CN218675345U - High-transmittance 9.2-10.7-micrometer laser broadband antireflection film - Google Patents
High-transmittance 9.2-10.7-micrometer laser broadband antireflection film Download PDFInfo
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Abstract
The utility model discloses a high transmissivity 9.2-10.7 mu m laser broadband antireflection film, its film system structure is: SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 /AIR, wherein SUB represents a zinc selenide substrate, AIR represents AIR, H1 represents a zinc selenide layer, H2 represents a zinc sulfide layer, L represents a YB layer, and the YB layer is an aluminum-doped YF 3 With calcium-doped BaF 3 A mixed film layer with the volume ratio of (2-3) to 1, k 1 ‑k 4 A coefficient representing a quarter reference wavelength optical thickness of each layer. The high-transmittance 9.2-10.7 mu m laser broadband antireflection film of the utility model has the average single-side reflectivity not more than 0.08 percent and the average double-side transmittanceThe rate is not less than 99.78%, the film stress is basically eliminated through the selection and the collocation of the film material, the adhesive force of the film is improved, and the obtained film has strong wear resistance and good high and low temperature resistance.
Description
Technical Field
The utility model relates to a high transmissivity 9.2-10.7 mu m laser broadband antireflection film, which belongs to the technical field of laser broadband high-efficiency antireflection films.
Background
In an optical element, light energy is lost due to reflection on the surface of the element, and in order to reduce the reflection loss on the surface of the element, a transparent dielectric film is often coated on the surface of the optical element, and such a film is called an antireflection film.
In the preparation process of the antireflection film, the optical properties such as reflectivity and transmissivity of the corresponding wave band need to be considered, and the mechanical properties such as film stress and adhesive force need to be considered, so that the use requirement can be better met. The film layer stress can directly cause the phenomena of film falling, color cracking and the like, and the performance of the product in all aspects is seriously influenced, so that the film layer stress is reduced or even eliminated, and the preparation of the antireflection film is very important. The reflectivity and the transmissivity are very important parameters for evaluating the performance of the antireflection film, and due to the importance of the antireflection film to an optical element, a plurality of research and development personnel are dedicated to the development of the antireflection film, and certain achievements are achieved on the reduction of the reflectivity and the improvement of the transmissivity of the antireflection film, for example, patent application with application number of CN202010731907.0, discloses an antireflection film for a sapphire substrate and a preparation method thereof, wherein the transmissivity is about 97% and the reflectivity is about 1.5%, but with the higher requirements of customers on the product quality, the optical performance of the antireflection film is still required to be further improved.
Disclosure of Invention
The utility model provides a high transmissivity 9.2-10.7 mu m's laser broadband antireflection film, average single face reflectivity is not more than 0.08%, average two-sided transmissivity is not less than 99.78%, and has eliminated rete stress basically, has improved the adhesive force of rete, and the wearability of gained rete is strong, and resistant high low temperature performance is good.
For solving the technical problem, the utility model discloses the technical scheme who adopts as follows:
a high-transmittance 9.2-10.7 μm laser broadband antireflection film comprises: SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 /AIR, wherein SUB represents a zinc selenide substrate, AIR represents AIR, H 1 Represents a zinc selenide layer, H 2 Represents a zinc sulfide layer, L represents a YB layer, and the YB layer is an aluminum-doped YF 3 With calcium-doped BaF 3 A mixed film layer with the volume ratio of (2-3) to 1, k 1 -k 4 A coefficient representing a quarter reference wavelength optical thickness of each layer.
The anti-reflection film basically eliminates the stress of the film layer and improves the adhesive force of the film layer through the selection and the collocation of the film layer, and the obtained film layer has strong wear resistance and good high and low temperature resistance; the average single-side reflectivity of the antireflection film is not more than 0.08%, and the average double-side transmittance is not less than 99.78%.
