using an ion source before coating;
(4) designing a membrane system structure: the substrate material is selected from chalcogenide glass Ge10As40Se50The high refractive index coating material is germanium Ge, the middle refractive index coating material is zinc sulfide ZnS, and the low refractive index coating material is YF3Or YbF3The low residual reflectivity antireflection film is realized by adopting a double-sided coating mode, and the film system structures on the two sides are as follows:
Sub/αH(βiMγiL)m/Air，i＝1，2，…，m，m≥5；
wherein H, M sequentially represents Ge, ZnS of 1/4 wavelength optical thickness, L represents YF of 1/4 wavelength optical thickness3YbF3In the film system structure, only the first layer is Ge serving as a transition layer for connecting the chalcogenide glass substrate and the overlying antireflection film, and alpha, betai，γiIs 1/4 wavelength optical thickness multiple, has a value directly related to the reference wavelength, and is 0.1 ≦ βj/γi≤20，j＝1，2，…， m；
(5) And (3) Ge film layer plating: placing the Ge film material in a crucible, plating by electron beam evaporation, wherein the background vacuum degree before film plating is higher than 5 × 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(6) and (3) ZnS film coating: the ZnS film material is placed in a crucible or an evaporation boat and plated by adopting an electron beam evaporation or resistance heating evaporation method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(7)YF3or YbF3Coating a film layer: YF is added3Or YbF3The film material is placed in an evaporation boat and is plated by a resistance heating evaporation method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(8) plating a film system: and sequentially plating the film layers on the front and back surfaces of the chalcogenide glass substrate according to the film structure and the film layer plating process parameters.
Preferably, in the step 1, firstly wiping the substrate by using absorbent gauze dipped with a mixed solution of alcohol and ether in a ratio of 1:1, then uniformly wiping the surface of the lens to be coated by using diamond polishing solution with the granularity W of 0.1, and finally wiping the surface of the lens to be coated by using absorbent gauze and absorbent cotton dipped with a mixed solution of alcohol and ether in a ratio of 1:1 wiping the surface of the substrate, and inspecting the surface of the substrate by a haar method until no oil stain, dust particles or scratches exist.
Preferably, in step 2, the vacuum chamber is cleaned and Ge, ZnS and YbF are added3The film materials are respectively placed in an evaporation crucible and an evaporation boat; putting the cleaned substrate in a coating clamp, and then placing the coating clamp on a vacuum chamber workpiece rack; opening the vacuum pumping system until the vacuum degree reaches 1 × 10-2And when Pa is needed, rotating the workpiece frame at the rotating speed of 12 revolutions per minute, opening the vacuum chamber for baking, heating the substrate to 170 ℃, and preserving heat for 1 hour.
Preferably, in step 3, the coated part is pre-cleaned for 5min by an ion source before coating, the ion beam pressure is 220V, and the ion beam current is 110 mA.
Preferably, in step 4, the substrate material is selected from chalcogenide glass material Ge10As40Se50The specific film system is as follows:
Sub/0.26H 0.31M 0.18L 2.08M 0.18L 4.04M 0.32L 3.22M 0.32L 2.96M 0.2L 2.78M 0.2L 0.31M 0.32L 1.35M 0.9L 2.98M 1.03L 0.49M 6.06L 0.9M 1.38L 0.77M 7.35L 0.31M 2.47L/Air
wherein H, M, L represents Ge, ZnS and YbF of 1/4 wavelength optical thickness, respectively3Sub is the substrate and Air is the Air.
Preferably, in step 5, when the Ge film is plated by adopting the electron beam evaporation method, the film layer deposition rate is
Preferably, in step 6, when the ZnS film is plated by electron beam evaporation or resistance heating evaporation, the film deposition rate is
Preferably, YbF is plated in step 7 by resistance heating evaporation3When the film is formed, the film layer deposition rate is
Preferably, the method further comprises the step (9) of opening the vacuum chamber and taking out the coated element when the temperature of the vacuum chamber is not higher than 80 ℃ after coating is finished.
The invention also provides the chalcogenide glass substrate low-residual-reflectivity antireflection film prepared by the method.
