CN104062693B - The preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three - Google Patents
The preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three Download PDFInfo
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Abstract
A kind of preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three proposed by the present invention, utilize this method, the laser damage threshold of lithium niobate antireflective coating in optical parametric oscillation mid-infrared laser device can be significantly increased, bears the 1065nm laser of 100 MJs of magnitudes, ensures laser stabilization work.The technical scheme is that：Thin-film material is selected based on middle infrared coating materials, ZnS is chosen as high-index material, in CaF2、YF3、YbF3Middle screening low-index material, using 1065nm as Film Design reference wavelength, on computers, design three wave band antireflective coatings；Using full-automatic coating machine, the template contral file that the coating machine automatically controls is produced；Quartz crystal oscillator is calibrated according to material experiment result, load selected Coating Materials in coating machine, the making that the three wave band antireflective coating antireflective coatings that near, middle infrared band has high laser damage threshold are made on lithium niobate is automatically performed by selected template contral file.
Description
Technical field
The present invention relates to it is a kind of be mainly used in 1065nm optical parameter oscillating lasers produce mid-infrared laser laser system,
Being obtained simultaneously on lithium columbate crystal has high laser damage threshold and 1040-1080nm, 1400-1600nm, 3000-
The preparation method that the antireflective coating blooming piece of reflectivity is reduced on tri- wave bands of 4000nm.
Background technology
Laser has four big optical characteristics of same tropism, high brightness, monochromaticjty and high-energy-density.Because its is relatively common
The special characteristics of light, laser and its application system serve more and more important effect in modern social development, extensively
Applied to various civil and military fields., will in order to reach system design in the optical system of laser and its application system
Ask, the optical element that light path is passed through in system, which is typically necessary, is coated with optical thin film.So-called optical thin film, refer to choose difference
The Coating Materials of light refractive index, the thickness for being calculated different coating materials by optical principle using the method physically or chemically deposited
With the surface for being deposited in order in membrane component to be plated, element is set finally to obtain the optical property with system requirements.
A kind of very important solid state laser is optical parametric oscillator laser in laser system, mid-infrared laser light source
It is the focus of current laser technology research, all solid state optical parameter oscillating laser is widely used in photoelectronic warfare, laser radar, thing
Physicochemical and biological spectrum analysis, optics frequency dividing and and frequency, quantum optices, the generation of THz electric field, the three primary colours based on RGB
The fields such as display system.A traditional 1065nm near-infrared basic frequency laser light source is needed in this laser, is passing through niobic acid
The nonlinear effect of light laser and crystal during crystalline lithium（Optical parametric oscillator）, produce 1400-1600nm, 3000-4000nm
Infrared laser.
Lithium niobate is key element in above-mentioned laser system, process conditions and coating process when being grown due to lithium niobate
Limitation, antireflective coating is coated with lithium niobate three main performance index：
1. laser damage threshold.Being used after lithium niobate plated film in light laser light path, the laser damage threshold of film is minimum,
The damage of film can cause whole system to fail, and laser output declines can not even work completely, laser fails.Film swashs
Light injury threshold requirement can bear the energy in laser cavity.
2. residual reflectivity.The refractive index n of lithium niobate is up to 2.2, and in the case of not plated film, one side residual reflectivity reaches
14%, it is two-sided to there is about 28% light to be reflected, the efficiency of laser is largely effected on, residual reflectivity should be more low better.
3. service band width.According to the application requirement of antireflective coating, membrane system has three different service bands, is applied to
The 1065nm wave bands of basic frequency laser, the 1400-1600nm wave bands and 3000-4000nm wave bands of optical parametric oscillation.
