CN115478252B - Non-interface high laser damage threshold film and preparation method thereof - Google Patents

Non-interface high laser damage threshold film and preparation method thereof Download PDF

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CN115478252B
CN115478252B CN202110668586.9A CN202110668586A CN115478252B CN 115478252 B CN115478252 B CN 115478252B CN 202110668586 A CN202110668586 A CN 202110668586A CN 115478252 B CN115478252 B CN 115478252B
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CN115478252A (en
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陈笑迎
游丽君
赵丽丽
宋力昕
王枫
郑刚
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694—Halides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
    • G02B27/0012—Optical design, e.g. procedures, algorithms, optimisation routines

Abstract

The invention relates to a non-interface high laser damage threshold film and a preparation method thereof. The preparation method comprises the following steps: for a film system structure with the total film layer number of N, N is more than or equal to 2; let the physical thickness of the nth layer be d n Dividing the nth layer into two small layers n with equal thickness a And n b The thickness of the two small layers is d n 2, wherein n a Near one side of the substrate, n b One side far away from the substrate; cleaning a substrate and drying the substrate in a clean room; respectively placing corresponding coating materials at the two evaporation source positions, and starting coating; and taking out the vacuum chamber after naturally cooling the vacuum chamber to the room temperature.

Description

Non-interface high laser damage threshold film and preparation method thereof
Technical Field
The invention relates to a preparation method for eliminating a film interface and improving a film laser damage threshold, in particular to a non-interface high laser damage threshold film and a preparation method thereof, and belongs to the field of optical films.
Background
The optical film is one of key elements in the laser system, and with the continuous development of a high-power laser system, the laser damage resistance of the optical film has become a bottleneck factor for limiting the further development of a strong laser technology, and the stability and the service life of the laser system are directly affected. A large number of experimental researches at home and abroad show that the defect density in the film is closely related to the laser damage threshold value. The existing optical film mostly adopts a film system structure with high and low refractive index materials which are alternately arranged, the thermal properties such as the refractive index, the absorption coefficient, the thermal conductivity and the like of the film can generate mutation at the interface of the film layer, so that the interface region has higher defects and impurity density, and according to the standing wave field theory, when laser interacts with the film, the extreme value of the electromagnetic field intensity is positioned at the interface of the film layer, and the problems of unmatched thermal property parameters of the material between the film layers, easy introduction of the interface effect such as the defects of the absorptive impurities and the like become key factors for restricting the improvement of the laser damage resistance of the film. Therefore, how to reduce the interface effect between the film layers and prepare a laser damage resistant film with higher performance has become a key problem to be solved. Researchers have made a great deal of research work on the influence of the film interface effect on the laser damage performance, and have tried to change the film thickness of the film so as to shift the position of the extreme value of the standing wave field to the film interface, but the method cannot thoroughly eliminate the influence of the film interface effect on the film laser damage performance.
Disclosure of Invention
Aiming at the problems, the inventor of the invention focuses on researching the bottleneck factor-film interface effect problem for limiting the improvement of the conventional multilayer film laser damage threshold, and the evaporation rate of the material is regulated and controlled linearly while the advantages of the electron beam evaporation method are maintained, so that the physical properties of the film continuously change along the normal direction of the film surface, no mutation is generated, the defect and impurity density are reduced, and the laser damage resistance of the film is improved.
In one aspect, the invention provides a method for preparing a non-interface high laser damage threshold film, which comprises the following steps:
(1) For a film system structure with the total film layer number of N (N is more than or equal to 2), setting the 1 st layer close to the substrate, and setting the N th layer as the outermost layer far away from the substrate;
(2) Let the physical thickness of the nth layer be d n Dividing the nth layer into two small layers n with equal thickness a And n b The thickness of the two small layers is d n 2, wherein n a Near one side of the substrate, n b One side far away from the substrate;
(3) Cleaning a substrate and drying the substrate in a clean room;
(4) Respectively placing corresponding coating materials at two evaporation source positions, wherein the background vacuum degree is less than or equal to 5 multiplied by 10 -3 Pa, etching the surface of the substrate for 5-10 min by using an ion source, wherein the baking temperature is 120-250 ℃, and the oxygen partial pressure is 0-5 multiplied by 10 -2 Pa；
(5) When n=1, the constant rate is first setPlating 1 st a A layer; when N is more than or equal to 2 and less than or equal to N, the (N-1) th part in the film system is steamed and plated simultaneously b Layer and nth a A layer. Setting the (n-1) b The initial rate of the layer is->By controlling the power of the electron gun to linearly change to 0 in the time t and simultaneously regulating the nth a The rate of the layer changes linearly from 0 to +.>n a Termination rate of layer and n b The layer start rate is the same, let->And satisfies the following: v (V) n ·t＝d n The method comprises the steps of carrying out a first treatment on the surface of the Finally, at a rate of V N Plating of the N b A layer; (6) And taking out the vacuum chamber after naturally cooling the vacuum chamber to the room temperature.