(III) advantageous effects
The invention realizes the anti-reflection effect of the substrate by depositing the anti-reflection films on the surfaces of the two sides of the chalcogenide glass. The method effectively controls the deformation of the lens surface shape through the means of film system design, transition layer screening, process optimization and the like, and increases the film layer firmness, thereby achieving the purpose of improving the environmental stability and the product qualification rate of the chalcogenide glass dual-waveband antireflection film, and further realizing the preparation of the high-transmission-performance three-band composite antireflection film with the transmittance of 1.064 mu m +/-0.02 mu m being more than 91%, the average transmittance of 3.7 mu m-4.8 mu m being more than 97.5% and the average transmittance of 8 mu m-12 mu m being more than 96%. The two side film systems of the invention are symmetrical structures, and the basic forms of the film systems on the two sides are as follows: sub/. alpha.H (. beta.)iMγiL)mthe/Air, wherein H, M and L represent high refractive index, medium refractive index and low refractive index materials respectively, so that the stress of the two side film layers is equivalent, and the surface shape quality of the coated substrate is improved. In addition, through process exploration, the germanium film is determined to be used as a transition layer, and the adhesion strength of the composite antireflection film can be effectively improved.
Drawings
FIG. 1 is a schematic view of a chalcogenide glass surface broadband antireflection film;
FIG. 2 shows an uncoated chalcogenide glass substrate (Ge)10As40Se50) A spectral plot;
FIG. 3 shows the coated chalcogenide glass substrate (Ge)10As40Se50) Spectral plot.
Detailed Description
In order to make the objects, contents, and advantages of the present invention clearer, the following detailed description of embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
The invention realizes the preparation of the 1.064 mu m, 3.7 mu m-4.8 mu m and 8 mu m-12 mu m three-spectral-band composite antireflection film on the chalcogenide glass substrate by means of film system design, transition layer screening, process optimization and the like. The two side film systems of the invention are symmetrical structures, and the basic forms of the film systems on the two sides are as follows: sub/. alpha.H (. beta.)iMγiL)mThe film coating structure comprises a film coating layer, a film coating layer and a film coating layer, wherein H, M, L respectively represents a high-refractive-index film layer, a middle-refractive-index film layer and a low-refractive-index film layer, and the film layers on the two sides have consistent stress, so that the surface shape quality and the mechanical property of a coated substrate are improved. Specifically, the design and preparation method of the three-spectral-range antireflection film with the surface of the chalcogenide glass substrate being 1.064 μm, 3.7 μm-4.8 μm and 8 μm-12 μm, provided by the invention, comprises the following steps:
(1) cleaning a substrate: the surface of the chalcogenide glass to be coated is cleaned by dipping clean absorbent gauze or cotton cloth and the like into polishing powder solution and cleaning agent.
(2) Heating a substrate: before coating, the coated part needs to be baked and heated, the temperature of the substrate is increased, the baking temperature is 140-180 ℃, and the heat is preserved for 1-2 hours.
(3) Pre-cleaning a substrate: and pre-cleaning the coated parts for 5-10 min by using an ion source before coating.
(4) Designing a membrane system structure: the substrate material is selected from chalcogenide glass (Ge)10As40Se50) The high refractive index coating material is germanium (Ge), the middle refractive index coating material is zinc sulfide (ZnS), and the low refractive index coating material is yttrium fluoride (or Ytterbium Fluoride) (YF)3(or YbF)3) Adopt two-sided coating film mode to realize low residual reflectivity antireflection film, the membrane system structure on two sides is:
Sub/αH(βiMγiL)m/Air(i＝1，2，…，m；m≥5)
wherein, Sub is substrate, Air is Air, H, M, L represents Ge, ZnS and YF with optical thickness of 1/4 wavelength3(or YbF)3). The film structure has Ge as the first layer for connecting chalcogenide glass substrate and overlying antireflection layerAnd (3) a transition layer of the shooting film. Alpha, betai，γiIs an optical thickness multiple of 1/4 wavelength, has a value directly related to the reference wavelength, and is 0.1 ≦ βj /γi≤20(i,j＝1，2，…，m；m≥5)。
(5) And (3) Ge film layer plating: placing the Ge film material in a crucible, plating by electron beam evaporation, wherein the background vacuum degree before film plating is higher than 5 × 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller.
(6) And (3) ZnS film coating: the ZnS film material is placed in a crucible (or an evaporation boat) and plated by adopting an electron beam evaporation (or resistance heating evaporation) method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller.
(7)YF3(or YbF)3) Coating a film layer: YF is added3(or YbF)3) The film material is placed in an evaporation boat and is plated by a resistance heating evaporation method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller.