The antireflective coating commonly used in laser system is all based on the optical interference film of principle of optical interference design.Routine subtracts
The material that reflectance coating chooses two kinds of different refractivities is defined as H, refractive index as thin-film material, the wherein high material of refractive index
Low material is defined as L, two kinds of material alternating deposits.Typically antireflective coating structure is：Substrate/(aHbL) ^m/ air, its
Middle m is positive integer, and a, b are respectively coefficient, and its unit thickness is antireflecting coating design reference wavelength 1065nm a quarter, its
Specific value depends on needing the index request for obtaining product, and a, b can be different in each layer, the total number of plies of membrane system and service band
Width it is relevant with the size of residual reflectivity.Existing technology has the defects of following：
1. resisting laser damage ability, threshold value are low.The defects of due to Crystal Growth of Lithium Niobate technique, plane of crystal have one
A little defects and non-stoichiometric composition, these defects, which are wrapped in film layer, after plated film forms plethora, reduces the laser of crystal
Damage threshold；Coating process control is bad, and the radiation of electron gun can cause film-forming temperature to raise, and lithium niobate holds at a certain temperature
Coring phenomenon easily occurs, defect and light laser interaction are formed on surface to be damaged.Mid-infrared light parametric oscillation
Laser works can be counted on one's fingers in mid infrared region, the thin-film material of middle infrared transparent, in the majority with sulfide, fluoride, technique
Process control is bad to cause thin-film material to decompose, and increase film layer absorbs, and causes thin film damage.The light of many document reports at present
Parametric oscillation mid-infrared laser device is the damage from laser for avoiding plated film rear film, often uses not technical scheme as plated film,
Exchange the steady operation of laser for using energy loss as cost.
2. spectral characteristic is poor.Caused by the aspect reason of design and processes two, such application is less at present, across three ripples
Section requires high to the design and processes process control difficulties of film, and membrane system uses in 1065nm laser, it is necessary to considers material
Anti- laser activity, middle infrared film system is thick, need to consider the stress characteristics of material, limit the selection of thin-film material, especially outermost
The refractive index of layer material directly affects the spectrum property of membrane system, and more preferable spectral characteristic requires more film layer numbers, but leads simultaneously
The stress increase of membrane system is caused, is seriously that film layer can come off.The combination of lithium niobate and many materials is bad, it is necessary to increase transition zone,
This considerably increases design and the difficulty made.When the wave band of leap is very wide, the dispersion of thin-film material is also to influence spectrum
Principal element, it is difficult to the accurate refractive index for determining thin-film material with the photometry or envelope method of routine in infrared region.
During the actual fabrication of optical thin film, can will plated film the work piece carrying tray that is placed in above coating materials to be evaporated of workpiece
In.The thickness of film comes conventionally by the intensity of the transmission or reflection optical signal of monitoring piece with the change of coating materials deposit thickness
Plated film process is controlled, this method is conventional optical monitor, and advantage is that reference wavelength is stable, and membrane system will not drift about, but
In infrared optical monitoring system it is very immature on home-made machine.The characteristics of quartz crystal monitoring method is can to monitor arbitrarily
The membrane system of thickness, every layer of error is independently cumulative, but this method is the indirect method of measurement, right with vacuum and temperature change
The stability requirement of coating machine is higher.
Meanwhile multiband antireflective coating film material is more than conventional antireflective coating, three kinds of materials to adjust three instruments because
Son, the requirement of control accuracy is also higher during to plated film.The careless slightly balance that may be influenceed in multiple wave bands in coating process,
Cause product residual reflectivity is excessive on a certain wave band and scrap.How to be controlled during actual plated film and reduce error, will largely
The upper product quality for determining to obtain.
The content of the invention
The purpose of the present invention be in view of the shortcomings of the prior art part, propose a kind of high laser damage threshold, it is low residual
Coreflection, the laser damage threshold of lithium niobate antireflective coating in optical parametric oscillation OPO mid-infrared laser devices can be significantly increased, is held
By the 1065nm laser of 100 MJs of magnitudes, the manufacture method of three wave band lithium niobate antireflective coatings of guarantee laser stabilization work.