For the antireflection film, different wave bands and applicable substrates are different, and applicable film systems are also different; the zinc sulfide layer and the zinc selenide layer are selected, so that the scattering loss is extremely low, and the thermal shock resistance is high; by plating the YB layer, the zinc selenide layer and the zinc sulfide layer on the zinc selenide substrate according to a specific sequence, the stress problem among the film layers is effectively solved, the compactness of the film layers is improved, the film layers are firmer, the wear resistance and the temperature resistance are improved, the single-side reflectivity is reduced to be below 0.08 percent, and the double-side transmissivity is improved to be above 99.78 percent.
YF doped with aluminum in mixed film layer 3 With calcium-doped BaF 3 The selection of (1) reduces the film stress by doping aluminum and calcium in specific amounts, on the one hand, and reduces the single-sided reflectivity of the film, on the other hand.
In order to better balance the optical performance and the mechanical performance, the aluminum-doped YF is adopted 3 In the method, the doping amount of aluminum is 2 to 6 weight percent; calcium-doped BaF 3 In the calcium content is 1wt% -20wt%.
The high-transmittance 9.2-10.7 μm wide-band anti-reflection film is double-side plated and has a film system structure of AIR/H 2 k 4 Lk 3 H 1 k 2 Lk 1 /SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 /AIR。
K above 1 -k 4 The magnitude of (b) is related to the reference wavelength λ, k being the same as k at 10600nm 1 The value of (a) is 0.03 to 0.06 2 Is 2.20 to 2.60, k 3 Is 0.30 to 0.60, k 4 The value of (A) is 0.10-0.35.
K for better compatibility of optical property and mechanical property of antireflection film 1 L is a first YB layer, k 2 H 1 Is a zinc selenide layer, k 3 L is a second YB layer, k 4 H 2 Is a zinc sulfide layer; the physical thickness of the first YB layer is 100 +/-20 nm, the physical thickness of the zinc selenide layer is 2680 +/-100 nm, the physical thickness of the second YB layer is 970 +/-50 nm, and the physical thickness of the zinc sulfide layer is 285 +/-20 nm.
The laser broadband antireflection film with high transmittance of 9.2-10.7 mu m is calculated by the surface type, and the film stress is close to 0. The absolute value of the calculated value less than 0.05Gpa is considered to be approximately equal to 0.
The application adopts a formula of Newton's ring method
Calculating the film stress, and when the film surface diameter ratio is more than 50 times larger than the thickness, calculating the curvature radius r of the interference seasoning to derive the film stress sigma, wherein ts is not the substrate thickness, t f As the film thickness, es is the Young's modulus of elasticity of the substrate, and v is the Poisson's ratio of the substrate.
The ultra-low stress 9.2-10.7 mu m laser broadband antireflection film adopts ion-assisted deposition in the film coating process; before film coating, baking the zinc selenide substrate at 100-130 ℃ for 0.5-1 h; the initial vacuum degree during film forming is (0.5-0.8) × 10-3Pa, and the ion source parameters are set as follows: the accelerating voltage is 200V, the screen electrode voltage is 450 +/-50V, and the beam current is 5-100mA.
In order to further improve the density of the deposited film and improve the optical and mechanical properties, the zinc selenide adopts a molybdenum boat evaporation-resistant mode, and the evaporation rate is controlled to be 0.3 +/-0.05 nm/s. The zinc sulfide is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.6 +/-0.1 nm/s.
When the YB layer is evaporated, firstly the YF doped with aluminum is evaporated 3 With calcium-doped BaF 3 Mixing according to the volume ratio of (2-3) to 1, and then adopting a molybdenum boat to prevent evaporation, wherein the evaporation rate is controlled at 0.5 +/-0.1 nm/s.
The technology not mentioned in the present invention refers to the prior art.
The utility model discloses high transmissivity 9.2-10.7 mu m's laser broadband anti-reflection film, average single face reflectivity is not more than 0.08%, and average two-sided transmissivity is not less than 99.78%, and has eliminated rete stress through the selection of coating materials and collocation basically, has improved the adhesive force of rete, and the wearability of gained rete is strong, and resistant high low temperature performance is good.
