266-nanometer high-power laser antireflection film and preparation method thereof

文档序号:632570 发布日期:2021-05-11 浏览:36次 中文

阅读说明:本技术 一种266纳米高功率激光增透膜及其制备方法 (266-nanometer high-power laser antireflection film and preparation method thereof ) 是由 王泽栋 李全民 李林峰 王国力 于 2021-02-02 设计创作,主要内容包括:本发明公开了一种266纳米高功率激光增透膜及其制备方法,一种266纳米高功率激光增透膜,膜层结构为:A/cL/bH/aL/SUB/aL/bH/cL/A,其中,SUB代表玻璃基底;A代表空气;H代表高折射率膜层;L代表低折射率膜层;a﹑b﹑c分别为各膜层的四分之一参考波长光学厚度的系数,a为1.6±0.2,b为0.53±0.2,c为1.13±0.2。本发明266纳米高功率激光增透膜,在紫外波段具有高抗激光损伤阈值,该增透膜在266nm波段处透过率可达99.9%以上,既有良好的光谱性能又有较好的机械稳性能和稳定性,可满足目前近紫外领域的一些高端应用。(The invention discloses a 266nm high-power laser antireflection film and a preparation method thereof, the 266nm high-power laser antireflection film comprises the following film layers: A/cL/bH/aL/SUB/aL/bH/cL/A, wherein SUB represents a glass substrate; a represents air; h represents a high refractive index film layer; l represents a low refractive index film layer; and a, b and c are coefficients of the optical thickness of the quarter reference wavelength of each film layer respectively, wherein a is 1.6 +/-0.2, b is 0.53 +/-0.2, and c is 1.13 +/-0.2. The 266-nanometer high-power laser antireflection film has a high laser damage resistance threshold value in an ultraviolet wave band, has a transmittance of over 99.9 percent at the 266nm wave band, has good spectral performance and good mechanical stability and stability, and can meet some high-end applications in the near ultraviolet field at present.)

1. A266 nm high-power laser antireflection film is characterized in that: the film layer structure is as follows: A/cL/bH/aL/SUB/aL/bH/cL/A, wherein SUB represents a glass substrate; a represents air; h represents a high refractive index film layer; l represents a low refractive index film layer; and a, b and c are coefficient theoretical values of the optical thickness of the quarter reference wavelength of each film layer respectively, wherein a is 1.6 +/-0.2, b is 0.53 +/-0.2, and c is 1.13 +/-0.2.

2. The 266nm high power laser antireflection film of claim 1, wherein: the high refractive index film layer is made of HfO2Or AL2O3

3. The 266nm high power laser antireflection film of claim 1 or 2, wherein: the low refractive index film layer is made of SIO2Or MgF2

4. The 266nm high power laser antireflection film of claim 1 or 2, wherein: the material used for the substrate is fused quartz, sapphire or calcium fluoride.

5. The 266nm high power laser antireflection film of claim 1 or 2, wherein: the physical thickness of the film layer is: aL is 75.44 + -7.5 nm, bH is 20 + -2 nm, and cL is 52.36 + -5.2 nm.

6. The preparation method of the 266nm high-power laser antireflection film as claimed in any one of claims 1 to 5, wherein the preparation method comprises the following steps: the method comprises the following steps:

(1) ultrasonic cleaning: ultrasonic cleaning is carried out to remove microscopic particles attached to the surface of the glass substrate;

(2) preparing a film: the method is characterized in that an electron beam or resistance thermal evaporation method is used for evaporation on a glass substrate, and high-purity oxygen is introduced into a vacuum chamber at the same time, so that the deposition material can be fully oxidized in a high vacuum state, wherein the purity of the high-purity oxygen is more than or equal to 99.99%.

7. The method of claim 6, wherein: in the step (2), before film formation, the substrate temperature is maintained at 350 ℃ for 250-.

8. The production method according to claim 6 or 7, characterized in that: in the step (2), Al is plated2O3Or HFO2When the gas filling amount of the high-purity oxygen is 10-180sccm, AL2O3Or HFO2The evaporation rate of (a) is 0.15-0.5 nm/s.

9. The production method according to claim 6 or 7, characterized in that: in the step (2), plating MgF2Without introducing high purity oxygen, MgF2The evaporation rate of (a) is 0.3-1.5 nm/s; deposition of SIO2When the gas filling amount of the high-purity oxygen is 10-150sccm, SIO2The evaporation rate of (a) is 0.3-1.5 nm/s.