The above-mentioned purpose of the present invention can be reached by following measures, a kind of wave band anti-reflection of resisting laser damage lithium niobate three
Penetrate film（Hereinafter referred to as antireflective coating）Preparation method, it is characterised in that comprise the following steps：
（1）It is determined that theoretical membrane system, with optical interference film theory for film structure design basis, chooses ZnS and is rolled over as high
Penetrate rate material, fluorination ytterbium YbF3For low-index material, the design reference wavelength using 600nm as antireflective coating, define respectively
ZnS、Al2O3And YbF3Unit optical thickness in λ/4 is H, M and L, increases by one layer of Al in antireflective coating substrate surface2O3Layer, make
For Stress match and resisting laser damage layer, on computers, using Film Design software Essential Macleod, according to
The wave band antireflective coating antireflective of 1065nm, 1400-1600nm, 3000-4000nm tri- requires to determine film structure；
（2）Using complete with quartz crystal vibration film-thickness monitoring, the high accuracy based on configuration software and PLC hardware controls
Auto Plating-film Machinery, and according to the theoretical film structure of above-mentioned acquisition, produce the template contral text that the coating machine automatically controls
Part；
（3）Load above-mentioned selected Coating Materials in coating machine, steamed using resistance and electron gun mixes the deposition side evaporated
Formula, coating machine are automatically performed the making of antireflective coating by selected template contral file.
The present invention has following beneficial effect compared to prior art.
The present invention is using Optimac Automatic Optimal Designs method as fundamental optimum design method, in existing antireflective coating technology base
On plinth, using increase Al2O3The method of transition zone, solve lithium niobate surface it is near, in infrared three wave band of laser antireflective coating ask
Topic, membrane system can bear the energy of 100 MJs of level 1065nm laser, improve YbF3Adhesive force, also reduce the table of lithium niobate
Susceptibility of the planar defect to 1065nm laser.
Improve the process for plating of antireflective coating.The present invention obtains simultaneously on lithium columbate crystal has high laser deflection
The blooming piece of reflectivity is reduced in value and tri- wave bands of 1040-1080nm, 1400-1600nm, 3000-4000nm.According to more
The experience of secondary result of the test, by strictly controlling the temperature of film forming, segregation phenomena of the lithium niobate in film forming procedure is reduced, protected
The laser damage threshold of membrane system is demonstrate,proved, after damage from laser experiment, the observation of laser confocal scanning microscope image shows, laser
Damage from lithium niobate lower face it is deeper the defects of originate, i.e. the volume defect of lithium niobate causes rather than from film and crystalline substance
The starting of body surface face.
The random error analysis of coupled computer software proves, uses the process control method of the invention formulated, Ke Yiyou
The negative effect of effect control random error, obtains the actual product being consistent with Theoretical Design（Such as Fig. 3,4）.
The present invention uses primary method of control of the quartz crystal film-thickness monitoring as film thickness, is commonly used in visible region
Although light-operated method control it is Wavelength stabilized, it is low compared with visible ray in the precision and stability of middle infrared band PbS detectors,
The precision of infrared monitoring is bad.Secondly, ZnS is steamed using resistance, Al2O3And YbF3Using the method for electron gun evaporation, ensure that
ZnS is not decomposed to be stablized with Tooling factor, has preferably repeatability
The present invention uses the Optimac optimization methods of Essential Macleod softwares, devises lithium niobate LiNbO3On
The wave band antireflective coating of 1040-1080nm, 1400-1600nm, 3000-4000nm tri- of low residual reflectivity.In actual fabrication process
In, thickness is controlled using quartz crystal film-thickness monitoring, actually obtains lithium niobate LiNbO3On above-mentioned three wave bands antireflective
Film, more than 100 MJs of 1065nm laser can be born, solves lithium niobate LiNbO substantially3On be coated with the technology of such membrane system and ask
Topic, the development and production of centering infrared laser light source have very high practical value.Using this method, beche-de-mer without spike can be significantly increased
The laser damage threshold of lithium niobate antireflective coating, the 1065nm for bearing 100 MJs of magnitudes swash in amount vibration OPO mid-infrared laser devices
Light, ensure laser stabilization work.
