CN103882378A - Method for preparing antireflection film having high laser-induced damage threshold on yttrium calcium oxytriborate (YCOB) crystals - Google Patents

Method for preparing antireflection film having high laser-induced damage threshold on yttrium calcium oxytriborate (YCOB) crystals Download PDF

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CN103882378A
CN103882378A CN201410050236.6A CN201410050236A CN103882378A CN 103882378 A CN103882378 A CN 103882378A CN 201410050236 A CN201410050236 A CN 201410050236A CN 103882378 A CN103882378 A CN 103882378A
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ycob
substrate
polishing
damage threshold
crystal
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CN103882378B (en
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张锦龙
丁涛
程鑫彬
谢雨江
王占山
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Tongji University
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Abstract

The invention discloses a method for preparing an antireflection film having high laser-induced damage threshold on the surfaces of nonlinear yttrium calcium oxytriborate crystals. With respect to strong anisotropy of YCOB crystals and the damage mechanism of the antireflection film, the method comprises the steps of etching a YCOB substrate with hydrofluoric acid, carrying out cold working on the YCOB substrate, etching the YCOB substrate with the ion beam, ultrasonically cleaning the YCOB substrate, cleaning the YCOB substrate with ion beam in vacuum, and plating a film on the YCOB substrate. The YCOB antireflection film prepared by the invention has excellent optical properties, high damage threshold, good environmental stability and can be compatible with the existing substrate processing, cleaning and film preparation process. The YCOB antireflection film has such advantages as good process repeatability, strong controllability and easy popularization and has a broad application prospect in the field of the high-power laser film in the further.