Drawings
FIG. 1 is a schematic structural view of a laser broadband antireflection film with a high transmittance of 9.2-10.7 μm in example 1 of the present invention;
FIG. 2 is a single-side reflection curve diagram of a laser broadband antireflection film design with a high transmittance of 9.2-10.7 μm in example 1 of the present invention;
FIG. 3 is a single-side reflection curve diagram of the test of the high transmittance 9.2-10.7 μm laser broadband antireflection film in example 1 of the present invention;
FIG. 4 is a graph showing the double-sided transmittance of the high transmittance 9.2-10.7 μm laser broadband antireflection film test in example 1 of the present invention;
FIG. 5 is a graph showing a comparison between the change of the front and rear surfaces of a substrate before and after single-side coating in example 1 of the present invention (the left side is before coating and the right side is after coating);
in the figure, k 1 ～k 4 Representing the corresponding film layer.
Detailed Description
For a better understanding of the present invention, the following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
As shown in FIG. 1, a high transmittance of 9.2-10.7 μmThe laser broadband antireflection film has a film system structure as follows: AIR/H 2 k 4 Lk 3 H 1 k 2 Lk 1 /SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 (ii)/AIR; wherein SUB represents a zinc selenide substrate, AIR represents AIR, H1 represents a zinc selenide layer, H2 represents a zinc sulfide layer, L represents a YB layer, and the YB layer is YF doped with 5wt% of aluminum 3 With 1.2 wt.% of calcium doped, k 1 Has a value of 0.04 2 Has a value of 2.30,k 3 Has a value of 0.40, k 4 Is 0.15.k is a radical of 1 The physical thickness of the L layer is 100nm, k 2 H 1 The physical thickness of the layer is 2680nm, k 3 The physical thickness of the L layer was 970nm, k 4 H 2 The physical thickness of the layer was 285nm.
The preparation of the high-transmittance 9.2-10.7 mu m laser broadband antireflection film adopts a Winteron light 1100 type film coating machine, adopts an INFICON IC6 control instrument for crystal control, and utilizes the change of the oscillation frequency of a quartz crystal to measure the quality and the thickness of the film. The ion source adopts a Kaufman ion source developed in Chao Jiu chapter of China. The vacuum chamber obtains the vacuum degree required by the membrane system by the mutual matching of a mechanical pump, a diffusion pump and a deep cooling unit system, and the vacuum degree is measured by a thermocouple meter.
Performing ultrasonic cleaning on the zinc selenide substrate before film plating to remove residual dirt on the surface, baking for 1h at the baking temperature of 100 ℃, wherein the initial vacuum degree is about 7.0 x 10 during film deposition -4 Pa. The ion source parameters are set as: the accelerating voltage is 200V, the screen electrode voltage is 400V, and the beam current is about 30 mA. In the process of film deposition, a Kaufman ion source is used for assisting deposition, the concentration density is increased, and the structural integrity is improved, so that the performance and the service time of the film are improved, and the evaporation rate and the film thickness are controlled by adopting a crystal control method.
ZnSe adopts molybdenum boat to prevent evaporation heat evaporation, the evaporation rate is controlled at 0.3nm/s, znS adopts copper crucible electron beam evaporation, the evaporation rate is controlled at 0.6nm/s; when the YB layer is evaporated, firstly the YF doped with aluminum 3 With calcium-doped BaF 3 Mixing according to the volume ratio of 2.5 to 1, and then adopting a molybdenum boat to prevent evaporation, wherein the evaporation rate is controlled at 0.5nm/s.
And (3) testing results:
and (3) testing optical performance: the single-sided reflectivity and the double-sided transmittance of the film are tested by adopting an infrared spectrometer, and the obtained spectral curve meets the design requirement: the average single-sided reflectivity of 9.2-10.7 μm is less than 0.08% as shown in fig. 3-4, the average double-sided transmittance is more than 99.78%, and the film stress is calculated to be-0.02 GPa according to Newton's ring method formula by the surface type as shown in fig. 5.
Testing the performance of the film layer:
in order to ensure the reliability of the optical element, the following environmental tests are carried out on the broadband antireflection film sample according to the requirements of the general specification of the GJB2485-95 optical film layer:
(1) Abrasion resistance test: wrapping 2 layers of dry absorbent gauze outside the rubber friction head, and rubbing the film layer along the same track under the pressure of 9.8N, wherein the film layer has no damage such as scratches after 2000 times of reciprocating.
