CN109991691A - Three wave band of laser anti-reflection films of one kind and preparation method thereof - Google Patents
Three wave band of laser anti-reflection films of one kind and preparation method thereof Download PDFInfo
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- CN109991691A CN109991691A CN201910297056.0A CN201910297056A CN109991691A CN 109991691 A CN109991691 A CN 109991691A CN 201910297056 A CN201910297056 A CN 201910297056A CN 109991691 A CN109991691 A CN 109991691A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims abstract description 28
- 238000002310 reflectometry Methods 0.000 claims abstract description 18
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 238000000869 ion-assisted deposition Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000007914 intraventricular administration Methods 0.000 claims description 3
- 238000010849 ion bombardment Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 abstract description 17
- 238000001228 spectrum Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000010408 film Substances 0.000 description 60
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 239000012528 membrane Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007735 ion beam assisted deposition Methods 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
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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
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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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
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- 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
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- Physics & Mathematics (AREA)
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- Optics & Photonics (AREA)
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- Surface Treatment Of Optical Elements (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of three wave band of laser anti-reflection films and preparation method thereof, three wave band of laser anti-reflection films, including basal layer have been sequentially depositing composite layer and MgF on basal layer2Layer；Composite layer includes the YF of alternating deposit3Layer and ZnSe layer, wherein basal layer and YF3Layer connects, MgF2Layer connects with ZnSe layer.Three wave band of laser anti-reflection films of the invention, single side reflectivity≤0.25% of single side reflectivity≤1% of 650nm wave band, 1570nm wave band, single side reflectivity < 0.25% of 10.6 mu m wavebands, meet the requirement of multiwavelength laser process equipment optical system, excellent optical performance, and film adhesion is strong, rub resistance is strong, water resistance and temperature tolerance are good, and existing good spectrum property has preferable mechanical steady performance and stability again；Prepare reproducible, process is simple to operation, easy to control.
Description
Technical field
The present invention relates to a kind of three wave band of laser anti-reflection films and preparation method thereof, belong to three wave band of laser anti-reflection film fields.
Background technique
Modern Vis/NIR analytical technology can make full use of the spectroscopic data of full spectral coverage or multi-wavelength to be divided
Analysis, has the characteristics that contain much information, speed is fast, favorable reproducibility, measures convenient, is widely used in food, agricultural, chemical industry and pharmacy etc.
Field.
In contemporary optics system, most of optical elements require plating antireflective film to reduce surface reflection, especially use
In particular surroundings to optical system, other than requiring film to have higher optical property, it is also necessary to can fight various badly to ring
Border.
However there is the problems such as easy layering, peeling, poor adhesive force in existing anti-reflection film, and there is no three wave band of laser to increase at present
The relevant report of permeable membrane.
Summary of the invention
In order to solve the problems, such as film layer layering, peeling, poor adhesive force, the existing good spectrum property of the film layer made has again
Preferable mechanical steady performance and stability, the present invention provide a kind of 10.6 μm of three wave band of laser anti-reflection film and
Preparation method.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of three wave band of laser anti-reflection films, including basal layer have been sequentially depositing composite layer and MgF on basal layer2Layer；It is compound
Layer includes the YF of alternating deposit3Layer and ZnSe layer, wherein basal layer and YF3Layer connects, MgF2Layer connects with ZnSe layer.
Applicant it has been investigated that, YF3Not only refractive index is low for film material, but also transparency range is also very wide, from visible light
To 14 μm, there is good optical property and processing performance, be a kind of fit closely low-index material；In addition MgF2 has
Hardness is high, good mechanical property, stable chemical performance, is not easy to deliquesce and corrode, it is mainly characterized by vacuum in terms of optical property
Visible light wave range has lower absorption, so outermost layer uses MgF2, the transmitance of film not only can be improved, moreover it is possible to make film
Layer is more resistant to friction；The YF that the application passes through specific structure3、ZnSe、MgF2The combination of three kinds of coating materials, so that anti-reflection film is in 650nm wave
Section single side reflectivity≤1%, 1570nm wave band single side reflectivity≤0.25%, 10.6 mu m waveband single side reflectivity <
0.25%, the requirement of multiwavelength laser process equipment optical system is met, and film adhesion is strong, rub resistance is strong,
Water resistance is strong, temperature tolerance is good, and existing good spectrum property has preferable mechanical steady performance and stability again.