Description

A kind of preparation method of three boracic acid oxygen calcium yttrium crystal (YCOB) high laser damage threshold anti-reflection films
Technical field
The present invention relates to a kind of method for preparing optical thin film, particularly relate to a kind of preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films.
Background technology
In strong laser system, powerful laser energy very easily produces destruction to the element in system, therefore gain media is had to very high resisting laser damage requirement.Because three boracic acid oxygen calcium yttriums (YCOB) crystal has, damage threshold is high, nonlinear factor is large, transmission region is wide, phase matched scope large, be difficult for the advantages such as deliquescence, be subject in recent years extensive concern and research, and be successfully applied in high power laser system.YCOB crystal refractive index is large, when laser incident, can produce stronger Fresnel reflection, reduces energy utilization efficiency and the stability of laser system, therefore significant for the development of YCOB crystal anti-reflection film.The anisotropy of YCOB crystal itself, the mechanics and the optical property that are coated on the film on crystal are brought to problems, comprising that unequal power distribution, adhesion of thin film between film and crystal is lower, respectively cause temperature to raise to the difference of thermal expansivity easily there is be full of cracks etc., is matching Design and optimizes preparation method and bring huge challenge to film.And because YCOB crystal anti-reflection film uses in high power laser system, its performance quality has determined the output performance of laser to a great extent, and the damage threshold that therefore improves YCOB crystal anti-reflection film is also very crucial research contents.The height of film damage threshold is the coefficient result of many factors, and for anti-reflection film, absorptivity impurity defect is one of factor of most critical.In the whole process of film preparation, all likely introduce defect, therefore in preparation process, full-flow process is optimized, the introducing of controlling defect is the effective means that improves YCOB crystal anti-reflection film damage threshold.
The object of the invention is for the problems referred to above, design grow tall transmission film system of a kind of double wave, by optimizing whole process preparation technology, controlled the introducing of defect, promote film mechanical characteristics simultaneously, realized the anti-reflection film preparation that transmissivity is high on YCOB crystal, sticking power is good, damage threshold is high.
Summary of the invention
Because YCOB crystal has anisotropy, difference of thermal expansion coefficients is larger, cause easily be full of cracks and poor adhesive force of film, and in whole preparation process, easily introduce defect impurity, cause film damage threshold to reduce, therefore applicant promotes damage threshold and the mechanical property of YCOB plane of crystal anti-reflection film by the whole process control technique of base plate carving and corrosion, substrate design, basal-plate ultrasonic cleaning, substrate ion beam etching, substrate ion beam cleaning, electron beam evaporation deposition.
Concrete preparation technology of the present invention and step are as follows:
(1) etching liquid of the YCOB crystal of conventional glossing processing being put into hydrofluoric acid and deionized water (1: 20 proportioning of volume ratio) mixed preparing carries out etching to substrate, etching time can obtain best effect at 30min, removes most of sub-surface damage layer.
(2) adopt nano level colloid silica (SiO 2) and pitch polishing pad carry out chemically machinery polished, make to show that roughness is less than 5A, reduce microscopic damage, further reduce sub-surface damage layer.
(3) substrate after chemically machinery polished is carried out to ion beam etching, remove polishing settled layer again more than 100nm, etching time is 20 minutes, and source parameters is electric current 1200mA, voltage 900V.
(4) the deionized water ultrasonic cleaning of the substrate after ion beam etching, removes grease and residual particles on substrate completely.
(5) by after added substrate (YCOB), after static 20 minutes, bleed, base vacuum is 1 × 10-3Pa again.Because bleed immediately after added, easily introduce defect at substrate surface.After bleeding, start heated substrates, in order to prevent that too fast heating from causing substrate be full of cracks, heat-processed is divided into 2 steps, first substrate is slowly heated to 100 degrees Celsius with 30 minutes from room temperature, constant temperature 20 minutes, then substrate is slowly heated to 150 degrees Celsius with 20 minutes, constant temperature 60 minutes.
(6) before plated film starts, first with ion source, substrate surface is cleaned, remove and in vacuum suction process, be adsorbed on the particulate pollutant on substrate.Ion source oxygen flow is 40sccm, and argon flow amount is 25sccm, and voltage is 350V, and electric current is 550mA.The ion beam cleaning time is 60s, and this is that this improves its threshold value and have important effect for the absorption that reduces film because effectively Ion Cleaning energy can affect the character of the how many and defect of the size of substrate surface defect.
(7) utilize electron beam evaporation Assisted by Ion Beam mode to be coated with the first layer SiO 2material, ion source oxygen flow is 50sccm, and argon flow amount is 5sccm, and voltage is 550V, and electric current is 670mA.Using Assisted by Ion Beam at the first layer, is in order to increase the sticking power of film on YCOB crystal, improves the stress of film and YCOB crystal simultaneously.Being coated with in the first layer thin-film process, SiO 2speed is 7.4A/s.Because select suitable sedimentation rate can improve the stress of film on YCOB crystal and obtain larger sticking power.
