CN112904461A - Ultraviolet band ultra-low absorption double-sided antireflection film and preparation method thereof - Google Patents
Ultraviolet band ultra-low absorption double-sided antireflection film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ultraviolet band ultra-low absorption double-sided antireflection film and a preparation method thereof, and the ultraviolet band ultra-low absorption double-sided antireflection film has the following structure: Air/(biliH) m/Sub/(aiHbiL) m/Air; wherein Sub represents a substrate; m is the number of cycles, m is an integer of 2-6; h represents a high-refractive-index film layer, and the refractive index of the high-refractive-index film layer is 1.5-3; l represents a low-refractive-index film layer, and the refractive index of the low-refractive-index film layer is 1-1.5; ai and bi respectively represent the optical thickness coefficient of each film layer, the numerical value of which is related to the reference wavelength lambda, and is more than or equal to 0 and less than or equal to 200 (ai lambda) and more than or equal to 0 and less than or equal to 200 (bi lambda). The ultraviolet band ultra-low absorption double-sided antireflection film has improved film system design and process, realizes 355nm ultraviolet antireflection by plating the film systems on the two side surfaces of an ultraviolet window glass substrate with the thickness of 5mm, reduces absorption, improves transmittance, and has the average transmittance of more than 99.5 percent and the single-sided reflection of less than 0.15 percent.
Description
Technical Field
The invention relates to an ultraviolet band ultra-low absorption double-sided antireflection film and a preparation method thereof, belonging to the field of 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.
The existing antireflection film of the ultraviolet band always has the problem of larger film layer absorption, so that the service life and the use effect of the lens can not meet the requirements of customers.
Disclosure of Invention
The invention provides an ultra-low absorption double-sided anti-reflection film in an ultraviolet band and a preparation method thereof, wherein the film systems are plated on the surfaces of two sides of a substrate through film system design and process improvement, the 355nm ultraviolet anti-reflection is realized, the average transmittance is more than 99.5%, the single-side reflection is less than 0.15%, and the laser damage resistance threshold is changed from the original 2J/cm2Increased to 5J/cm2(laser pulse width is 10ns) and the service life is prolonged from the original 1 month to the current 6-12 months (according to the use environment of a client).
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
an ultraviolet band ultra-low absorption double-sided antireflection film comprises the following structures: Air/(biliH) m/Sub/(aiHbiL) m/Air; wherein Sub represents a substrate; m is the number of cycles, m is an integer of 2-6; h represents a high-refractive-index film layer, and the refractive index of the high-refractive-index film layer is 1.5-3; l represents a low-refractive-index film layer, and the refractive index of the low-refractive-index film layer is 1-1.5; ai and bi respectively represent the optical thickness coefficient of each film layer, the numerical value of which is related to the reference wavelength lambda, and is more than or equal to 0 and less than or equal to 200 (ai lambda) and more than or equal to 0 and less than or equal to 200 (bi lambda).
The applicant finds that the distribution of the film system temperature field and the thermal stress field has a decisive effect on the damage threshold of the high-power laser film, and the laser damage threshold of the film can be greatly improved by controlling the distribution of the temperature field and the thermal stress field to a certain extent through film system optimization; on the other hand, in consideration of various factors such as absorption, scattering and infirm caused by coating efficiency and a thick film layer, the ultraviolet band ultralow-absorption antireflection film with excellent optical performance and mechanical performance is obtained by matching the minimum number of film layers and the minimum thickness of the absorbed film material, the problem that the existing antireflection film with the ultraviolet band is large in absorption is solved, the use effect of the lens is improved, and the service life of the lens is prolonged.
Preferably, the film layers on the front and back sides of the substrate are symmetrically arranged.
For the ultraviolet band, the absorption of the film material in this band is the first factor, and in view of absorption, refractive index, adhesion, moisture resistance, temperature resistance, etc., it is preferable that the film material for the high refractive index film layer is silicon dioxide (SiO)2) Or lanthanum fluoride (LaF)3) (ii) a The film material used by the low refractive index film layer is a fluoride material. Further preferably, the fluoride material is magnesium fluoride MgF2AlF, aluminum fluoride3Or sodium fluoroaluminate Na3AlF6。
The material used for the substrate is ultraviolet window glass with the refractive index of 1-2. Preferably, the material used for the substrate is calcium fluoride, sapphire or fused silica, etc.