In order to further increase the mechanical property and optical property of anti-reflection film, it is preferable that YF3The number of plies phase of layer and ZnSe layer
Deng being 4-6 layers.
Further preferably, YF3The number of plies of layer and ZnSe layer is 5 layers namely three wave band of laser anti-reflection films include basal layer,
The first YF has been sequentially depositing on basal layer3Layer, the first ZnSe layer, the 2nd YF3Layer, the second ZnSe layer, the 3rd YF3Layer, the 3rd ZnSe
Layer, the 4th YF3Layer, the 4th ZnSe layer, the 5th YF3Layer, the 5th ZnSe layer and MgF2Layer.
The mechanical property and optical property of anti-reflection film in order to balance, it is preferable that the first YF3The thickness of layer is less than the 2nd YF3Layer
Thickness, the 2nd YF3The thickness of layer is less than the 3rd YF3The thickness of layer, the 4th YF3The thickness of layer is between the first YF3The thickness of layer and the
Two YF3Between the thickness of layer, the 5th YF3The thickness of layer is less than the first YF3The thickness of layer；The thickness of first ZnSe layer is greater than second
The thickness of ZnSe layer, the thickness of third ZnSe layer are greater than the thickness of the first ZnSe layer, and the thickness of the 4th ZnSe layer is between first
Between the thickness of ZnSe layer and the thickness of third ZnSe layer, the thickness of the 5th ZnSe layer is between the thickness of the second ZnSe layer and first
Between the thickness of ZnSe layer, MgF2The thickness of layer is greater than the thickness of the 5th ZnSe layer, so mutual stress complementary effect of film layer
It is good, it can preferably guarantee the mechanical performance and spectrum property of anti-reflection film.The application thickness refers both to physics thickness when being not specifically noted
Degree.
In order to further enhance the complementary effect between each film layer, the 3rd YF3Layer with a thickness of the 5th YF3The thickness of layer
25-30 times；5-6 times of the thickness with a thickness of the second ZnSe layer of third ZnSe layer；3rd YF3Layer with a thickness of third ZnSe layer
3-4 times of thickness；MgF21.8-2.2 times of the thickness with a thickness of the 5th ZnSe layer of layer.
Cost and product quality requirement in order to balance, it is preferable that the first YF3Layer with a thickness of 204 ± 10nm, the first ZnSe layer
With a thickness of 420 ± 10nm, the 2nd YF3Layer with a thickness of 390 ± 10nm, the second ZnSe layer with a thickness of 270 ± 10nm, third
YF3Layer with a thickness of 5328 ± 10nm, third ZnSe layer with a thickness of 1500 ± 10nm, the 4th YF3Layer with a thickness of 246 ±
10nm, the 4th ZnSe layer with a thickness of 486 ± 10nm, the 5th YF3Layer with a thickness of 192 ± 10nm, the thickness of the 5th ZnSe layer
For 342 ± 10nm, MgF2Layer with a thickness of 690 ± 10nm.
Preceding 10 layers of YF in above structure, on basal layer3, two kinds of coating materials of ZnSe be used alternatingly, outermost layer use MgF2, raw
At structure: SUB/aNbHcNdHeNfHgNhHiNjHkM/A, wherein SUB represents basal layer, A represents air, N represents YF3Layer, M
Represent MgF2Layer, H represent ZnSe layer；A-k represents the coefficient of every layer a quarter reference wavelength (600nm) optical thickness, point
Not are as follows: 0.34,0.70,0.65,0.45,8.88,2.50,0.41,0.81,0.32,0.57,1.15.
The high-index material of common infrared band has ZnSe and ZnS, it is preferable that the application basal layer is ZnSe substrate
Layer.Since this membrane system wants small to the absorption of 10.6 mum wavelength light, 0.5-15 μm of ZnSe transparency range, scattering loss is extremely low, to heat
Therefore it is the preferred material for making infrared high power laser light membrane system that impact, which has very high ability to bear,.It is preferred that substrate thickness
Degree is 2 ± 0.2mm.
Three wave band of laser anti-reflection film of the application, is sequentially depositing composite layer and MgF on the base layer in a manner of vacuum evaporation2
Layer.