(6) subsequent thin film be coated with employing electron-beam evaporation mode because use electron beam evaporation to be coated with to make film damage threshold higher and can not introduce defect, this also has positive meaning to improving its damage threshold.Being coated with in process, HfO 2speed is 1.4A/s, SiO 2speed is 6.5A/s, and at HfO 2rete be coated with the active oxygen ion that is filled with 60sccm in process, make metal Hf being coated with fully oxidation in process, avoid causing because of oxygen loss the reduction of damage threshold.
(7) plated film finishes rear sample the slow annealing of vacuum chamber also aging 10 hours, and slowly annealing is in order to discharge the later stress of film forming, prevents that film from chapping.
The present invention is compared with conventional preparation technology, its feature is for YCOB crystal peculiar property and service requirements, optimize whole process preparation technology taking control defect, raising sticking power as the mode of core, effectively improved damage threshold and the sticking power of YCOB crystal anti-reflection film.Key of the present invention is following 2 points:
1. the easily feature such as be full of cracks of, heating large for YCOB crystalline anisotropy, thermal expansion coefficient difference, we are to base
Plate carries out combine with the Assisted by Ion Beam mode of plated film of ion beam cleaning, slowly heating step by step, electron beam evaporation,
Select HfO 2with SiO 2as being coated with material, the problems referred to above are effectively solved.
2. in order to improve the threshold for resisting laser damage of YCOB crystal anti-reflection film, in whole thin-film-coating flow process, carry out the optimization of technique taking control defect as core.Before plated film, with hf etching, the chemically machinery polished of nano level colloid silica, ion beam etching, washed with de-ionized water removal YCOB crystal subsurface defect layer, and adopt ion beam cleaning further to control plane of crystal defect.In thin-film-coating process, select suitable parameter, control defect and introduce, and be coated with HfO 2process in be filled with active oxygen, the oxidation efficiency that further improves film is to reduce the native defect in film.
Technique effect of the present invention is as follows:
1. can effectively solve the difficult problem that is coated with that the features such as YCOB crystalline anisotropy bring, the membrane stress that coats is less, sticking power is large and transmissivity is high, can in laser system, normally stablize use.
2. the YCOB crystal film damage threshold that uses the inventive method to prepare is high.Contrast the YCOB crystal anti-reflection film that does not have familiar lacunas control technique to be coated with, found that the film defects impaired loci that uses the inventive method to coat is few, damage threshold is improved largely.
3. the inventive method is simple, and expense is cheap, reproducible, and in whole preparation process, these method practicality are extremely strong, is suitable for batch production, can meet the market requirement of laser technology fast development, has good economic benefit.
Brief description of the drawings
Fig. 1 is the transmittance graph of YCOB crystal 1064nm and 527nm dual wavelength anti-reflection film.
Embodiment
This is described in further detail the present invention by specific examples, as follows:
YCOB crystal 1064nm and 527nm dual wavelength anti-reflection film are coated with
1. plated sample preparation product YCOB crystalline size is 10*10*3mm.The structure of this film system is: S L (H L) ^3A, and S is substrate YCOB crystal, and A is air, and H is high-index material HfO 2, L is low-index material SiO 2, every layer film thickness is 190nm/54.8nm/62.53nm/119nm/22nm/165.54, and filming equipment is the Japanese light coating equipment OTFC-1800 that speeds, and configuration ion source is 17cm radio-frequency ion source.
2. be coated with by previous process steps, the YCOB substrate after conventional polishing is carried out to etching with the etching liquid of hydrofluoric acid and deionized water (1: 20 proportioning of volume ratio) mixed preparing, etching time is at 30min.Substrate washed with de-ionized water after chin erosion, then use nano level colloid silica (SiO 2) and pitch polishing pad carry out chemically machinery polished, surfaceness <5A, ionic fluid chin erosion for substrate after polishing, etching time is 20 minutes, source parameters is electric current 1200mA, voltage 900V.Substrate washed with de-ionized water after ion beam etching, removes grease and residual particles on substrate completely.Then YCOB crystal is put on the work rest of filming equipment, after static 20 minutes, started to bleed, base vacuum is 1 × 10-3Pa.Substrate (YCOB) heat-processed is divided into 2 steps, first substrate is slowly heated to 90 degrees Celsius from room temperature with 20 minutes, constant temperature 20 minutes, then substrate was slowly heated to 140 degrees Celsius with 20 minutes, constant temperature 20 minutes.Before plated film starts, with ion source during to base-plate cleaning, oxygen flow 30sccm, argon flow amount 30sccm, voltage 350V, electric current 550mA.When plated film, high low-index material uses respectively metal Hf and SiO 2ring.While being coated with the first layer SiO2 material, ion beam assisted depositing parameter is: oxygen flow 50sccm, argon flow amount 5sccm, voltage 550V, electric current 670mA; SiO 2speed be 8A/s.Be coated with subsequent film and adopt electron-beam evaporation mode, HfO 2speed is 2A/s, SiO 2speed is 8A/s, is being coated with HfO 2the oxygen that is filled with 60sccm in the process of rete provides ion-oxygen.Be coated with after end, after slow cooling is aging by its taking-up.
3. the sample being coated with is tested with spectrophotometer, be greater than 99% at 1064nm and 527nm place transmissivity, spectrum property meets the user demand in high power laser system completely.Concrete curve of spectrum Fig. 1 in brief description of the drawings.
4. on nanosecond laser damage test platform, carry out damage check, adopt 1-on-1 testing standard, the damage threshold of this sample is greater than 10J/cm2 (laser parameter is λ=532nm, pulsewidth 10ns).
The YCOB crystal 1064 being coated with this invention and 527nm dual wavelength anti-reflection film, its spectral response curve meets service requirements completely, and damage threshold is higher, has very strong practical value.

