CN120255047A - A high-stability laser optical film based on an asymmetric multilayer high-reflective film and a preparation method thereof - Google Patents
A high-stability laser optical film based on an asymmetric multilayer high-reflective film and a preparation method thereof Download PDFInfo
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Abstract
本申请涉及光学薄膜技术领域，具体涉及一种基于非对称多层高反膜的高稳定性激光光学薄膜及其制备方法。在ER：YAG晶体或光学玻璃表面依次镀制首层Al2O3高硬度膜、周期性堆叠膜、末层Al2O3高硬度膜，周期性堆叠膜在半反射端和全反射端的交替次数为5次~15次，构成非对称膜系结构，形成从90%～99.98%的高反射率膜层，膜的抗损伤阈值、环境可靠性均满足光学薄膜国家标准，满足实用要求。
The present application relates to the field of optical thin film technology, and specifically to a high-stability laser optical thin film based on an asymmetric multilayer high-reflection film and a preparation method thereof. A first layer of Al 2 O 3 high-hardness film, a periodic stacked film, and a final layer of Al 2 O 3 high-hardness film are sequentially plated on the surface of an ER:YAG crystal or optical glass. The alternation number of the periodic stacked film at the semi-reflection end and the total reflection end is 5 to 15 times, forming an asymmetric film system structure, forming a high reflectivity film layer from 90% to 99.98%. The damage resistance threshold and environmental reliability of the film meet the national standards for optical thin films and meet practical requirements.
Description
Technical Field
The application relates to the technical field of optical films, in particular to a high-stability laser optical film based on an asymmetric multi-layer high-reflection film and a preparation method thereof.
Background
The mid-infrared laser generally refers to laser with the wavelength of 2-3 mu m, the wave band is positioned at a water absorption peak, and the water content of human tissues is more than 70%, so the laser has wide application in the medical cosmetology field. And plating a highly reflective film for a lasing substance (e.g., crystal) is a necessary condition for lasing. However, the band laser energy can absorb water molecules easily, so that the adhesive force and the damage resistance threshold of the film layer are difficult to reach the practical requirements.
The traditional film system structure is designed by adopting a TiO 2/SiO2 or HfO 2/SiO2 symmetrical film system, and has the problems that 1) the damage resistance threshold is low, so that the film is easy to thermally crack under high energy density, 2) the reliability is low, the film layer is degraded due to water vapor permeation in a damp and hot environment, and the reflectivity is remarkably attenuated despite the high refractive index contrast.
In view of the above, a high-stability laser optical film based on an asymmetric multi-layer high-reflection film and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a high-stability laser optical film based on an asymmetric multi-layer high-reflection film and a preparation method thereof, wherein a first Al 2O3 high-hardness film, a periodic stacked film and a last Al 2O3 high-hardness film are plated on the surface of an ER (ER) YAG crystal or optical glass in sequence, the alternation times of the periodic stacked film at a semi-reflection end and a total reflection end are 5-15 times, an asymmetric film system structure is formed, a high-reflectivity film layer of 90% -99.98% is formed, and the damage resistance threshold and the environmental reliability of the film meet the national standard of the optical film and meet the practical requirements. Solves the problems of lower damage resistance threshold and lower reliability in the prior art.
In order to solve the technical problems, the invention adopts the following scheme:
A high-stability laser optical film based on an asymmetric multi-layer high-reflection film comprises Al 2O3 high-hardness films positioned at the first layer and the last layer of a piece to be plated, a periodic stacking film between the first layer and the last layer, and a high-refractive-index Ta 2O5 film layer and a low-refractive-index SiO 2 film layer which are alternately stacked;
the alternation times of the periodic stacked film at the semi-reflection end and the total reflection end are 5 times to 15 times, so that an asymmetric film system structure is formed.
Further, in the periodic stack film, the number of alternations of the half reflective ends is 5 times, and the number of alternations of the total reflective ends is 15 times.
Further, in the Al 2O3 high-hardness film and the asymmetric film system structure, the thickness of each film layer is 230 nm-570 nm.
Further, the coating method adopts ion source sputtering.