As a specific preferred scheme in the present application, the structure of the ultraviolet band ultra-low absorption double-sided antireflection film is as follows: Air/LHLHLH/Sub/HLHLHLHLHL/Air, wherein H represents SiO2Film layer, L represents MgF2And (5) film layer.
As another specific preferred scheme of the present application, the structure of the ultraviolet band ultra-low absorption double-sided antireflection film is as follows: air/1.06L0.63H1.27L0.66H/Sub/0.66H1.27L0.63H1.06L/Air, wherein H represents LaF3Film layer, L represents AlF3And (5) film layer.
The preparation method of the ultraviolet band ultra-low absorption double-sided antireflection film comprises the following steps:
(1) heating a substrate: before coating, baking and heating the substrate in a vacuum state to increase the temperature of the substrate, wherein the baking temperature is 100-350 ℃, and the baking time is 1-3 hours;
(2) ion beam cleaning: carrying out ion beam cleaning on the substrate, wherein the ion cleaning time is 1-15 min, the ion beam voltage is 50-200V, and the ion beam current is 1-8A;
(3) plating a film system on the front surface of the substrate: according to the film system structure in the film system design, sequentially plating each film layer on the front surface of the substrate;
(4) plating a substrate reverse side film system: and (4) after the front film system is plated, taking out the element, and repeating the steps (1) to (3) to plate the film layers on the back surface in sequence.
The method uses specific process conditions such as electron beam evaporation and baking temperature, adopts a double-sided coating mode, can realize that the ultraviolet window glass with the thickness of 5mm has good transmission effect in a 355nm wave band, and has the average transmission rate of more than 99 percent; the optical efficiency of the ultraviolet window glass is improved, the laser damage resistance threshold of the optical lens is ensured, and the optical element has longer service life in ultraviolet laser application.
In order to improve the film adhesion, in the step (1), before baking, the substrate is wiped by using a mixture of (2-4): 1) of absorbent gauze dipped with absolute ethyl alcohol and ether, and then the substrate is cleaned by adopting an ultrasonic cleaning mode.
The control of the conditions during the preparation of the membrane layers is also very critical, the preparation conditions of each membrane layer not only influence the performance such as compactness of a single membrane layer, but also influence the bonding force with an adjacent membrane layer and the optical performance of an integral membrane layer, preferably, in the step (3) and the step (4),
coating a SiO2 film layer: mixing SiO2The film material is put into a crucible and plated by adopting an electron beam evaporation method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.1 nm/s;
plating an MgF2 film layer: MgF2The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.08-0.09 nm/s;
coating a LaF3 film layer: mixing LaF3The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.05-0.1 nm/s;
AlF3 film coating: placing AlF3 film material in crucible or molybdenum boat, and plating by electron beam evaporation or resistance heating method with background vacuum degree higher than 1.5 × 10-3Pa, deposition rate of 0.05-0.1 nm/s.
Through the film system design and process improvement, the 355nm ultraviolet anti-reflection is realized by plating film systems on the two side surfaces of the 5 mm-thick ultraviolet window glass substrate, the absorption is reduced, the transmittance is improved, the average transmittance is more than 99.5%, and the single-side reflection is less than 0.15%.
The background vacuum degree refers to that the vacuum pumping system is utilized to make the gas in a certain space reach a certain vacuum degree in the vacuum coating process, and the vacuum degree just can meet the vacuum degree required by the deposition of the coated article (different goods have different requirements on the background vacuum degree).
The prior art is referred to in the art for techniques not mentioned in the present invention.
The ultraviolet band ultra-low absorption double-sided antireflection film has improved film system design and process, realizes 355nm ultraviolet antireflection by plating the film systems on the two side surfaces of an ultraviolet window glass substrate with the thickness of 5mm, reduces absorption, improves transmittance, has average transmittance of more than 99.5 percent and single-sided reflection of less than 0.15 percent, improves the threshold value of laser damage resistance and prolongs the service life.