(2) Salt spray test: and (3) continuously spraying for 12h for two cycles at the ambient temperature of 35 ℃ and the NaCl concentration of 5%, wherein the total time is 24h, and the film layer is not abnormal.
(3) Soaking test: the sample was completely immersed in distilled or deionized water, and the film layer was not abnormal after one week.
(4) High and low temperature test: keeping the temperature at minus 65 ℃ for 2 hours, quickly switching from minus 65 ℃ to 80 ℃ for 2 hours, keeping the temperature from 80 ℃ to minus 65 ℃ for 2 hours, and circulating for 12 times without abnormity of the film layer.
(5) Adhesion force experiment: the film layer is firmly adhered to the surface of the film layer by using a 3M adhesive tape with the width of 1cm, and after the adhesive tape paper is quickly pulled up from the edge of the part to the vertical direction of the surface, the film layer is not fallen or damaged, and the process is repeated for 60 times, so that the film layer is still not fallen or damaged.
Comparative example 1
Mixing YF of YB layer with aluminum 3 With calcium-doped BaF 3 Replacement is by pure YF 3 With BaF 3 The single-sided reflectance of the film was 0.56% and the film stress was-15.26 GPa in all of the cases described in example 1,9.2 to 10.7. Mu.m.
Comparative example 2
BaF omitting calcium doping in YB layer 3 The rest being referred to the factThe single-sided reflectance of examples 1,9.2 to 10.7 μm was 1.21%, and the film stress calculation result was-20.35 GPa.
Comparative example 2
YF for omitting aluminum-doped YB layer 3 The single-sided reflectance of the film was 1.93% and the film stress was-22.18 GPa in all of the cases described in examples 1,9.2 to 10.7. Mu.m.
Claims (5)
1. A high-transmittance 9.2-10.7 μm laser broadband antireflection film is characterized in that: the film system structure is as follows: SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 /AIR, wherein SUB represents a zinc selenide substrate, AIR represents AIR, H1 represents a zinc selenide layer, H2 represents a zinc sulfide layer, L represents a YB layer, and the YB layer is an aluminum-doped YF 3 With calcium-doped BaF 3 A mixed film layer with the volume ratio of (2-3) to 1, k 1 -k 4 A coefficient representing a quarter reference wavelength optical thickness of each layer.
2. The high transmittance 9.2-10.7 μm laser broadband antireflection film according to claim 1, characterized in that: double-sided plating, the film system structure is AIR/H 2 k 4 Lk 3 H 1 k 2 Lk 1 /SUB/k 1 Lk 2 H 1 k 3 Lk 4 H 2 /AIR。
3. The high-transmittance 9.2-10.7 μm laser broadband antireflection film according to claim 1 or 2, characterized in that: k is a radical of formula 1 The value of (a) is 0.03 to 0.06 2 Is 2.20 to 2.60, k 3 Is 0.30 to 0.60, k 4 The value of (A) is 0.10-0.35.
4. The high-transmittance 9.2-10.7 μm laser broadband antireflection film according to claim 1 or 2, characterized in that: k is a radical of formula 1 L is a first YB layer, k 2 H 1 Is a zinc selenide layer, k 3 L is a second YB layer, k 4 H 2 A zinc sulfide layer; the physical thickness of the first YB layer is 100 +/-20 nm, and the physical thickness of the zinc selenide layer2680 + -100 nm, the physical thickness of the second YB layer 970 + -50 nm and the physical thickness of the zinc sulfide layer 285 + -20 nm.
5. The high-transmittance 9.2-10.7 μm laser broadband antireflection film according to claim 1 or 2, characterized in that: the average single-sided reflectivity is not more than 0.08 percent, and the average double-sided transmittance is not less than 99.78 percent.
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Inventor after: Liu Xiangyin Inventor after: Chen Li Inventor after: Chen Jiajia Inventor after: Li Quanmin Inventor after: Wu Yutang Inventor before: Liu Xiangyin Inventor before: Chen Li Inventor before: Chen Jiajia Inventor before: Li Quanmin Inventor before: Wu Yutang |
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