10. The production method according to claim 6 or 7, characterized in that: in the step (2), during evaporation, an isolation baffle is added between the evaporation source and the glass substrate, and the isolation baffle is positioned below the glass substrate and above the evaporation source and used for blocking and adsorbing invalid evaporation materials.

Technical Field

The invention relates to a 266-nanometer high-power laser antireflection film and a preparation method thereof, belonging to the technical field of antireflection films.

Background

Ultraviolet laser has the advantages of short wavelength, high molecular energy, small diffraction effect and the like, and is widely applied to the fields of material processing, photoetching, medical treatment, scientific research and the like.

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 antireflection film of the ultraviolet laser product on the market at present has the problems of low transmittance, low light damage resistance threshold, poor use effect, short service life and the like.

Disclosure of Invention

The invention provides a 266nm high-power laser antireflection film and a preparation method thereof, the reflectivity of the obtained antireflection film at a 266nm wave band is less than 0.05%, the transmittance can reach more than 99.9%, the damage threshold of the anti-shock light is improved and can reach 6J/cm2(266nm,7 ns); the use effect and the service life of the product are improved; can meet the requirements of some high-end applications in the near ultraviolet field at present.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a266 nm high-power laser antireflection film, the film layer structure is: A/cL/bH/aL/SUB/aL/bH/cL/A, wherein SUB represents a glass substrate; a represents air; h represents a high refractive index film layer; l represents a low refractive index film layer; and a, b and c are coefficient theoretical values of the optical thickness of the quarter reference wavelength of each film layer respectively, wherein a is 1.6 +/-0.2, b is 0.53 +/-0.2, and c is 1.13 +/-0.2.

The reference wavelength is 266 nm.

According to the design and preparation method of the laser film with the high laser damage threshold in the ultraviolet band, the transmittance of the antireflection film at the 266nm band can reach more than 99.9%. The threshold value of the damage of the anti-light reaches 6J/cm2(266nm,7 ns); can meet the requirements of some high-end applications in the near ultraviolet field at present.

In order to further reduce the absorption of the antireflection film, the material of the high-refractive-index film layer is HfO2Or AL2O3(ii) a The low refractive index film layer is made of SIO2Or MgF2

The material used for the substrate is preferably fused quartz, sapphire, calcium fluoride or the like.

The preferred physical thicknesses of each film layer are: aL is 75.44 + -7.5 nm, bH is 20 + -2 nm, and cL is 52.36 + -5.2 nm.

The preparation method of the 266nm high-power laser antireflection film comprises the following steps:

(1) ultrasonic cleaning: microscopic particles attached to the surface of the glass substrate are removed through ultrasonic cleaning, so that the adhesiveness of the film layer is stronger;

(2) preparing a film, namely evaporating on a glass substrate by using an electron beam or resistance thermal evaporation method, and introducing high-purity oxygen into a vacuum chamber at the same time, so that the deposition material can be fully oxidized in a high vacuum state, wherein the purity of the high-purity oxygen is more than or equal to 99.99 percent, so as to reduce the absorption of the film and improve the laser damage resistance threshold; the method not only retains the unique favorable performance of the laser film prepared by the thermal evaporation method, but also improves the intrinsic absorption and defect density of the film, and has the characteristics of strong pertinence, high quality, simplicity and feasibility. And (3) during vapor deposition, plating one surface of the glass substrate, then repeating the step (2) to plate the other surface, and enabling the processes of double-surface film plating to be consistent.

The percentage of the purity of the high-purity oxygen is volume percentage.

The control of the conditions during the preparation of the film layers is very critical, the preparation conditions of each film layer not only influence the performance such as compactness of a single film layer, but also influence the binding force with an adjacent film layer and the optical performance of an integral film layer, preferably, in the step (2), before film formation, the temperature of the substrate is firstly kept at 350 ℃ of 250-; plating AL2O3When the gas filling amount of the high-purity oxygen is 10-180sccm, AL2O3The evaporation rate of (a) is 0.15-0.5 nm/s; plating AL2O3Or HFO2When the gas filling amount of the high-purity oxygen is 10-180sccm, AL2O3Or HFO2The evaporation rate of (a) is 0.15-0.5 nm/s; MGF plating2When it is used, high-purity oxygen, MgF, is not filled2The evaporation rate of (a) is 0.3-1.5 nm/s; plating SIO2When the gas filling amount of the high-purity oxygen is 10-150sccm, SIO2The evaporation rate of (a) is 0.5-1.5 nm/s.