Preferably, the material of the coating material comprises oxide and fluoride.
Preferably, the oxide is HfO 2 、SiO 2 、SiO、Ta 2 O 5 、TiO 2 、MgO、Al 2 O 3 、Nb 2 O 5 、ZrO 2 、Y 2 O 3 At least one of (a) and (b); the fluoride is MgF 2 、LiF、LaF 3 、NaF、ThF 4 At least one of them.
Preferably, the substrate is glass, crystal or metal.
On the other hand, the invention also provides the interfacial-free high laser damage threshold film prepared by the preparation method.
The beneficial effects are that:
in the invention, under the condition of using the same coating material, the film layer interface in the conventional multilayer film is eliminated by controlling the linear change of the evaporation rate of the evaporation source, the continuous change of physical properties such as film components, refractive index and the like along the normal direction of the film surface is realized, and the defect source is reduced. Compared with the conventional multilayer film, the interface-free high laser damage threshold film prepared by the invention can obviously improve the laser damage threshold.
Drawings
Fig. 1 is a graph of evaporation rate change curves of a non-interface high laser damage threshold film and a corresponding conventional multilayer film in a plating process in example 1 and comparative example 1, wherein (a) is a time change curve of different evaporation source rates of the conventional 3-layer film, and (b) is a time change curve of different evaporation source rates of the non-interface high laser damage threshold film, taking the film layer number n=3 as an example;
FIG. 2 is a graph showing the comparison of laser damage threshold values of an interfacial-free high laser damage threshold film prepared by the present invention and a corresponding conventional multilayer film;
fig. 3 is a SEM picture of the cross-sectional structure of the actually prepared interfacial-free film and the conventional multilayer film, in example 1 and comparative example 1, wherein (a) is a picture of the cross-sectional structure of the conventional 3-layer film, and the interface of the film is clearly discernable, taking the n=3 number of films as an example; (b) The film components are continuously changed along the normal direction of the film surface in the picture of the interfacial-free film section structure. The brightness at the interface between the film and the substrate in (a) is caused by charge accumulation in a local area during the SEM section sample preparation and test.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
In the invention, aiming at the interface effect problems of unmatched material thermophysical parameters, easy introduction of absorptive impurity defects and the like at the interface of the conventional multilayer film layers, the deposition rate of the evaporation source is continuously and linearly regulated so as to ensure that the physical properties of the film continuously change along the normal direction of the film surface, no mutation is generated, the sources of film impurities and defects are reduced, and the laser damage threshold of the film is obviously improved.
The following illustrates an exemplary method for preparing the interfacial-free high laser damage threshold film.
The corresponding film system structure is designed according to the requirement of the laser protection band, and the film system is provided with N layers, so that the layer 1 is close to the substrate, and the layer N is the outermost layer. Let the physical thickness of the nth layer (N is any one of 1 to N) be d n Dividing the nth layer into two small layers n with equal thickness a And n b . The thickness of the two small layers is d n 2, wherein n a Near one side of the substrate, n b Away from the side of the substrate. In the same film structure, the high-folding materials can be selected from different types, and the low-folding materials can also be selected from different types.
The substrate is cleaned and dried in a clean room. The substrate is glass, crystal, metal, or the like.
Respectively placing coating materials at two evaporation source positions, wherein the background vacuum degree is less than or equal to 5 multiplied by 10 -3 Pa, etching the surface of the substrate for 5-10 minutes by using an ion source, wherein the baking temperature is 120-250 ℃, and the oxygen partial pressure is 0-5 multiplied by 10 -2 Pa。
When n=1, the constant rate is first setPlating 1 st a A layer; when N is more than or equal to 2 and less than or equal to N, the (N-1) th part in the film system is steamed and plated simultaneously b Layer and nth a A layer. Setting the (n-1) b The initial rate of the layer is->By controlling the power of the electron gun to linearly change to 0 in the time t and simultaneously regulating the nth a The rate of the layer changes linearly from 0 to +.>n a Termination rate of layer and n b The layer start rate is the same, let->And satisfies the following: v (V) n ·t＝d n The method comprises the steps of carrying out a first treatment on the surface of the Finally, at a rate of V N Plating of the N b Wherein the maximum rate of the oxide is in the range of 0.1 to 1nm/s and the maximum rate of the fluoride is in the range of 0.1 to 1.5nm/s.
And taking out the vacuum chamber after naturally cooling the vacuum chamber to the room temperature.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1:
taking 1064nm laser protection band as an example, designing the film layer number N=3 of the film system, wherein the 1 st layer and the 3 rd layer are made of TiO 2 Layer 2 is SiO 2 ，d 1 ＝d 3 ＝118nm，d 2 =184.1 nm; quartz glass is selected as a coating substrate, and is cleaned and dried in a clean room; siO is respectively put into the two evaporation source positions 2 And Ti is 3 O 5 Coating material, extracting background vacuum less than 5 x 10 -3 Pa, heating the substrate to 200 ℃; etching and cleaning the surface of the substrate for 10 minutes by using an ion source before evaporation;