The preparation method of three wave band of laser anti-reflection film of the application, includes the following steps:
1) to YF3、ZnSe、MgF2Coating materials carries out independent fritting processing, removes the impurity inside coating materials；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force (1.8 ± 0.2) × 10 in vacuum intraventricular pressure-3Pa, baking
Under conditions of temperature is 100 ± 5 DEG C, composite layer and MgF are sequentially depositing on the surface of basal layer2Layer.
In order to improve the adhesive force of binding force and film layer between film layer, above-mentioned steps 2) in, it is assisted using Kaufman ion
Deposit composite layer and MgF2Layer.Applicant it has been investigated that, can increase gather density in this way, improve structural intergrity and stress
Match, thus improve the performance of film layer and use the time,
The ion source line of ion assisted deposition is preferably 20A.Ion assisted deposition is used in coating process, is effectively solved
Stress problem between film layer promotes the compactness of film layer, keeps film layer stronger, the service life is longer.
In order to further increase the adhesive force of film layer, the method clean substrate layer of ion bombardment is used in step 2).Application
People it has been investigated that, coefficient of concentration can be improved in this way, reinforce the adhesive force of film layer.
The application controls optical thickness using light-operated method, while controlling evaporation rate, the evaporation rate of YF3 using brilliant control method
The evaporation rate controlled in 0.4 ± 0.02nm/s, ZnS and MgF2 is controlled respectively in 0.25 ± 0.02nm/s and 0.7 ± 0.02nm/
s。
It includes three waves of Ke Jian Guang ﹑ near-infrared and LONG WAVE INFRARED that The present invention gives a kind of in the surface of zinc selenide vapor deposition
The structure and preparation method of the anti-reflection film of section, by ion assisted deposition, adjusting process parameter, obtained excellent optical performance,
Prepare that reproducible, film adhesion is strong, three wave band anti-reflection films of rub resistance, which reflects in the single side of 650nm wave band
Rate≤1%, 1570nm wave band single side reflectivity≤0.25%, 10.6 mu m waveband single side reflectivity < 0.25%, meet more
The requirement of wavelength laser process equipment optical system.
The unmentioned technology of the present invention is referring to the prior art.
Three wave band of laser anti-reflection films of the invention, single side reflectivity≤1%, the single side of 1570nm wave band of 650nm wave band are anti-
Single side reflectivity < 0.25% for penetrating rate≤0.25%, 10.6 mu m waveband meets multiwavelength laser process equipment optical system
Requirement, excellent optical performance, and film adhesion is strong, rub resistance is strong, and water resistance and temperature tolerance are good, existing good light
Spectrality can have preferable mechanical steady performance and stability again；Prepare reproducible, process is simple to operation, easy to control.
Detailed description of the invention
Fig. 1 is the structural schematic diagram (basal layer is eliminated in figure) of three wave band of laser anti-reflection films in embodiment 1；
Fig. 2 be embodiment 1 in three wave band of laser anti-reflection films 650nm wave band and 1570nm wave band single side reflectivity curve
(abscissa is wavelength nm, and ordinate is reflectivity %)；
Fig. 3 be in embodiment 1 three wave band of laser anti-reflection films in the single side reflectivity curve of 10.6 mu m wavebands (abscissa is wavelength
Nm, ordinate are reflectivity %)；
Fig. 4 be embodiment 1 in three wave band of laser anti-reflection films 650nm wave band and 1570nm wave band two-sided H103 resin
(abscissa is wavelength nm, and ordinate is transmitance %)；
Fig. 5 be in embodiment 1 three wave band of laser anti-reflection films in the two-sided H103 resin of 10.6 mu m wavebands (abscissa is wavelength
Nm, ordinate are transmitance %)；
In figure, a is the first YF3Layer, b are the first ZnSe layer, and c is the 2nd YF3Layer, d are the second ZnSe layer, and e is the 3rd YF3
Layer, f are third ZnSe layer, and g is the 4th YF3Layer, h are the 4th ZnSe layer, and i is the 5th YF3Layer, j are the 5th ZnSe layer, k MgF2
Layer；Basal layer is ZnSe basal layer, and 1 is basal layer side, and 2 be air side.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Using 800 type coating machine of southern light in lower example, crystalline substance control uses INFICON SQC-310 controller, is to utilize quartz
Crystal oscillation frequency changes to measure film quality thickness.The Kaufman ion source of nine chapter development of section, leads in ion source use
Rationally control ion energy is crossed, the consistency of deposition film can be improved, improves optically and mechanically performance.Vacuum chamber leans on mechanical pump
The vacuum degree for cooperating to obtain requirement of experiment with diffusion pumping system, measures vacuum degree with thermocouple needle.