A preparation method of a high-stability laser optical film based on an asymmetric multi-layer high-reflection film comprises the following steps:
s1, alcohol cleaning and vacuum pretreatment are carried out on a piece to be plated;
S2, ion source sputtering coating, namely filling argon gas for 20sccm, bombarding a piece to be coated for 15min-20 min by adopting an auxiliary ion source, then filling argon gas and oxygen gas, and sequentially sputtering and depositing an Al 2O3 film layer, a Ta 2O5 film layer and a SiO 2 film layer by adopting a main ion source;
S3, periodically stacking, namely repeatedly and alternately plating a Ta 2O5 film layer and a SiO 2 film layer on the semi-reflecting end and the total-reflecting end of the piece to be plated for 5 times to 15 times to form an asymmetric film system structure;
S4, preparing a surface packaging layer, namely sputtering and depositing an Al 2O3 film layer on the outermost layer;
S5, taking out the product after being cooled to 50 ℃ in vacuum, and obtaining the plated product plated with the asymmetric film system structure.
Further, in the step S1, the surface of the workpiece to be plated is cleaned by soaking absorbent cotton in alcohol, the workpiece to be plated is fixed on a vacuum chamber clamp, the workpiece to be plated is vacuumized until the cavity pressure is less than 10Pa, then is heated to 120 ℃ and is kept for 30min, and the background vacuum is below 4.0 multiplied by 10 -4 Pa.
Further, in the steps S2 and S4, the Al 2O3 film sputtering rate is 0.8A/S, the thickness is 225 nm-300 nm, the Ta 2O5 film sputtering rate is 0.8A/S, the thickness is 415 nm-430 nm, the SiO 2 film sputtering rate is 0.9A/S, and the thickness is 550 nm-570 nm.
Further, in step S3, the number of alternating stacks of the half reflective ends is 5 times and the number of alternating stacks of the total reflective ends is 15 times in the periodically stacked film.
Further, in the ion source sputtering coating, the vacuum chamber pressure is controlled to be 1.0X10 -2 Pa to 6.0X10 - 2 Pa, and the film thickness is monitored in real time by a crystal oscillator method.
Further, the part to be plated is ER YAG crystal or optical glass. YAG crystal is a high-quality crystal material for emitting laser with the wavelength of 2.94 mu m, and 2.94 mu m is positioned at a hydroxyl (-OH) absorption peak, can be strongly absorbed by biological tissues, and is widely applied to laser medical systems and other fields.
The application has the beneficial effects that the periodic stacked film is formed by alternately stacking the high refractive index Ta 2O5 film layer and the low refractive index SiO 2 film layer between the first layer and the last layer based on the specific Al 2O3 high-hardness film of the first layer and the last layer, the alternation times at the semi-reflecting end are 5 times and 15 times at the total-reflecting end, the damage-resistant threshold of the optical film can be obviously enhanced, the first Al 2O3 high-hardness film reduces the surface scratch risk, the last Al 2O3 high-hardness film prevents water vapor and oxygen from penetrating, inhibits the oxidation or hydrolysis of the inner film layer, and improves the environmental stability.
Drawings
FIG. 1 is a schematic diagram of the film structure of a part to be plated according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present invention fall within the protection scope of the present invention.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise.
Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description.
In addition, descriptions of well-known structures, functions and configurations may be omitted for clarity and conciseness. Those of ordinary skill in the art will recognize that various changes and modifications of the examples described herein can be made without departing from the spirit and scope of the present disclosure.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate.
In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
Example 1
The embodiment 1 of the application discloses a high-stability laser optical film based on an asymmetric multi-layer high-reflection film, which comprises an Al 2O3 high-hardness film positioned at the first layer and the last layer of a piece to be plated, wherein the Al 2O3 high-hardness film between the first layer and the last layer is formed by alternately stacking a high-refractive-index Ta 2O5 film layer and a low-refractive-index SiO 2 film layer;
The alternation times of the periodic stacked film at the semi-reflection end and the total reflection end are 5 times to 15 times, so that an asymmetric film system structure is formed. Wherein the number of alternations at the half reflective end is 5 times and the number of alternations at the total reflective end is 15 times. Meanwhile, in the Al 2O3 high-hardness film and the asymmetric film system structure, the thickness of each film layer is 230 nm-570 nm. The coating method adopts ion source sputtering.