Drawings
FIG. 1 is a schematic structural view of an ultra-low absorption anti-reflective film in an ultraviolet band in example 1 of the present invention;
FIG. 2 is a design curve of an ultra-low absorption antireflection film in an ultraviolet band in example 1 of the present invention;
FIG. 3 is a reflection coating curve of an ultra-low absorption antireflection film in an ultraviolet band in example 1 of the present invention;
FIG. 4 is a transmission coating curve of an ultra-low absorption ultraviolet reflection reducing coating in the UV wavelength band in example 1 of the present invention
FIG. 5 is a schematic structural view of an ultra-low absorption anti-reflective film for ultraviolet band in example 2 of the present invention;
FIG. 6 is a design curve of an ultra-low absorption antireflective film in the ultraviolet band of example 2 according to the present invention;
FIG. 7 is a reflection coating curve of an ultra-low absorption antireflection film in an ultraviolet band in example 2 of the present invention;
FIG. 8 is a transmission coating curve of an ultra-low absorption antireflection film in an ultraviolet band in example 2 of the present invention;
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 preparation of the film is completed on an optical relaxation OTFC-1300 vacuum box type film coating machine, and the film thickness adopts a light control and crystal control system. The film coating machine is provided with an electron beam evaporation source mode and a thermal resistance evaporation source mode, and a condensing pump ensures that the equipment is oilless and waterless.
Example 1
As shown in figure 1, the ultraviolet band ultra-low absorption double-sided antireflection film has the structure of Air/LHLHLH/Sub/HLHLHLHLHL/Air, wherein H represents SiO2A film layer with the thickness of 63mm, wherein L represents MgF2The thickness of the film layer is 60mm, Sub represents a substrate, the thickness of the substrate is 5mm, and the material is fused quartz.
The preparation method of the antireflection film comprises the following steps:
(1) heating a substrate: wiping a substrate by using absorbent gauze dipped with a 3:1 mixed solution of absolute ethyl alcohol and diethyl ether, cleaning the substrate by adopting an ultrasonic cleaning mode, baking and heating the substrate in a vacuum state, and increasing the temperature of the substrate, wherein the baking temperature is 160-170 ℃, and the baking time is 1.5 hours;
(2) ion beam cleaning: carrying out ion beam cleaning on the substrate, wherein the ion cleaning time is 2min, the ion beam voltage is 100V, and the ion beam current is 4A;
(3) plating a film system on the front surface of the substrate: according to the film system structure in the film system design, sequentially plating each film layer on the front surface of the substrate;
(4) plating a substrate reverse side film system: after the front film system is plated, taking out the element, and repeating the steps (1) - (3) to plate the back film layers in sequence;
in the step (3) and the step (4), SiO2Coating a film layer: mixing SiO2The film material is put into a crucible and plated by adopting an electron beam evaporation method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.1 nm/s; MgF2Coating a film layer: MgF2The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.08 nm/s;
the indexes are detected by a white Russian RT spectrophotometer which is shown in figure 3 and figure 4, and the single-side reflection is smallAt 0.15%, the double-sided transmittance is more than 99.5%, and the laser damage resistance threshold is 2J/cm2Increased to 5J/cm2(laser pulse width is 10ns) and the service life is prolonged from the original 1 month to the current 6-12 months (according to the use environment of a client).
In order to ensure the reliability of the optical element, environmental tests were performed on the samples according to the use requirements:
and (3) testing the adhesive force: A3M special adhesive tape with the width of 1 inch is tightly attached to the surface of the coated film, and then the coated film is quickly pulled up along the vertical direction of the film surface, and the film is repeatedly pulled for 10 times without demoulding phenomenon.
And (3) testing the damp heat: the film layer has no problem after being soaked in water with the temperature of 50 ℃ for 24 hours.
High temperature resistance verification: after the temperature is raised to 300 ℃ and the baking is carried out for 1 hour at the normal temperature, the film layer is free from problems.
Example 2
As shown in fig. 2, the ultraviolet band ultra-low absorption double-sided antireflection film has the following structure: air/1.06L0.63H1.27L0.66H/Sub/0.66H1.27L0.63H1.06L/Air, each layer has a theoretical thickness of 36.84/81.84/35.17/68.3/Sub//68.3/35.17/81.84/36.84nm, wherein H represents LaF3Film layer, L represents AlF3The film layer, Sub represents a substrate, the thickness of the substrate is 5mm, and the material is sapphire.