Brief description of the drawings
Fig. 1 is that the three wave band antireflective coating theories of the invention for working in 1065nm, 1400-1600nm, 3000-4000nm are set
Index contour schematic diagram.
Simulated spectra curve synoptic diagram during Fig. 2 thickness random errors 0.03.
The near-infrared curve synoptic diagram of the test result for the actual product that Fig. 3 is coated with according to present invention process.
Infrared curve synoptic diagram in the test result for the actual product that Fig. 4 is coated with according to present invention process.
Embodiment
Refering to Fig. 1.According to the present invention high damage threshold lithium niobate antireflective coating preparation method,
（1）It is determined that theoretical membrane system, chooses zinc sulphide ZnS as high-index material, fluorination ytterbium YBF3For low-refraction material
Material, alundum (Al2O3) Al2O3For middle refraction materials, ZnS, Al are defined respectively2O3And YBF3Unit optical thickness in λ/4 is
H, M and L, thicknesses of layers determine according to experimental thin films pulling experiment and damage from laser experiment.On computers, using Film Design
Software Essential Macleod, the initial configuration of membrane system is determined according to the performance parameter of the antireflective of three wave bands requirement；Thin
In the design of film, constraints is in lithium niobate and the 1st layer of YBF3Between have one layer of Al2O3Layer.
（2）Using with quartz crystal vibration film-thickness monitoring, the full-automatic plated film with configuration software and PLC hardware
Machine, according to the theoretical film structure of above-mentioned acquisition, produce the template contral file that the coating machine automatically controls；
（3）Load selected Coating Materials in coating machine, ZnS is using resistance steaming mode, Al2O3And YBF3Using electron beam
Evaporation mode, coating machine are automatically performed the making of antireflective coating by selected template contral file.
In order to solve lithium niobate LiNbO3The adhesive force of upper plated film and the needs for improving laser damage threshold, can be used
Cross material oxidation aluminium Al2O3, product can bear adhesive tape and pull after plated film, and specific thickness is tested by damage from laser and determined, by oxygen
Change aluminium Al2O3The constraints that thickness optimizes as film design, i.e., aluminum oxide thickness is not optimized, to 1040-1080nm, 1400-
1600nm, 3000-4000nm residual reflectivity establish design object function, if reflectivity R (λi) desired wavelength point reflection
Rate, residual reflectivity R ' (λi) be theoretical wavelength point residual reflectivity, wiFor any wavelength points weight, then quadratic sum Σ wi (R
(λi)-R’(λi))2For optimizing evaluation function, it is contemplated that theory target reflectivity is 0 on three wavelength, and is optimized on three wavelength
Degree it is consistent, weight should be consistent, weight wiUniformly be set to 1, near-infrared cultellation density is 5nm, in it is infrared be 40nm.It is first
First, ZnS is chosen as high-index material H, Al2 O3For middle refraction materials M, YbF3For low-index material L, with wavelength X
For 1065nm, ZnS, Al are defined respectively2 O3、YbF3Unit optical thickness in λ/4 is H, M and L, then determines initial membrane system, if
Membrane system initial configuration is lithium niobate/MHLHL/ air, using 5-11 layers as initial membrane system, is optimized respectively.The property of antireflective coating
Energy parameter is that the average residual reflectivity of passband is less than 1%.On computers, using Film Design software Essential Macleod
Above-mentioned H/M/L is simulated, by 5 layers, 7 layers, 9 layers, 11 layers separately design out some film structures, according to control method
It is required that the method screened by random error, chooses an optimal Film Design.Membrane system selection principle be：Meet that design is residual
The requirement of coreflection rate, small without ultra-thin super thick layer, random errors affect, the film structure for finally determining antireflective coating is：
Three wave band antireflective coating substrates/Stress match layer and antibody Monoclonal transition zone/optics antireflection film system/air.That is niobium
The film structure of sour lithium antireflective coating is：
Substrate/0.12M4.056H1.054M0.837H1.605L0.534H3.123L/ air, design reference wavelength
600nm.Base material is lithium niobate, and spectrum dimmer reflecting scope 1040-1080nm, 1400-1600nm, 3000-4000nm is average
Residual reflectivity is less than 1%, and laser damage threshold is more than 3J/cm2。
It will be seen from figure 1 that the last 7 layers of antireflective coating Theoretical Design residual reflectivity spectrogram preferably gone out.In Fig. 2 institutes
Show in the residual reflectivity distribution map simulated with the thickness random error of relative error 0.03, it can be seen that such with chance error
Under difference, the theoretical curve of film still meets design requirement, designs the tolerance and manufacturability having had.