Claims (8)

1. a preparation method for nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films, is characterized in that comprising the following steps:
1) hf etching of YCOB substrate after conventional polishing: the etching liquid of the YCBO substrate after conventional polishing being put into hydrofluoric acid and deionized water mixed preparing carries out etching, removes settled layer more completely;
2) floating polishing of YCOB substrate: adopt floating polishing technique, use pitch polishing pad, by SiO 2polishing powder is dissolved in deionized water, and fused quartz substrate is carried out to polishing, by Roughness Surface on Control below 5A;
3) ion beam etching of YCOB substrate: the YCOB substrate after using RF ion source to polishing carries out etching, removes polishing settled layer again more than 100nm;
4) ultrasonic cleaning of YCOB substrate after ion beam etching: use ultrasonic cleaning technology to remove substrate surface grease and residual particles more than 300nm;
5) the vacuumizing and heat of YCOB substrate: by Controlling System, substrate is heated step by step, make temperature rising, and constant temperature 1 hour;
6) YCOB substrate upper film preparation: use ion source to carry out vacuum ionic Shu Qingxi to YCOB substrate, use subsequently electron beam evaporation method to prepare HfO on YCOB substrate 2/ SiO 2film.
2. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, it is characterized in that: described step 1) in etching liquid be hydrofluoric acid and deionized water (1: 20 proportioning of volume ratio) mixed preparing, etching time is 30 minutes.
3. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, is characterized in that: described step 2) in SiO used 2the median size of polishing powder is less than 1 μ m, and the concentration of polishing powder is less than 2%, and surface of polished roughness is less than 5A.
4. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, it is characterized in that: described step 3) in after YCOB substrate polishing, YCOB substrate after using RF ion source to polishing carries out etching, remove polishing settled layer again more than 100nm, etching time is 20 minutes, source parameters is electric current 1200mA, voltage 900V.
5. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, is characterized in that: described step 4) in hyperacoustic frequency be 1 megahertz, use soda acid cleaning solution, proportioning is NH 4oH:H 2o 2: H 2o=1: 4: 10, ultrasonic time 30-60 minute, ultrasonic power is 2-3Kw, uses deionized water rinsing 2 times after ultrasonic cleaning, then dries up with dry air.
6. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, it is characterized in that: described step 5) in YCOB crystal is put on the work rest of filming equipment, after static 20 minutes, start to bleed, base vacuum is 1 × 10-3Pa; Substrate (YCOB) heat-processed is divided into 2 steps, first substrate is slowly heated to 100 degrees Celsius from room temperature with 30 minutes, constant temperature 20 minutes, then substrate was slowly heated to 150 degrees Celsius with 20 minutes, constant temperature 60 minutes.
7. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, it is characterized in that: described step 6) in use argon gas and oxygen mix plasma body to clean substrate surface, the purity of xenon and oxygen is better than 99.999%, throughput ratio is 1: 1, the ion beam cleaning time was 60 seconds, ion beam voltage is 350v, and ion beam current is 550mA.
8. the preparation method of nonlinear crystal three boracic acid oxygen calcium yttrium plane of crystal high laser damage threshold anti-reflection films according to claim 1, is characterized in that: described step 6) in when plated film high low-index material use respectively metal Hf and SiO 2ring; While being coated with the first layer SiO2 material, ion beam assisted depositing parameter is: oxygen flow 50sccm, argon flow amount 5sccm, voltage 550V, electric current 670mA; SiO 2speed be 8A/s; Be coated with subsequent film and adopt electron-beam evaporation mode, HfO 2speed is 2A/s, SiO 2speed is 8A/s, is being coated with HfO 2in the process of rete, be filled with the ion oxygen of 60sccm; Be coated with after end, after 10 hours slow coolings of vacuum are aging by its taking-up.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104973794A (en) * 2015-05-28 2015-10-14 同济大学 Ion beam etching apparatus and method of optical substrate for laser film element
CN106199801A (en) * 2016-08-31 2016-12-07 奥普镀膜技术（广州）有限公司 A kind of 40G100G optical filter thin-film-coating method
CN106435487A (en) * 2016-10-10 2017-02-22 同济大学 Preparation method of lithium triborate crystal high-laser-damaged-threshold antireflection film
CN106925565A (en) * 2017-02-09 2017-07-07 同济大学 A kind of etch cleaner method of lbo crystal
CN109216180A (en) * 2017-07-03 2019-01-15 东京毅力科创株式会社 Substrate processing method using same and substrate board treatment
CN109262377A (en) * 2018-11-15 2019-01-25 首都师范大学 For being passivated the polishing process of CsI (TI) plane of crystal defect
CN110007377A (en) * 2019-04-15 2019-07-12 南京波长光电科技股份有限公司 A kind of picosecond laser high power anti-reflection film and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006092949A1 (en) * 2005-02-28 2006-09-08 Nalux Co., Ltd. Optical element with laser damage suppression film
CN102825028A (en) * 2012-09-11 2012-12-19 同济大学 Cleaning method of glazed surface of YCOB crystal
CN102965614A (en) * 2012-11-23 2013-03-13 同济大学 Preparation method of laser film
CN103231302A (en) * 2013-04-12 2013-08-07 同济大学 Method for obtaining super-smooth surface low-sub-surface-damage crystal