(8) Plating a film system: and sequentially plating the film layers on the front and back surfaces of the chalcogenide glass substrate according to the film structure and the film layer plating process parameters.
With a chalcogenide glass material (Ge)10As40Se50) As a substrate, the structure of the film system is shown in FIG. 1, and the spectrum curve of the substrate before film coating is shown in FIG. 2.
(1) Firstly, a substrate is preliminarily wiped by using absorbent gauze dipped with a mixed solution (1:1) of alcohol and ether. Then uniformly wiping the surface of the lens to be coated with a diamond polishing solution with the granularity W0.1, finally wiping the surface of the substrate with a mixed solution (1:1) of degreasing gauze and degreasing cotton cloth dipped with alcohol and ether, and inspecting the surface of the substrate by a haar method until no oil stain, dust particles and scratches exist.
(2) Cleaning the vacuum chamber, and mixing Ge, ZnS and YbF3The membrane materials are respectively placed in an evaporation crucible and an evaporation boat.
(3) Putting the cleaned substrate in a coating clamp, and then placing the coating clamp on a vacuum chamber workpiece rack.
(4) Opening the vacuum pumping system until the vacuum degree reaches 1 × 10-2And when Pa is needed, rotating the workpiece frame at the rotating speed of 12 revolutions per minute, opening the vacuum chamber for baking, heating the substrate to 170 ℃, and preserving heat for 1 hour.
(5) Pre-cleaning a substrate: and (3) pre-cleaning the coated parts for 5min by using an ion source before coating, wherein the ion beam pressure is 220V, and the ion beam current is 110 mA.
(6) Designing a membrane system structure: the substrate material is selected from chalcogenide glass material (Ge)10As40Se50) The specific film system is as follows:
Sub/0.26H 0.31M 0.18L2.08M 0.18L4.04M 0.32L 3.22M 0.32L 2.96M 0.2L 2.78M 0.2L 0.31M 0.32L 1.35M 0.9L 2.98M 1.03L 0.49M 6.06L 0.9M 1.38L 0.77M 7.35L 0.31M 2.47L/Air
wherein H, M, L represents Ge, ZnS and YbF of 1/4 wavelength optical thickness, respectively3。
(7) Plating a Ge film by adopting an electron beam evaporation method, wherein the deposition rate of the film layer is
The ZnS film is plated by adopting an electron beam evaporation or resistance heating evaporation method, and the film layer deposition rate is
YbF plating by resistance heating evaporation3Film, film layer deposition rate of
Film deposition rate and film thicknessControlled by a quartz crystal controller.
(8) Plating a film system: and sequentially plating the film layers on the front and back surfaces of the sulfur-based glass substrate according to the film structure and the film layer plating process parameters.
(9) And opening the vacuum chamber when the temperature of the vacuum chamber is not higher than 80 ℃ after the film coating is finished, and taking out the film coated element.
(10) The transmittance and reflectance of the coated element were measured using an infrared fourier spectrometer, as shown in fig. 3, in which the transmittance was 91.6% at 1.064 μm, 97.7% at 3.7-4.8 μm average, and 96.1% at 8-12 μm average.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The preparation method of the chalcogenide glass substrate low-residual-reflectivity antireflection film is characterized by comprising the following steps of:
(1) cleaning a substrate: cleaning the surface of chalcogenide glass to be coated with a film by using a dipping polishing powder solution and a cleaning agent;
(2) heating a substrate: baking and heating the coated part before coating, increasing the temperature of the substrate to 140-180 ℃, and keeping the temperature for 1-2 hours;
(3) pre-cleaning a substrate: pre-cleaning the coated parts for 5-10 min by using an ion source before coating;
(4) designing a membrane system structure: the substrate material is selected from chalcogenide glass Ge10As40Se50The high refractive index coating material is germanium Ge, the middle refractive index coating material is zinc sulfide ZnS, and the low refractive index coating material is YF3Or YbF3The low residual reflectivity antireflection film is realized by adopting a double-sided coating mode, and the film system structures on two sides are as follows:
Sub/αH(βiMγiL)m/Air，i＝1，2，…，m，m≥5；
wherein H, M sequentially represents Ge, ZnS of 1/4 wavelength optical thickness, L represents YF of 1/4 wavelength optical thickness3YbF3In the film system structure, only the first layer is Ge serving as a transition layer for connecting the chalcogenide glass substrate and the overlying antireflection film, and alpha, betai，γiIs 1/4 wavelength optical thickness multiple, has a value directly related to the reference wavelength, and is 0.1 ≦ βj/γi≤20，j＝1，2，…，m；