During antireflective coating actual fabrication, using with quartz crystal vibrate film-thickness monitoring XTC2, it is engineered after by " group
State king " software and the full-automatic coating machine of Siemens S7-300 PLC control, film thickness monitoring software is self-developing.Then, according to
The theoretical membrane system of acquisition and the Tooling factor of coating machine, film structure file is exported from Essential Macleod softwares（It is defeated
Go out to the CSV formatted file compatible with EXCEL）, by thickness and film structure data copy to EXCEL template files（For
The normative document of TXX550 coating machine control systems）, TXT format text files are converted to by special switching software, it is counted
Meet TXX550 coating machine control software reading formats according to structural arrangement mode, that is, produced the membrane system and controlled automatically in coating machine
The template contral file of system.To different material evaporation characteristics, different evaporation sources can be used, zinc sulphide ZnS materials are easy
Decompose, using resistance evaporation, control evaporation current to control the evaporating temperature of ZnS materials, ensure the work that ZnS is not decomposed and stablized
Have the factor, the metastable aluminium oxide Al of chemical property2O3With fluorination ytterbium YbF3Using electron gun evaporation, accurate thickness monitoring
Film-thickness monitoring is vibrated by quartz crystal to realize, the template file above made is read by control software, by template file
Data（I.e. foregoing film structure）Successively read, data are sent into XTC200 quartz crystals vibration film-thickness monitoring, software control phase
The resistance steaming answered and electron gun, XTC200 film thickness gauges send out film layer end signal, successively complete being coated with for membrane system.
Fig. 3 and Fig. 4 is the three wave band antireflective coatings using actual production of the present invention respectively in Lamda1050 spectrophotometers
Absolute reflectance test result and Spectrum Optical GX Fourier spectrometer reflectance test results, can be with from figure
See, product residual reflectivity slightly meets the requirement of designing technique index made of reality, close to theoretical design requirements.
Laser damage threshold test is carried out to lithium columbate crystal after plated film, its laser damage threshold is in 3J/cm2Left and right, use
Laser confocal scanning microscope observation impaired loci and quantitative measurment damage morphologies, the design gross thickness of membrane system is 930nm, actual
The depth of the damage spot measured is tens of more than um, the starting point of damage not since film, be from lithium niobate in itself
Internal flaw causes, and membrane system is to be resistant to stimulated light in itself, and Laser Experiments result also demonstrates that the present invention can be advantageously applied to
In 100 MJs of 1065nm laser devices.