The preparation method of the antireflection film comprises the following steps:
(1) heating a substrate: wiping a substrate by using absorbent gauze dipped with a 3:1 mixed solution of absolute ethyl alcohol and diethyl ether, cleaning the substrate by adopting an ultrasonic cleaning mode, baking and heating the substrate in a vacuum state, and increasing the temperature of the substrate, wherein the baking temperature is 160-170 ℃, and the baking time is 1.5 hours;
(2) ion beam cleaning: carrying out ion beam cleaning on the substrate, wherein the ion cleaning time is 2min, the ion beam voltage is 100V, and the ion beam current is 4A;
(3) plating a film system on the front surface of the substrate: according to the film system structure in the film system design, sequentially plating each film layer on the front surface of the substrate;
(4) plating a substrate reverse side film system: after the front film system is plated, taking out the element, and repeating the steps (1) - (3) to plate the back film layers in sequence;
in the step (3) and the step (4), LaF3Coating a film layer: mixing LaF3The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.08 nm/s; AlF3Coating a film layer: subjecting AlF to3The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate 0.08 nm/s.
The white Russian RT spectrophotometer is used for index detection, and as can be seen from figures 5 and 6, the coating curve obtained by actual production can meet the use requirement and is basically consistent with the theoretical value. Single-side reflection less than 0.15%, double-side transmittance greater than 99.5%, and laser damage resistance threshold of 2J/cm2Increased to 5J/cm2(laser pulse width is 10ns) and the service life is prolonged from the original 1 month to the current 6-12 months (according to the use environment of a client).
In order to ensure the reliability of the optical element, environmental tests were performed on the samples according to the use requirements:
and (3) testing the adhesive force: A3M special adhesive tape with the width of 1 inch is tightly attached to the surface of the coated film, and then the coated film is quickly pulled up along the vertical direction of the film surface, and the film is repeatedly pulled for 10 times without demoulding phenomenon.
And (3) testing the damp heat: the film layer has no problem after being soaked in water with the temperature of 50 ℃ for 24 hours.
High temperature resistance verification: after the temperature is raised to 300 ℃ and the baking is carried out for 1 hour at the normal temperature, the film layer is free from problems.
Claims (10)
1. An ultraviolet band ultra-low absorption double-sided antireflection film is characterized in that: the structure is as follows: Air/(biliH) m/Sub/(aiHbiL) m/Air; wherein Sub represents a substrate; m is the number of cycles, m is an integer of 2-6; h represents a high-refractive-index film layer, and the refractive index of the high-refractive-index film layer is 1.5-3; l represents a low-refractive-index film layer, and the refractive index of the low-refractive-index film layer is 1-1.5; ai and bi respectively represent the optical thickness coefficient of each film layer, the numerical value of which is related to the reference wavelength lambda, and is more than or equal to 0 and less than or equal to 200 (ai lambda) and more than or equal to 0 and less than or equal to 200 (bi lambda).
2. The ultraviolet band ultra-low absorption double-sided antireflection film of claim 1, wherein: the film material of the high-refractive-index film layer is SiO2Or LaF3(ii) a The film material used by the low refractive index film layer is a fluoride material.
3. The ultraviolet band ultra-low absorption double-sided antireflection film of claim 2, wherein: the fluoride material is MgF2、AlF3Or Na3AlF6。
4. The ultra-low absorption double-sided antireflective film of any one of claims 1 to 3, wherein: the material used for the substrate is ultraviolet window glass with the refractive index of 1-2.
5. The ultraviolet band ultra-low absorption double-sided antireflection film of claim 4, wherein: the material used for the substrate is calcium fluoride, sapphire or fused quartz.
6. The ultra-low absorption double-sided antireflective film of any one of claims 1 to 3, wherein: the structure is as follows: Air/LHLHLH/Sub/HLHLHLHLHL/Air, wherein H represents SiO2Film layer, L represents MgF2And (5) film layer.
