CN112501557A - Sapphire substrate 1-5 mu m ultra-wideband antireflection film and preparation method thereof - Google Patents
Sapphire substrate 1-5 mu m ultra-wideband antireflection film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a sapphire substrate 1-5 mu M ultra-wideband antireflection film and a preparation method thereof, wherein the sapphire substrate 1-5 mu M ultra-wideband antireflection film has a structure of A/cMgLaH/SUB/aHbLcM/A, wherein SUB represents a sapphire substrate, A represents air, H represents an Al2O3 layer, L represents an SiO2 layer, and M represents an MgF2 layer; a. b and c represent the coefficients of the optical thickness of a quarter of the reference wavelength of each layer, a is 2.62-3.56, b is 1.88-2.55, and c is 2-2.31. The sapphire substrate 1-5 mu m ultra-wideband antireflection film has excellent optical performance, the average reflection of the antireflection film on a single surface of 1-5 mu m is less than 2.4 percent, and the average transmission of the double surfaces is more than 95.4 percent; the preparation repeatability is good; the film has strong adhesive force, friction resistance, water resistance and high temperature resistance.
Description
Technical Field
The invention relates to a sapphire substrate 1-5 mu m ultra-wideband antireflection film and a preparation method thereof, belonging to the field of antireflection films.
Background
For some equipment such as goggles, front-view infrared windows, hoods and the like, the equipment is required to have high infrared band transmittance and low absorption optical performance, and also needs to have good mechanical strength, corrosion resistance and other performances; the sapphire material has a wider transmission waveband, and the transmission area is from ultraviolet to middle infrared; sapphire also has excellent physical and chemical properties such as high melting point, high strength, corrosion resistance, and the like, and is very suitable as a material for such optical components.
However, due to limited equipment and process levels, SiO is currently being fabricated on sapphire substrates2The light transmission range of the equal film is narrow and is only 0.5-1.5 mu m; therefore, the preparation of the broadband antireflection film on the sapphire substrate has great significance.
Disclosure of Invention
The invention provides a sapphire substrate 1-5 mu m ultra-wideband antireflection film and a preparation method thereof, and the ultra-wideband antireflection film with excellent optical performance, good preparation repeatability, strong film adhesion and friction resistance is obtained by improving a film material and a preparation process, wherein the average reflection of the antireflection film on a single surface of 1-5 mu m is less than 3%, the average transmission of the double surfaces is more than 94%, and the use requirement of an optical system is met.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a sapphire substrate 1-5 μm ultra-wideband antireflection film has a structure of A/cMgLaH/SUB/aHbLcM/A, wherein SUB represents a sapphire substrate, A represents air, and H represents Al2O3Layer, L represents SiO2Layer, M represents MgF2A layer; a. b and c represent the coefficients of the optical thickness of a quarter of the reference wavelength of each layer, a is 2.62-3.56, b is 1.88-2.55, and c is 2-2.31.
The reference wavelength for the film system design is 550 nm.
The values of a, b and c are related to the reference wavelength lambda, and the larger lambda is, the smaller the values of a, b and c are.
The sapphire selected by the application has a wider transmission waveband from ultraviolet light and visible light to near infrared and medium wave infrared; and also has excellent physical, chemical and high strength, high hardness, corrosion resistance and other properties.
The applicant has found that the substrate is sapphire, SiO2The single layer has better anti-reflection effect in the wave band, so that SiO with low refraction is selected2Coating materials; but due to SiO2The thermal expansion coefficient of the material is greatly different from that of sapphire, and the high thermal stress can be generated due to large temperature change in the film deposition process, so that the strength and the thermal stability of the product can be reduced, and even components can be damaged; and the main component of the sapphire is Al2O3，Al2O3The film has high transmission and small absorption in the spectrum range from ultraviolet to middle and far infrared, and has good physical and chemical properties, so that the neutral refractive index film material Al is selected2O3As a substrate and SiO2A transition layer of (a); additionally MgF2Has high hardness, good mechanical property, stable chemical property, difficult deliquescence and corrosion, and optical property, and is mainly characterized in that the absorption in the wave band is low (the light transmission area is 0.2-6 mu m), and the magnesium fluoride film layer is plated to reduce the reflection of the lens interface to the incident light, reduce the halation and improve the imaging quality (reduce the film interference), so the MgF is used as the outermost layer2Not only can improve the transmittance of the film, but also can make the film layer more resistant to friction.