Claims (7)
1. a kind of preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three, it is characterised in that comprise the following steps：
（1）It is determined that theoretical membrane system, theoretical for based on film structure, ZnS is as high index of refraction material for selection by optical interference film
Material, fluorination ytterbium YbF3For low-index material, using 600nm be antireflective coating as reference wavelength, define ZnS, Al respectively2O3With
YbF3Unit optical thickness in λ/4 is H, M and L, increases by one layer of Al in antireflective coating substrate surface2O3Layer, as Stress match
With resisting laser damage layer, on computers, using Film Design software, according to 1065nm, 1400-1600nm, 3000-4000nm
Three section antireflective coating antireflective requirements, determine the film structure of lithium niobate antireflective coating；To 1040-1080nm, 1400-
1600nm, 3000-4000nm residual reflectivity establish design object function, if reflectivity R (λi) desired wavelength point reflection
Rate, residual reflectivity R ' (λi) be theoretical wavelength point residual reflectivity, wiFor any wavelength points weight, then quadratic sum Σ wi (R
(λi)-R’(λi))2For optimizing evaluation function, theory target reflectivity is 0 on three wavelength, weight wi1 is uniformly set to, near-infrared
Cultellation density is 5nm, in infrared cultellation density be 40nm；
（2）Using with quartz crystal vibration film-thickness monitoring, the full-automatic plated film based on configuration software and PLC hardware controls
Machine, according to the theoretical film structure of above-mentioned acquisition, produce the template contral file that the coating machine automatically controls；
（3）Load selected Coating Materials in coating machine, steamed using resistance and electron gun mixes the depositional mode evaporated, coating machine
By selected template contral file, the making of antireflective coating is automatically performed.
2. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that institute
Stating film structure is：Substrate/antibody Monoclonal transition zone/optics antireflection film system/air.
3. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that institute
The film structure for stating lithium niobate antireflective coating is：Substrate/0.12M4.056H1.054M0.837H1.605L0.534H3.123L/
Air, design reference wavelength 600nm.
4. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that base
Bottom material is lithium niobate, the average residual reflectivity of spectrum dimmer reflecting scope 1040-1080nm, 1400-1600nm, 3000-4000nm
Rate is less than 1%, and laser damage threshold is more than 3J/cm2。
5. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that
ZnS materials are using resistance evaporation, Al2O3And YbF3Using electron gun evaporation, thickness monitoring vibrates film-thickness monitoring by quartz crystal
Come what is realized.
6. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that subtract
The performance parameter of reflectance coating is that the average residual reflectivity of passband is less than 1%.
7. the preparation method of the wave band antireflective coating of resisting laser damage lithium niobate three as claimed in claim 1, it is characterised in that root
According to the theoretical membrane system of acquisition and the Tooling factor of coating machine, film structure file is exported from Essential Macleod softwares,
By thickness and film structure data copy to EXCEL template files, TXT format text files are converted to by switching software, made
Make the template contral file that the membrane system automatically controls in coating machine.
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| CN104561908A (en) * | 2014-12-31 | 2015-04-29 | 西南技术物理研究所 | Preparation method for multi-waveband high-reflective film |
| CN107300782B (en) * | 2017-08-15 | 2019-10-18 | 天津津航技术物理研究所 | A kind of middle infrared band laser protection window of visible light-near-infrared-and design method |
| CN110333561B (en) * | 2019-07-30 | 2024-02-20 | 威海世高光电子有限公司 | Antireflection film, preparation method thereof and miniature projection system |
| CN112578481B (en) * | 2020-12-11 | 2022-03-15 | 中材人工晶体研究院有限公司 | Large-angle medium-long wave infrared anti-reflection protective film and preparation method thereof |
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| JP2007148037A (en) * | 2005-11-28 | 2007-06-14 | Tamron Co Ltd | Antireflection film and manufacturing method thereof |
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| JP2007148037A (en) * | 2005-11-28 | 2007-06-14 | Tamron Co Ltd | Antireflection film and manufacturing method thereof |
| CN101424748A (en) * | 2008-12-01 | 2009-05-06 | 杭州科汀光学技术有限公司 | Visual field, 1.06 mum and 8-12 mum three-wave-band highly effective antireflection film |
| CN101620280A (en) * | 2009-06-30 | 2010-01-06 | 中国航空工业集团公司洛阳电光设备研究所 | Film system of infrared double-waveband antireflection film system and plating method thereof |
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