(5) And (3) Ge film layer plating: placing the Ge film material in a crucible, plating by electron beam evaporation, wherein the background vacuum degree before film plating is higher than 5 × 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(6) and (3) ZnS film coating: the ZnS film material is placed in a crucible or an evaporation boat and plated by adopting an electron beam evaporation or resistance heating evaporation method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(7)YF3or YbF3Coating a film layer: YF is added3Or YbF3The film material is placed in an evaporation boat and is plated by a resistance heating evaporation method, and the background vacuum degree before film plating is higher than 5 multiplied by 10-3Pa, film deposition rate of
The film deposition rate and the film thickness are controlled by a quartz crystal controller;
(8) plating a film system: sequentially plating each film layer on the front and back surfaces of the chalcogenide glass substrate according to the film structure and the film layer plating technological parameters;
in the step 1, firstly, a substrate is preliminarily wiped by using absorbent gauze dipped with a mixed solution 1:1 of alcohol and ether, then the surface of the lens to be coated is uniformly wiped by using diamond polishing solution with the granularity W of 0.1, and finally, the absorbent gauze and absorbent cotton cloth are dipped with a mixed solution 1 of alcohol and ether: 1 wiping the surface of a substrate, and inspecting the surface of the substrate by a haar method until no oil stain, dust particles or scratches exist;
in step 2, the vacuum chamber is cleaned, and Ge, ZnS and YbF are added3The film materials are respectively placed in an evaporation crucible and an evaporation boat; putting the cleaned substrate in a coating clamp, and then placing the coating clamp on a vacuum chamber workpiece rack; opening the vacuum pumping system until the vacuum degree reaches 1 × 10-2When Pa is needed, rotating the workpiece frame at the rotating speed of 12 revolutions per minute, opening the vacuum chamber for baking, heating the substrate to 170 ℃, and preserving heat for 1 hour;
in step 3, pre-cleaning the coated parts for 5min by using an ion source before coating, wherein the ion beam pressure is 220V, and the ion beam current is 110 mA;
in step 4, the substrate material is selected from chalcogenide glass material Ge10As40Se50The specific film system is as follows:
Sub/0.26H 0.31M 0.18L 2.08M 0.18L 4.04M 0.32L 3.22M 0.32L 2.96M 0.2L 2.78M 0.2L 0.31M 0.32L 1.35M 0.9L 2.98M 1.03L 0.49M 6.06L 0.9M 1.38L 0.77M 7.35L 0.31M 2.47L/Air
wherein H, M, L represents Ge, ZnS and YbF of 1/4 wavelength optical thickness, respectively3Sub is the substrate and Air is the Air.
2. The method of claim 1, wherein in step 5, when the Ge film is plated by electron beam evaporation, the film deposition rate is
3. The method of claim 1, wherein in step 6, when the ZnS film is formed by electron beam evaporation or resistance heating evaporation, the film deposition rate is set to
4. The method of claim 1 wherein step 7 comprises plating YbF by resistance heating evaporation3When the film is formed, the film layer deposition rate is
5. The method according to claim 4, further comprising a step (9) of opening the vacuum chamber and taking out the coated member when the temperature of the vacuum chamber is not higher than 80 ℃ after the coating is finished.
6. A chalcogenide glass substrate low residual reflectance anti-reflective film produced using the method of any one of claims 1 to 5.
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| CN112578481B (en) * | 2020-12-11 | 2022-03-15 | 中材人工晶体研究院有限公司 | Large-angle medium-long wave infrared anti-reflection protective film and preparation method thereof |
| CN113031123A (en) * | 2021-03-02 | 2021-06-25 | 长春理工大学 | Antireflection sheet preparation method and antireflection sheet |
| CN113341487A (en) * | 2021-06-03 | 2021-09-03 | 河南平原光电有限公司 | ZnSe substrate 10.3-10.9 mu m high-strength antireflection film and plating method |
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| CN115980898B (en) * | 2023-03-21 | 2023-06-20 | 成都沃达惠康科技股份有限公司 | Multi-element multi-layer middle infrared high-reflection film and preparation method thereof |
| CN116500715A (en) * | 2023-04-24 | 2023-07-28 | 中山吉联光电科技有限公司 | Neutral optical attenuation sheet and preparation method thereof |
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