The semi-reflecting end and the total reflecting end of the piece to be plated are plated with the Al 2O3 high-hardness film, the Al 2O3 high-hardness film and the Al 2O3 high-hardness film in sequence, wherein the alternating times of the semi-reflecting end and the total reflecting end are different to form an asymmetric film system structure, the high-refractive-index Ta 2O5 film layer and the low-refractive-index SiO 2 film layer are alternately stacked, the reflection efficiency is improved, and meanwhile, the damage-resistant threshold value is improved while the high reflectivity is ensured.
Al 2O3 high-hardness films are plated on the first layer and the last layer, the first layer Al 2O3 is in direct contact with the external environment, the high hardness and the wear resistance of the film resist laser-induced damage and particle scouring, the risk of surface scratch is reduced, and meanwhile, the film is used as a transition layer between YAG crystals or optical glass and a subsequent film, the interface stress is reduced, and the bonding strength with the high-refractive-index Ta 2O5 film is improved. The final Al 2O3 is used as a packaging layer, prevents water vapor and oxygen from penetrating, inhibits oxidation or hydrolysis of an internal film layer, improves the stability of a wet heat environment, and ensures that the finally obtained optical film has high damage resistance threshold and is reliable and strong.
Example 2
A preparation method of a high-stability laser optical film based on an asymmetric multi-layer high-reflection film comprises the following steps:
S1, alcohol cleaning and vacuum pretreatment are carried out on a piece to be plated (the piece to be plated is ER: YAG crystal or optical glass), absorbent cotton is soaked by alcohol to clean the surface of the piece to be plated, the piece to be plated is fixed on a vacuum chamber clamp, the piece to be plated is vacuumized until the cavity pressure is less than 10Pa, then is heated to 120 ℃ and is kept for 30min, and the background vacuum is below 4.0X10 -4 Pa.
S2, ion source sputtering coating, namely filling argon gas for 20sccm, bombarding a piece to be coated for 15min-20 min by adopting an auxiliary ion source, then filling argon gas and oxygen gas, and sequentially sputtering and depositing an Al 2O3 film layer, a Ta 2O5 film layer and a SiO 2 film layer by adopting a main ion source;
Wherein, the sputtering rate of the Al 2O3 film layer is 0.8A/s, and the thickness is 225 nm-300 nm;
Ta 2O5 film sputtering rate is 0.8A/s, and thickness is 415 nm-430 nm;
the sputtering rate of the SiO 2 film layer is 0.9A/s, and the thickness is 550 nm-570 nm.
In the ion source sputtering film plating, the vacuum chamber pressure is controlled between 1.0×10 -2 Pa and 6.0×10 -2 Pa, and the film thickness is monitored in real time by a crystal oscillation method.
S3, periodically stacking, namely repeatedly and alternately plating a Ta 2O5 film layer and a SiO 2 film layer on the semi-reflecting end and the total-reflecting end of the piece to be plated for 5 times to 15 times to form an asymmetric film system structure;
wherein the number of alternating stacks of half reflective ends is 5 times, and the number of alternating stacks of total reflective ends is 15 times
S4, preparing a surface packaging layer, namely sputtering and depositing an Al 2O3 film layer on the outermost layer, wherein the sputtering rate is 0.8A/S, and the thickness is 225-300 nm;
S5, taking out the product after being cooled to 50 ℃ in vacuum, and obtaining the plated product plated with the asymmetric film system structure.
Example 3
In this example 3, the film plating was performed on the basis of example 2, wherein the semi-reflective end film structure of the part to be plated was Al 2O3/（Ta2O5/SiO2）^5/Al2O3, the thickness of the film was 230 nm/(430 nm/570 nm)/(5/230 nm), i.e., the first and last layers of the semi-reflective end were Al 2O3, and the high refractive index Ta 2O55 film layer and the low refractive index SiO 2 film layer interposed between the first and last layers were alternately stacked 5 times to form a periodic stacked film.