plating 1 st at a constant rate of 0.25nm/s a A layer; then vapor deposition is carried out at the same time 1 st b Layer 2 a Layer, set 1 st b The initial rate of the layer was 0.25nm/s, which was linearly varied to 0 in 472s by controlling the electron gun power while regulating 2 nd a The rate of the layer was linearly varied from 0 to 0.39nm/s over 472 s; vapor deposition at the same time 2 nd b Layer 3 a Layer 2 b The initial rate of the layer was 0.39nm/s, which was linearly varied to 0 in 472s by controlling the power of the electron gun while regulating 3 rd a The rate of the layer was linearly varied from 0 to 0.25nm/s over 472 s; plating at a constant rate of 3 rd b A layer. And taking out the sample after the vacuum room temperature naturally cools to room temperature.
Laser damage experiments (test laser wavelength 1064nm, pulse width 12 ns) are carried out on the non-interface high laser damage threshold film prepared by the method and the conventional 3-layer film not prepared by the method, and as shown in a histogram of example 1 in fig. 2, the damage threshold of the non-interface high laser damage threshold film is obviously improved.
Example 2:
the number of the film layers of the designed film system is N=7, and the film coating material of the odd-numbered layers is Ta 2 O 5 The even layer material is SiO 2 Ta with 1064nm as reference wavelength 2 O 5 Layer thickness of 127.4nm, siO 2 The thickness of the layer is 184.1nm, quartz glass is selected as a coating substrate, and the coating substrate is cleaned and dried in a clean room; siO is respectively put into the two evaporation source positions 2 And Ta 2 O 5 Coating material, extracting background vacuum less than 5 x 10 -3 Pa, heating the substrate to 200 ℃; etching and cleaning the surface of the substrate for 10 minutes by using an ion source before evaporation;
plating at a constant rate of 0.27nm/s 1 st a A layer; vapor deposition at the same time 1 st b Layer 2 a Layer, set 1 st b The initial rate of the layer was 0.27nm/s, which was linearly varied to 0 in time 472s by controlling the electron gun power while regulating 2 nd a The rate of the layer is linearly varied from 0 over 472sAt 0.39nm/s; vapor deposition at the same time 2 nd b Layer 3 a Layer 2 b The initial rate of the layer was 0.39nm/s; by controlling the power of the electron gun to linearly change to 0 within the time 472s, and simultaneously regulating and controlling the 3 rd a The rate of the layer was linearly varied from 0 to 0.27nm/s over 472 s; repeating the above process until the vapor deposition is completed at the 7 th stage a A layer; finally plating at a constant rate 7 th b A layer. And taking out the sample after the vacuum room temperature naturally cools to room temperature.
Laser damage experiments (test laser wavelength 1064nm, pulse width 12 ns) are carried out on the non-interface high laser damage threshold film prepared by the method and the conventional 7-layer film not prepared by the method, and as shown in a histogram of example 2 in fig. 2, the damage threshold of the non-interface high laser damage threshold film is obviously improved.
Experiments show that the film layer interface effect is eliminated through the preparation of the film without the interface high laser damage threshold value, and the film laser damage threshold value is obviously improved.
Example 3
The number of the film layers of the designed film system is N=3, and the film coating material of the odd-numbered layers is HfO 2 The even layer material is SiO 2 With 532nm as reference wavelength, hfO 2 The thickness of the layer is 76.9nm, siO 2 The thickness of the layer is 92.0nm, quartz glass is selected as a coating substrate, and the coating substrate is cleaned and dried in a clean room; siO is respectively put into the two evaporation source positions 2 And HfO 2 Coating material, extracting background vacuum less than 5 x 10 -3 Pa, heating the substrate to 200 ℃; etching and cleaning the surface of the substrate for 10 minutes by using an ion source before evaporation;
plating 1 st at a constant rate of 0.2nm/s a A layer; then vapor deposition is carried out at the same time 1 st b Layer 2 a Layer, set 1 st b The initial rate of the layer was 0.2nm/s, which was linearly varied to 0 in 385s by controlling the electron gun power while regulating 2 nd a The rate of the layer was linearly varied from 0 to 0.24nm/s over 385 s; vapor deposition at the same time 2 nd b Layer 3 a Layer 2 b The initial rate of the layer was 0.24nm/s by controlling the electron gunThe power is linearly changed to 0 in 385s, and the 3 rd is regulated a The rate of the layer was linearly varied from 0 to 0.2nm/s over 385 s; plating 3 rd at constant rate of 0.2nm/s b A layer. And taking out the sample after the vacuum room temperature naturally cools to room temperature.
Laser damage experiments (test laser wavelength 532nm, pulse width 12 ns) are carried out on the non-interface high laser damage threshold film prepared by the method and the conventional 3-layer film not prepared by the method, and as shown in a histogram of example 3 in fig. 2, the damage threshold of the non-interface high laser damage threshold film is obviously improved.
Comparative example 1
The conventional 3-layer film system is Ta 2 O 5 /SiO 2 /Ta 2 O 5 Ta with 1064nm as reference wavelength 2 O 5 Layer thickness of 127.4nm, siO 2 The layer thickness was 184.1nm.
Comparative example 2
In a conventional 7-layer film system, the film coating material of the odd layer is Ta 2 O 5 The even layer material is SiO 2 . Ta with 1064nm as reference wavelength 2 O 5 Layer thickness of 127.4nm, siO 2 The layer thickness was 184.1nm.
Comparative example 3
The conventional 3-layer film system is HfO 2 /SiO 2 /HfO 2 With 532nm as reference wavelength, hfO 2 The thickness of the layer is 76.9nm, siO 2 The layer thickness was 92.0nm.