In order to improve the quality of the antireflection film, in the step (2), during evaporation, an isolation baffle is added between the evaporation source and the glass substrate, and the isolation baffle is positioned below the glass substrate and above the evaporation source and used for blocking and adsorbing ineffective evaporation materials, so that the pollution near the glass substrate is reduced, and the probability of forming film defects is reduced.

The key factors causing damage in the laser film are absorption and defects in the film, and the defects of the film can be effectively reduced by the method.

The prior art is referred to in the art for techniques not mentioned in the present invention.

The 266-nanometer high-power laser antireflection film has a high laser damage resistance threshold value at an ultraviolet wave band, the transmittance of the antireflection film at the 266nm wave band can reach more than 99.9 percent, the damage resistance threshold value of the antireflection film is improved and can reach 6J/cm2(266nm,7ns), not only has good spectral performance but also has better mechanical stability and stability, improves the using effect of the product, prolongs the service life and can meet some high-end applications in the near ultraviolet field at present.

Drawings

FIG. 1 is a schematic structural view of a 266nm high-power laser antireflection film in example 1 of the present invention;

FIG. 2 is a graph showing a design curve of a 266nm high power laser antireflection film in example 1 of the present invention;

FIG. 3 is a graph of a detection spectrum of a 266nm high-power laser antireflection film in example 1 of the present invention, where a is a single-sided R%, and b is a double-sided T%;

in the figure, 1 is a fused quartz substrate, and 2 is MgF2Film layer, 3 is AL2O3Film layer, 4 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.

Example 1

As shown in fig. 1, the 266nm high power laser antireflection film has a film structure of: A/cL/bH/aL/SUB/aL/bH/cL/A, wherein SUB represents a fused quartz substrate; a represents air; h represents AL2O3A film layer; l represents MgF2A film layer; a, b and c are coefficients of quarter reference wavelength optical thickness of each film layer, a is 1.6, b is 0.53, c is 1.13, and each film layerThe physical thickness of the film is A/52.36nm/20nm/75.44nm/SUB/75.44nm/20nm/52.36nm/A in sequence.

The preparation method of the 266nm high-power laser antireflection film comprises the following steps:

(1) and (3) maintaining an evaporation environment: an isolation baffle is arranged between the evaporation source and the glass substrate to block and adsorb ineffective evaporation materials, so that the pollution near the glass substrate is reduced, and the probability of forming film defects is reduced;

(2) ultrasonic cleaning: removing microscopic particles attached to the surface of the glass substrate to make the film layer have stronger adhesiveness;

(3) in the step (2), before film formation, the substrate temperature is maintained at 260-270 ℃ and the constant temperature is kept for more than 40min, the substrate temperature is maintained at 260-270 ℃ in the film formation process, an electron beam (or resistance) thermal evaporation method is used for evaporation and MgF plating on a glass substrate2When in use, high-purity oxygen (more than or equal to 99.99 percent) is not introduced, and MgF2The evaporation rate of (3) is 0.6 nm/s; plating AL2O3When the aeration quantity of the high-purity oxygen is 100sccm and AL2O3The evaporation rate of (3) was 0.2 nm/s.

And (3) testing optical performance: the single-sided reflectivity and the double-sided transmittance of the film were measured by using a PHOTO RT spectrophotometer of white russia, as shown in fig. 2-3, the obtained spectral curve reached the design requirement, and the damage-resistant threshold reached 6J/cm2(266nm,7 ns). The steps are repeated for 3 times, and the product performance is not fluctuated.

Testing the environmental 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:

a. 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.

b. Adhesion force experiment: the adhesive tape with the width of 2cm and the peel strength I of more than 2.94N/cm is firmly adhered to the surface of the film layer, and after the adhesive tape is quickly pulled up from the edge of the part to the vertical direction of the surface, the film layer is repeatedly pulled for 25 times without falling off or damage.

c. Soaking test: and completely immersing the sample into distilled water or deionized water, wherein the film layer does not have the defects of new peeling, stripping, cracks, foaming and the like after 96 hours.

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