The total reflection end film system structure is Al 2O3/（Ta2O5/SiO2）^15/Al2O3, the film thickness is 297 nm/(422 nm/561.9 nm)/(15/297 nm), namely the first layer and the last layer of the total reflection end are Al 2O3, and the high refractive index Ta 2O5 film layer and the low refractive index SiO 2 film layer between the first layer and the last layer are alternately stacked for 15 times to form a periodical stacked film.
Example 4
In this example 4, a film coating was performed on the basis of example 2, wherein the semi-reflective film structure of the part to be coated was Al 2O3/（Ta2O5/SiO2）^5/Al2O3, the film thickness was 227.3 nm/(418.8 nm/557.6 nm)/(5/227.3 nm), i.e., the first and last layers of the semi-reflective film were Al 2O3, and the high refractive index Ta 2O5 film and the low refractive index SiO 2 film between the first and last layers were alternately stacked 5 times to form a periodic stacked film.
The total reflection end film system structure is Al 2O3/（Ta2O5/SiO2）^15/Al2O3, the film thickness is 290 nm/(420 nm/558 nm)/(15/290 nm), namely, the first layer and the last layer of the total reflection end are Al 2O3, and the high refractive index Ta 2O5 film layer and the low refractive index SiO 2 film layer between the first layer and the last layer are alternately stacked for 5 times to form a periodical stacked film.
Example 5
In this example 5, the film plating was performed on the basis of example 2, wherein the semi-reflective film structure of the part to be plated was Al 2O3/（Ta2O5/SiO2）^5/Al2O3, the film thickness was 231.9 nm/(427.2 nm/568.8 nm)/(5/231.9 nm), i.e., the first and last layers of the semi-reflective film were Al 2O3, and the high refractive index Ta 2O5 film and the low refractive index SiO 2 film interposed between the first and last layers were alternately stacked 5 times to form a periodic stacked film.
The total reflection end film system structure is Al 2O3/（Ta2O5/SiO2）^15/Al2O3, the film thickness is 289 nm/(425 nm/563 nm)/(5/289 nm), namely the first layer and the last layer of the total reflection end are Al 2O3, and the high refractive index Ta 2O5 film layer and the low refractive index SiO 2 film layer between the first layer and the last layer are alternately stacked for 5 times to form a periodical stacked film.
Comparative example
The semi-reflective end film structure of the to-be-plated part of the comparative example is (ZNS/YBF 3)/(6), and the thickness is (350 nm/490 nm)/(6);
The total reflection end film system mechanism is (ZNS/YBF 3)/(15), the thickness is (350 nm/490 nm)/(15), and the plating method adopts vacuum electron beam evaporation. The half-reverse end is formed by alternately stacking a ZNS film layer and a YBF 3 film layer for 6 times, and the full-reverse end is formed by alternately stacking a ZNS film layer and a YBF 3 film layer for 15 times.
The coated article obtained in examples 3 to 5 and comparative example were subjected to semi-reflective end and total reflective end reflectance and energy value measurements as shown in Table 1 below.
Table 1 table of reflectivity and energy value of semi-reflective end and total reflective end in finished plated articles of examples 3-5 and comparative example
As can be seen from table 1, in examples 3 to 5, there was no significant difference in reflectivity between the half reflective end and the total reflective end, but the energy value was significantly improved, which indicates that the present application is based on the specific Al 2O3 high hardness films of the first and the last layers, and the periodic stacked films between the first and the last layers, which are formed by alternately stacking the high refractive index Ta 2O5 film layer and the low refractive index SiO 2 film layer, and the number of alternations at the half reflective end was 5 times and the number of alternations at the total reflective end was 15 times, which can significantly enhance the damage resistance threshold of the optical film, and also improve the environmental reliability of the film.
The present invention is not limited to the preferred embodiments, and the present invention is described above in any way, but is not limited to the preferred embodiments, and any person skilled in the art will appreciate that the present invention is not limited to the embodiments described above, while the above disclosure may be used to make some changes or modifications to equivalent embodiments, any simple modification, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention will still fall within the scope of the technical solutions of the present invention.