The ultra-wideband antireflection film with the thickness of 1-5 microns is prepared on the sapphire substrate through reasonable material selection and ion-assisted deposition.
In order to achieve both optical and mechanical properties, Al is preferred2O3The layer has a thickness of 218.78-312.4 nm and is made of SiO2The thickness of the layer is 177.13-252.92 nm, MgF2The thickness of the layer was 200 nm. The selection of the thickness range can ensure the compactness and the adhesive force of each layer, reduce the absorption and improve the optical performance. The above defines the physical thickness of the outermost layer of 200nm, MgF2Film material makingWhen the protective layer is an outermost layer, the physical thickness of the protective layer is more than 200nm, so that the performance of the film layer is unstable.
The preparation method of the sapphire substrate 1-5 mu m ultra-wideband antireflection film comprises the following steps:
1) cleaning the sapphire substrate;
2) baking for 20-30 minutes under the conditions that the vacuum degree is 1.0E-3Pa and the baking temperature is 250 +/-10 ℃;
3) setting ion source parameters: accelerating voltage of 200V, screen voltage of 250-500V, beam current of 20-100mA, and before coating, performing ion cleaning on the substrate for 2-20 min;
4) firstly, sequentially carrying out Al on the front surface of a sapphire substrate2O3Layer, SiO2Layer and MgF2Depositing a film layer, and then repeating the steps (2) to (4) to sequentially carry out Al on the reverse side of the sapphire substrate2O3Layer, SiO 22 layers and MgF2And (3) depositing a film layer, wherein Ar gas is flushed into the vacuum chamber in the film layer deposition process, so that the vacuum degree is maintained at 6.0E-3 Pa.
The drying in the step 1) is to keep for 20-30 minutes after the temperature reaches 250 +/-10 ℃ so as to ensure that the substrate is fully heated.
In the step 4), in the process of film deposition, a koffman ion source is used for assisting deposition, the concentration density is increased, the structural integrity is improved, the stress problem between films is effectively solved, the compactness of the films is improved, the films are firmer, the service life is longer, the performance and the service time of the films are improved, the optical thickness is controlled by adopting a light control method, the evaporation rate is controlled by adopting a crystal control method, the stability of the evaporation rate of each film material is maintained, and the product index is prevented from being influenced by the change of the refractive index of each film material.
The applicant determines the preparation process and process parameters of the application through long-term research and development and multiple experimental verification and optimization.
In the step 4), the setting of the vacuum degree can improve the density of the deposited film and improve the optical and mechanical properties, and the product performance is negatively influenced by too high or too low of the vacuum degree.
In order to improve the cleanness of the substrate and ensure the adhesive force of the antireflection film, in the step 1), the degreasing wiping cloth is dipped in a mixed solution of absolute ethyl alcohol and diethyl ether according to the volume ratio of 1 (3 +/-0.5) for wiping, so that the residual dirt on the surface is removed.
In step 4), Al is coated before film coating2O3And MgF2The film materials are separately pre-melted respectively, so that impurity gases in the film materials are removed, and the relative stability of the vacuum degree during film deposition is ensured; reduce the splashing of the film material and ensure the smooth finish of the surface of the substrate to reach the standard.
The applicant finds in long-term research and development practice that control of evaporation rate during preparation of each film layer is very critical, and for matching of different substrates and different film layers, even if evaporation rate of the same material is not referred, evaporation rate influences not only compactness of a single film layer, but also binding force with an adjacent film layer, and poor control of evaporation rate of any film layer influences optical performance and mechanical performance of an integral film layer, preferably, in step 4), Al is selected as a material for forming the film layer, and the evaporation rate of the film layer is controlled by Al2O3The layer is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.2 +/-0.01 nm/s; SiO22The layer is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.8 +/-0.01 nm/s; MgF2The layer is evaporated by graphite crucible electron beam, and the evaporation rate is controlled at 0.8 +/-0.01 nm/s.