Embodiment 1
As shown in Figure 1, a kind of three wave band of laser anti-reflection films, including basal layer, including basal layer, it is sequentially depositing on basal layer
There is the first YF3Layer, the first ZnSe layer, the 2nd YF3Layer, the second ZnSe layer, the 3rd YF3Layer, third ZnSe layer, the 4th YF3Layer, the
Four ZnSe layers, the 5th YF3Layer, the 5th ZnSe layer and MgF2Layer；Basal layer is ZnSe basal layer.
ZNSE base layer thickness is 2mm, the first YF3Layer with a thickness of 204nm, the first ZnSe layer with a thickness of 420nm, the
Two YF3Layer with a thickness of 390nm, the second ZnSe layer with a thickness of 270nm, the 3rd YF3Layer with a thickness of 5328nm, the 3rd ZnSe
Layer with a thickness of 1500nm, the 4th YF3Layer with a thickness of 246nm, the 4th ZnSe layer with a thickness of 486nm, the 5th YF3The thickness of layer
Degree be 192nm, the 5th ZnSe layer with a thickness of 342nm, MgF2Layer with a thickness of 690nm.
The preparation method of above-mentioned three wave band of laser anti-reflection film, includes the following steps:
1) to YF3, ZnSe and MgF2Coating materials carries out independent fritting processing, removes the impurity inside coating materials；
2) before plated film, the ion bombardment of 5min is carried out to substrate, it is therefore an objective to which cleaning substrate improves coefficient of concentration, strengthening membrane
The adhesive force of layer, is subsequently placed in vacuum chamber, is by force 1.8 × 10 in vacuum intraventricular pressure-3Pa, the condition that baking temperature is 100 DEG C
Under, composite layer and MgF are sequentially depositing on the surface of basal layer2Layer, it is auxiliary using Kaufman ion source during film deposition
Deposition is helped, gather density is increased, improves structural intergrity and Stress match, thus improve the performance of film layer and use the time,
Optical thickness is controlled using light-operated method, while evaporation rate, source parameters setting are as follows: acceleration voltage are controlled using brilliant control method
250V, plate voltage 400V, line 20mA, YF3Evaporation rate control in 0.4nm/s, the evaporation rate control of ZnS exists
0.25nm/s, MgF2Evaporation rate control in 0.7nm/s.
Using the PHOTO RT spectrophotometer of Byelorussia and the Spectrum100 infrared spectrometer pair of PE company, the U.S.
The single side reflectivity of film is thrown in above-mentioned increasing and two-sided transmitance is tested, and the obtained curve of spectrum reaches design requirement, sees figure
2-5。
Embodiment 2
A kind of three wave band of laser anti-reflection films, including basal layer, including basal layer have been sequentially depositing the first YF on basal layer3
Layer, the first ZnSe layer, the 2nd YF3Layer, the second ZnSe layer, the 3rd YF3Layer, third ZnSe layer, the 4th YF3Layer, the 4th ZnSe layer,
5th YF3Layer, the 5th ZnSe layer and MgF2Layer；Basal layer is ZnSe basal layer.
ZNSE base layer thickness is 2mm, the first YF3Layer with a thickness of 206nm, the first ZnSe layer with a thickness of 423nm, the
Two YF3Layer with a thickness of 394nm, the second ZnSe layer with a thickness of 265nm, the 3rd YF3Layer with a thickness of 5325nm, the 3rd ZnSe
Layer with a thickness of 1502nm, the 4th YF3Layer with a thickness of 249nm, the 4th ZnSe layer with a thickness of 488nm, the 5th YF3The thickness of layer
Degree be 195nm, the 5th ZnSe layer with a thickness of 345nm, MgF2Layer with a thickness of 692nm.
To film obtained by above-mentioned each example according to the requirement of GJB2485-95 optical film layer general specification, following environment examination is carried out
It tests:
(1) wear-resistant strength is tested: being wrapped up in 2 layers of drying defatted gauze outside rubber friction head, is kept under 4.9N pressure along same
One track rubs to film layer, and round-trip 40 times, film layer is without scratch equivalent damage.