Claims (10)
1. The high-stability laser optical film based on the asymmetric multi-layer high-reflection film is characterized by comprising Al 2O3 high-hardness films positioned at the first layer and the last layer of a piece to be plated, and periodic stacked films between the first layer and the last layer, wherein the periodic stacked films are formed by alternately stacking high-refractive-index Ta 2O5 film layers and low-refractive-index SiO 2 film layers;
the alternation times of the periodic stacked film at the semi-reflection end and the total reflection end are 5 times to 15 times, so that an asymmetric film system structure is formed.
2. The high stability laser optical film based on asymmetric multi-layer high reflection film according to claim 1, wherein the number of alternations of half reflection ends in the periodic stack film is 5 times and the number of alternations of total reflection ends is 15 times.
3. The high-stability laser optical film based on an asymmetric multi-layer high-reflection film according to claim 1, wherein in the Al 2O3 high-hardness film and the asymmetric film system structure, the thickness of each film layer is 230-570 nm.
4. The high-stability laser optical film based on the asymmetric multi-layer high-reflection film according to claim 1, wherein the coating method adopts ion source sputtering.
5. A method for preparing a high-stability laser optical film based on an asymmetric multi-layer high-reflection film, which is characterized in that the high-stability laser optical film based on the asymmetric multi-layer high-reflection film as claimed in any one of claims 1 to 4 is adopted, and comprises the following steps:
s1, alcohol cleaning and vacuum pretreatment are carried out on a piece to be plated;
S2, ion source sputtering coating, namely filling argon gas for 20sccm, bombarding a piece to be coated for 15min-20 min by adopting an auxiliary ion source, then filling argon gas and oxygen gas, and sequentially sputtering and depositing an Al 2O3 film layer, a Ta 2O5 film layer and a SiO 2 film layer by adopting a main ion source;
S3, periodically stacking, namely repeatedly and alternately plating a Ta 2O5 film layer and a SiO 2 film layer on the semi-reflecting end and the total-reflecting end of the piece to be plated for 5 times to 15 times to form an asymmetric film system structure;
S4, preparing a surface packaging layer, namely sputtering and depositing an Al 2O3 film layer on the outermost layer;
S5, taking out the product after being cooled to 50 ℃ in vacuum, and obtaining the plated product plated with the asymmetric film system structure.
6. The method for preparing the high-stability laser optical film based on the asymmetric multi-layer high-reflection film according to claim 5, wherein in the step S1, absorbent cotton is soaked by alcohol to clean the surface of a piece to be plated, the piece to be plated is fixed on a vacuum chamber clamp, the piece to be plated is vacuumized until the cavity pressure is less than 10Pa, then the piece to be plated is heated to 120 ℃ for 30min, and the background vacuum is less than 4.0X10 -4 Pa.
7. The method for preparing the high-stability laser optical film based on the asymmetric multi-layer high-reflection film according to claim 5, wherein in the steps S2 and S4, the sputtering rate of the Al 2O3 film layer is 0.8A/S, the thickness is 225-300 nm, the sputtering rate of the Ta 2O5 film layer is 0.8A/S, the thickness is 415-430 nm, and the sputtering rate of the SiO 2 film layer is 0.9A/S, and the thickness is 550-570 nm.
8. The method for preparing a high-stability laser optical film based on an asymmetric multi-layer high-reflection film according to claim 5, wherein in step S3, the number of alternating stacks of half reflection ends is 5 times and the number of alternating stacks of total reflection ends is 15 times in the periodic stack film.
9. The method for preparing the high-stability laser optical film based on the asymmetric multi-layer high-reflection film according to claim 5, wherein in the ion source sputtering film plating process, the vacuum chamber pressure is controlled to be 1.0×10 -2 Pa to 6.0×10 -2 Pa, and the film thickness is monitored in real time by a crystal oscillation method.
10. The method for preparing the high-stability laser optical film based on the asymmetric multi-layer high-reflection film according to claim 5, wherein the to-be-plated piece is ER YAG crystal or optical glass.
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