Claims (5)

1. The preparation method of the interfacial-free high laser damage threshold film is characterized by comprising the following steps of:
(1) For a film system structure with the total film layer number of N, N is more than or equal to 2, the layer close to the substrate is set to be the 1 st layer, and the N layer is the outermost layer far away from the substrate;
(2) Let the physical thickness of the nth layer be d n Dividing the nth layer into two small layers n with equal thickness a And n b The thickness of the two small layers is d n 2, wherein n a Near one side of the substrate, n b One side far away from the substrate;
(3) Cleaning a substrate and drying the substrate in a clean room;
(4) Respectively placing corresponding coating materials at two evaporation source positions, wherein the background vacuum degree is less than or equal to 5 multiplied by 10 -3 Pa, etching the surface of the substrate for 5-10 minutes by using an ion source, wherein the baking temperature is 120-250 ℃, and the oxygen partial pressure is 0-5 multiplied by 10 -2 Pa；
(5) When n=1, the constant rate is first setPlating 1 st a A layer; when N is more than or equal to 2 and less than or equal to N, the (N-1) th part in the film system is steamed and plated simultaneously b Layer and nth a A layer; setting the (n-1) b The initial rate of the layer is->By controlling the power of the electron gun to linearly change to 0 in the time t and simultaneously regulating the nth a The rate of the layer changes linearly from 0 to +.>n a Termination rate of layer and n b The layer start rate is the same, let->And satisfies the following: v (V) n ·t＝d n The method comprises the steps of carrying out a first treatment on the surface of the Finally, at a rate of V N Plating of the N b A layer;
(6) And taking out the vacuum chamber after naturally cooling the vacuum chamber to the room temperature.
2. The method according to claim 1, wherein the coating material comprises: oxides, fluorides.
3. The preparation method according to claim 2, wherein the oxide is HfO 2 、SiO 2 、SiO、Ta 2 O 5 、TiO 2 、MgO、Al 2 O 3 、Nb 2 O 5 、ZrO 2 、Y 2 O 3 At least one of (a) and (b); the fluoride is MgF 2 、LiF、LaF 3 、NaF、ThF 4 At least one of them.
4. A method of preparation according to any one of claims 1 to 3 wherein the substrate is glass, crystalline or metal.
5. An interfacial-free high laser damage threshold film prepared according to the method of any one of claims 1-4.
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