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006092949A1 (en) * 2005-02-28 2006-09-08 Nalux Co., Ltd. Optical element with laser damage suppression film
CN102825028A (en) * 2012-09-11 2012-12-19 同济大学 Cleaning method of glazed surface of YCOB crystal
CN102965614A (en) * 2012-11-23 2013-03-13 同济大学 Preparation method of laser film
CN103231302A (en) * 2013-04-12 2013-08-07 同济大学 Method for obtaining super-smooth surface low-sub-surface-damage crystal

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104973794A (en) * 2015-05-28 2015-10-14 同济大学 Ion beam etching apparatus and method of optical substrate for laser film element
CN106199801A (en) * 2016-08-31 2016-12-07 奥普镀膜技术（广州）有限公司 A kind of 40G100G optical filter thin-film-coating method
CN106435487A (en) * 2016-10-10 2017-02-22 同济大学 Preparation method of lithium triborate crystal high-laser-damaged-threshold antireflection film
CN106925565A (en) * 2017-02-09 2017-07-07 同济大学 A kind of etch cleaner method of lbo crystal
CN109216180A (en) * 2017-07-03 2019-01-15 东京毅力科创株式会社 Substrate processing method using same and substrate board treatment
CN109216180B (en) * 2017-07-03 2023-09-08 东京毅力科创株式会社 Substrate processing method and substrate processing apparatus
CN109262377A (en) * 2018-11-15 2019-01-25 首都师范大学 For being passivated the polishing process of CsI (TI) plane of crystal defect
CN110007377A (en) * 2019-04-15 2019-07-12 南京波长光电科技股份有限公司 A kind of picosecond laser high power anti-reflection film and preparation method thereof
CN110007377B (en) * 2019-04-15 2024-06-21 南京波长光电科技股份有限公司 Picosecond laser high-power antireflection film and preparation method thereof

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