The prior art is referred to in the art for techniques not mentioned in the present invention.
The sapphire substrate 1-5 mu m ultra-wideband antireflection film has excellent optical performance, the average reflection of the antireflection film on a single surface of 1-5 mu m is less than 2.4 percent, and the average transmission of the double surfaces is more than 95.4 percent; the preparation repeatability is good; the film has strong adhesive force, friction resistance, water resistance and high temperature resistance.
Drawings
FIG. 1 is a schematic structural diagram of a 1-5 μm ultra-wideband antireflection film on a sapphire substrate according to the present invention;
FIG. 2 is a theoretical design reflection curve diagram of a sapphire substrate 1-5 μm ultra-wideband antireflection film in example 1 of the present invention;
FIG. 3 is a single-sided reflection curve diagram of a sapphire substrate 1-5 μm ultra-wideband antireflection film in example 1 of the present invention;
FIG. 4 is a graph showing the transmission curves of a sapphire substrate 1-5 μm ultra-wideband antireflection film on one side and two sides, where a is the two sides and b is the one side in example 1 of the present invention;
FIG. 5 is a theoretical design reflection curve diagram of a sapphire substrate 1-5 μm ultra-wideband antireflection film in example 2 of the present invention;
FIG. 6 is a single-sided reflection curve diagram of a sapphire substrate 1-5 μm ultra-wideband antireflection film in example 2 of the present invention;
FIG. 7 is a graph showing the transmission curves of a sapphire substrate 1-5 μm ultra-wideband antireflection film on one side and two sides, where a is the two sides and b is the one side in example 2 of the present invention;
in the figure, 1 is a sapphire substrate, and 2 is Al2O3Layer, 3 is SiO2Layer, 4 is MgF2Layer 5 is air.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The coating adopts a Ducheng south China science and technology 1100 type coating machine, crystal control adopts an INFICON IC6 controller, and the quality and the thickness of the film are measured by using the oscillation frequency change of a quartz crystal. The ion source adopts a Kaufman ion source developed in the nine chapters of Chinese Keke. The vacuum chamber obtains the vacuum degree required by the membrane system by the mutual matching of the mechanical pump, the molecular pump and the deep cooling unit system, and the vacuum degree is measured by a thermocouple meter.
Example 1
As shown in figure 1, the structure of the ultra-wideband antireflection film with a sapphire substrate of 1-5 μm is A/cMgLaH/SUB/aHbLcM/A, wherein SUB represents the sapphire substrate (thickness 1mm), A represents air, and H represents Al2O3Layer, L represents SiO2Layer, M represents MgF2A layer; the reference wavelength of the film system design is 550nm, and a, b and c respectively represent the coefficients of the optical thickness of a quarter of the reference wavelength of each layer, which are respectively: 2.62, 1.88 and 2. The actual thicknesses of the three film layers are in order: al (Al)2O3The layer is 218.78nm and SiO2The layer is 177.13nm MgF2The layer is 200nm, the physical thickness of the outermost layer is limited to 200nm by the design, and when the MgF2 film material is used as the protection of the outermost layer, the physical thickness is more than 200nm to causeThe film layer performance is unstable.