7. The ultra-low absorption double-sided antireflective film of any one of claims 1 to 3, wherein: the structure is as follows: air/1.06L0.63H1.27L0.66H/Sub/0.66H1.27L0.63H1.06L/Air, wherein H represents LaF3Film layer, L represents AlF3And (5) film layer.
8. The method for preparing an ultra-low absorption double-sided antireflection film of an ultraviolet band according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
(1) heating a substrate: before coating, baking and heating the substrate in a vacuum state to increase the temperature of the substrate, wherein the baking temperature is 100-350 ℃, and the baking time is 1-3 hours;
(2) ion beam cleaning: carrying out ion beam cleaning on the substrate, wherein the ion cleaning time is 1-15 min, the ion beam voltage is 50-200V, and the ion beam current is 1-8A;
(3) plating a film system on the front surface of the substrate: according to the film system structure in the film system design, sequentially plating each film layer on the front surface of the substrate;
(4) plating a substrate reverse side film system: and (4) after the front film system is plated, taking out the element, and repeating the steps (1) to (3) to plate the film layers on the back surface in sequence.
9. The method of claim 8, wherein: in the step (1), before baking, the substrate is wiped by using the mixed solution of (2-4) and (1) of absorbent gauze dipped with absolute ethyl alcohol and ether, and then the substrate is cleaned by adopting an ultrasonic cleaning mode.
10. The production method according to claim 8 or 9, characterized in that: in the step (3) and the step (4),
SiO2coating a film layer: mixing SiO2The film material is put into a crucible and plated by adopting an electron beam evaporation method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.1 nm/s;
MgF2coating a film layer: MgF2The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.08-0.09 nm/s;
LaF3coating a film layer: mixing LaF3The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.05-0.1 nm/s;
AlF3coating a film layer: placing AlF3 film material in crucible or molybdenum boat, and plating by electron beam evaporation or resistance heating method with background vacuum degree higher than 1.5 × 10-3Pa, deposition rate of 0.05-0.1nm/s；
Na3AlF6Coating a film layer: mixing Na3AlF6The film material is put into a crucible or a molybdenum boat and plated by adopting an electron beam evaporation or resistance heating method, and the background vacuum degree is higher than 1.5 multiplied by 10-3Pa, deposition rate of 0.05-0.1 nm/s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114853355A (en) * | 2022-04-08 | 2022-08-05 | 常州市万华激光科技有限公司 | Preparation method of ultraviolet 193nm antireflection film |
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| CN104593723A (en) * | 2015-01-21 | 2015-05-06 | 中国科学院光电技术研究所 | AlF prepared by improving thermal evaporation3Method for aging of film in deep ultraviolet and vacuum ultraviolet wave band |
| CN106067652A (en) * | 2016-07-29 | 2016-11-02 | 杭州科汀光学技术有限公司 | A kind of dual wavelength anti-reflection film for excimer laser and optical film thickness monitoring system |
| CN205670198U (en) * | 2016-05-24 | 2016-11-02 | 蓝思科技股份有限公司 | A kind of damage resistant hyaline membrane |
| CN109844573A (en) * | 2016-08-09 | 2019-06-04 | 依视路国际公司 | There are the optical goods of high reflection near infrared region and blue light region |
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2021
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5850309A (en) * | 1996-03-27 | 1998-12-15 | Nikon Corporation | Mirror for high-intensity ultraviolet light beam |
| CN104593723A (en) * | 2015-01-21 | 2015-05-06 | 中国科学院光电技术研究所 | AlF prepared by improving thermal evaporation3Method for aging of film in deep ultraviolet and vacuum ultraviolet wave band |
| CN205670198U (en) * | 2016-05-24 | 2016-11-02 | 蓝思科技股份有限公司 | A kind of damage resistant hyaline membrane |
| CN106067652A (en) * | 2016-07-29 | 2016-11-02 | 杭州科汀光学技术有限公司 | A kind of dual wavelength anti-reflection film for excimer laser and optical film thickness monitoring system |
| CN109844573A (en) * | 2016-08-09 | 2019-06-04 | 依视路国际公司 | There are the optical goods of high reflection near infrared region and blue light region |
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| CN114853355A (en) * | 2022-04-08 | 2022-08-05 | 常州市万华激光科技有限公司 | Preparation method of ultraviolet 193nm antireflection film |
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