(2) adhesive force is tested: the 3M adhesive tape for being 1cm with width is cemented in film surface, by adhesive tape from the edge court of part
The rapid pull-up of the vertical direction on surface, film layer nothing fall off, are not damaged.
(3) soak test: sample is completely immersed in distilled water or deionized water, and film layer is without exception after 96 hours.
(4) hot test: being raised to 150 DEG C of constant temperature from room temperature and toast 1 hour, then be down to room temperature, so continue cycling through twice,
Film layer is without exception.
The present invention solves film inter-laminar stress and film layer using ion beam assisted deposition by the reasonable selection of coating materials
Adhesive force, the existing good spectrum property of the film layer made has preferable mechanical steady performance and stability again.
Claims (10)
1. a kind of three wave band of laser anti-reflection films, it is characterised in that: including basal layer, be sequentially depositing on basal layer composite layer and
MgF2Layer；Composite layer includes the YF of alternating deposit3Layer and ZnSe layer, wherein basal layer and YF3Layer connects, MgF2Layer and ZnSe layer
Connect.
2. three wave band of laser anti-reflection film as described in claim 1, it is characterised in that: YF3Layer is equal with the number of plies of ZnSe layer,
It is 4-6 layers.
3. three wave band of laser anti-reflection film as claimed in claim 2, it is characterised in that: including basal layer, successively sink on basal layer
Product has the first YF3Layer, the first ZnSe layer, the 2nd YF3Layer, the second ZnSe layer, the 3rd YF3Layer, third ZnSe layer, the 4th YF3Layer,
4th ZnSe layer, the 5th YF3Layer, the 5th ZnSe layer and MgF2Layer.
4. three wave band of laser anti-reflection film as claimed in claim 3, it is characterised in that: the first YF3Layer with a thickness of 204 ± 10nm,
First ZnSe layer with a thickness of 420 ± 10nm, the 2nd YF3Layer with a thickness of 390 ± 10nm, the second ZnSe layer with a thickness of 270
± 10nm, the 3rd YF3Layer with a thickness of 5328 ± 10nm, third ZnSe layer with a thickness of 1500 ± 10nm, the 4th YF3The thickness of layer
Degree be 246 ± 10nm, the 4th ZnSe layer with a thickness of 486 ± 10nm, the 5th YF3Layer with a thickness of 192 ± 10nm, the 5th ZnSe
Layer with a thickness of 342 ± 10nm, MgF2Layer with a thickness of 690 ± 10nm.
5. the three wave band of laser anti-reflection films as described in claim 1-4 any one, it is characterised in that: basal layer is ZnSe substrate
Layer, base layer thickness are 2 ± 0.2mm；Single side reflectivity≤1%, the 1570nm wave band of three wave band of laser anti-reflection film 650nm wave bands
Single side reflectivity≤0.25%, 10.6 mu m wavebands single side reflectivity < 0.25%.
6. the preparation method of three wave band of laser anti-reflection films described in claim 1-5 any one, it is characterised in that: steamed with vacuum
The mode of hair is sequentially depositing composite layer and MgF on the base layer2Layer.
7. preparation method as claimed in claim 6, characterized by the following steps:
1) to YF3, ZnSe and MgF2Coating materials carries out independent fritting processing, removes the impurity inside coating materials；
2) it after cleaning basal layer, is placed in vacuum chamber, is by force (1.8 ± 0.2) × 10 in vacuum intraventricular pressure-3Pa, baking temperature
Under conditions of 100 ± 5 DEG C, composite layer and MgF are sequentially depositing on the surface of basal layer2Layer.
8. preparation method as claimed in claim 7, it is characterised in that: multiple using Kaufman ion assisted deposition in step 2)
Close layer and MgF2Layer.
9. preparation method as claimed in claim 8, it is characterised in that: ion source line is 20A.
10. preparation method as claimed in claim 8 or 9, it is characterised in that: clear using the method for ion bombardment in step 2)
Clean basal layer；YF3Evaporation rate control in 0.4 ± 0.02nm/s, the evaporation rate control of ZnS in 0.25 ± 0.02nm/s,
MgF2Evaporation rate control in 0.7 ± 0.02nm/s.
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