Preparing the antireflection film: cleaning the sapphire substrate before film coating: wiping with a degreasing wiping cloth dipped with a 1:3 mixed solution of absolute ethyl alcohol and diethyl ether to remove surface dirt. The initial vacuum degree is 1.0E-3Pa, the baking temperature is 250 ℃, and the baking time is 30 minutes. The ion source parameters are set as: the accelerating voltage is 200V, the screen electrode voltage is 400V, and the beam current is 60 mA. Before coating, the substrate is subjected to ion cleaning for 5min, so that the substrate is cleaned, the condensation coefficient is improved, and the adhesive force of the film layer is enhanced. 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, the optical thickness is controlled by adopting a light control method, and the evaporation rate is controlled by adopting a crystal control method. Firstly, sequentially carrying out Al on the front surface of a sapphire substrate2O3Layer, SiO2Layer and MgF2Depositing a film layer, then repeatedly drying until the film layer is deposited, and sequentially carrying out an Al2O3 layer and SiO on the reverse side of the sapphire substrate2Layer and MgF2And (3) depositing a film layer, wherein Ar gas is flushed into the vacuum chamber in the film layer deposition process, so that the vacuum degree is maintained at 6.0E-3 Pa. Al is firstly plated before film plating2O3And MgF2And respectively performing independent pre-melting on the membrane materials. Al (Al)2O3Adopting a copper crucible electron beam for evaporation, and controlling the evaporation rate at 0.2 nm/s; SiO22Adopting a copper crucible electron beam for evaporation, and controlling the evaporation rate at 0.8 nm/s; MgF2The graphite crucible electron beam evaporation is adopted, and the evaporation rate is controlled at 0.8 nm/s.
And (3) testing optical performance: the single-side reflectivity and the double-side transmissivity of the film are tested by adopting a PHOTO RT spectrophotometer and an infrared spectrophotometer Spectrum100 of white Russia, and the obtained spectral curve meets the design requirement, as shown in figures 3-4: the single-sided reflection was 2.4% and the double-sided transmission was 95.4%.
Example 2
As shown in figure 1, the structure of the sapphire substrate 1.5-5 μm ultra-wideband antireflection film is A/cMgLaH/SUB/aHbLcM/A, wherein SUB represents the sapphire substrate, A represents air, and H represents Al2O3Layer, L representsSiO2Layer, M represents MgF2A layer; the reference wavelength of the film system design is 550nm, and a, b and c respectively represent the coefficients of the optical thickness of a quarter of the reference wavelength of each layer, which are respectively: 3.56, 2.55 and 2.31. The actual thicknesses of the three film layers are in order: al (Al)2O3The layer is 312.4nm, SiO2The layer is 252.92nm MgF2The layer is 200nm, the physical thickness of the outermost layer is limited to 200nm by the design, and MgF2When the film material is used as the outermost layer for protection, the physical thickness of the film material is more than 200nm, which causes the unstable performance of the film layer.
Preparing the antireflection film: cleaning the sapphire substrate before film coating: wiping with a degreasing wiping cloth dipped with a 1:3 mixed solution of absolute ethyl alcohol and diethyl ether to remove surface dirt. The initial vacuum degree is 1.0E-3Pa, the baking temperature is 250 ℃, and the baking time is 30 minutes. The ion source parameters are set as: the accelerating voltage is 200V, the screen electrode voltage is 400V, and the beam current is 60 mA. Before coating, the substrate is subjected to ion cleaning for 5min, so that the substrate is cleaned, the condensation coefficient is improved, and the adhesive force of the film layer is enhanced. 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, the optical thickness is controlled by adopting a light control method, and the evaporation rate is controlled by adopting a crystal control method. Firstly, sequentially carrying out Al on the front surface of a sapphire substrate2O3Layer, SiO2 layer and MgF2Depositing a film layer, drying repeatedly until the film layer is deposited, and sequentially carrying out Al on the reverse side of the sapphire substrate2O3Layer, SiO2Layer and MgF2And (3) depositing a film layer, wherein Ar gas is flushed into the vacuum chamber in the film layer deposition process, so that the vacuum degree is maintained at 6.0E-3 Pa. Al is firstly plated before film plating2O3And MgF2And respectively performing independent pre-melting on the membrane materials. Al (Al)2O3Adopting a copper crucible electron beam for evaporation, and controlling the evaporation rate at 0.2 nm/s; SiO2 is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled at 0.8 nm/s; MgF2The graphite crucible electron beam evaporation is adopted, and the evaporation rate is controlled at 0.8 nm/s.
And (3) testing optical performance: the single-sided reflectivity and the double-sided transmittance of the film are tested by adopting a PHOTO RT spectrophotometer and an infrared spectrophotometer Spectrum100 of white Russia, and the obtained spectral curve meets the design requirements, as shown in figures 5-7: the single-sided reflection was 1.7% and the double-sided transmission was 96.1%.
Film layer performance test results:
in order to ensure the reliability of the optical element, the following environmental tests were performed on the broadband antireflection film samples of examples 1-2 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 4.9N for 25 times without damage such as scratches.
(2) Adhesion force experiment: and (3) adhering a 3M adhesive tape with the width of 1cm to the surface of the film layer firmly, and quickly pulling up the adhesive tape from the edge of the part to the vertical direction of the surface, wherein the film layer is not fallen off and damaged.
(3) Soaking test: the sample is completely immersed in distilled water or deionized water, and no abnormality occurs in the membrane layer after 96 hours.
(4) High-temperature test: baking from normal temperature to 150 ℃ for 1 hour, cooling to normal temperature, and circulating twice, wherein the film layer has no abnormity.
The method adopts an ion beam assisted deposition technology, and adopts reasonable selection of film materials to plate 1-5 micron ultra-wideband anti-reflection on a sapphire substrate, so that the obtained film has good spectral performance, good mechanical stability and good stability.
Claims (6)
1. A sapphire substrate 1-5 mu m ultra-wideband antireflection film is characterized in that: the structure of the sapphire substrate is A/cMgLaH/SUB/aHbLcM/A, wherein SUB represents a sapphire substrate, A represents air, and H represents Al2O3Layer, L represents SiO2Layer, M represents MgF2A layer; a. b and c represent the coefficients of the optical thickness of a quarter of the reference wavelength of each layer, a is 2.62-3.56, b is 1.88-2.55, and c is 2-2.31.
2. The sapphire substrate 1-5 μm ultra-wideband antireflection film of claim 1, wherein:Al2O3the layer has a thickness of 218.78-312.4 nm and is made of SiO2The thickness of the layer is 177.13-252.92 nm, MgF2The thickness of the layer was 200 nm.
3. The method for preparing the sapphire substrate 1-5 μm ultra-wideband antireflection film of claim 1 or 2, which is characterized in that: the method comprises the following steps:
1) cleaning the sapphire substrate;
2) baking for 20-30 minutes under the conditions that the vacuum degree is 1.0E-3Pa and the baking temperature is 250 +/-10 ℃;
3) setting ion source parameters: accelerating voltage of 200V, screen voltage of 250-500V, beam current of 20-100mA, and before coating, performing ion cleaning on the substrate for 2-20 min;
4) firstly, sequentially carrying out Al on the front surface of a sapphire substrate2O3Layer, SiO2Depositing a film layer of the MgF2 layer and then repeating the steps (2) to (4) to carry out Al on the reverse side of the sapphire substrate in sequence2O3Layer, SiO2Layer and MgF2And (3) depositing a film layer, wherein Ar gas is flushed into the vacuum chamber in the film layer deposition process, so that the vacuum degree is maintained at 6.0E-3 Pa.
4. The method of claim 2, wherein: in the step 1), the degreasing wiping cloth is dipped in a mixed solution of absolute ethyl alcohol and ether with the volume ratio of 1 (3 +/-0.5) for wiping, and the residual dirt on the surface is removed.
5. The production method according to claim 4 or 5, characterized in that: in step 4), Al is coated before film coating2O3And MgF2And respectively performing independent pre-melting on the membrane materials.
6. The production method according to claim 4 or 5, characterized in that: in step 4), Al2O3The layer is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.2 +/-0.01 nm/s; SiO22The layer is evaporated by adopting a copper crucible electron beam, and the evaporation rate is controlled to be 0.8 +/-0.01 nm/s; MgF2The layer is evaporated by using an electron beam in a graphite crucible,the evaporation rate is controlled at 0.8 +/-0.01 nm/s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113584481A (en) * | 2021-08-11 | 2021-11-02 | 南京波长光电科技股份有限公司 | Carbon dioxide laser superhard film and preparation method thereof |
| CN114815004A (en) * | 2022-05-20 | 2022-07-29 | 无锡泓瑞航天科技有限公司 | Infrared metallized full-through sapphire window sheet and preparation method and application thereof |
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