CN104330845A - Method for preparing four-wavelength laser reflector - Google Patents
Method for preparing four-wavelength laser reflector Download PDFInfo
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- CN104330845A CN104330845A CN201410721017.6A CN201410721017A CN104330845A CN 104330845 A CN104330845 A CN 104330845A CN 201410721017 A CN201410721017 A CN 201410721017A CN 104330845 A CN104330845 A CN 104330845A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/08—Mirrors
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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
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Abstract
The invention belongs to the technical field of high-precision optical element preparation, and in particular relates to a method for preparing a four-wavelength laser reflector. A high-reflectivity medium film reflector at multiple wavelength points is prepared by virtue of comprehensive utilization of a series of physical and chemical methods such as chemical washing, ion beam sputtering washing, four-wavelength high-reflective film system design, film layer deposition based on a ion beam sputtering technique, and later treatment. In the film layer design, only two materials with high reflectivity and low reflectivity are adopted, and the film layer preparation process can be completed through only once deposition. The reflector has relatively high reflectivity at 1064nm, 532nm, 355nm and 266nm. The reflector prepared by using the method can work stably in a multi-wavelength laser, is high in laser damage resistance and can meet the application requirements of a multi-wavelength output laser.
Description
Technical field
The invention belongs to high-accuracy optical element preparing technical field, be specifically related to a kind of preparation method of four wavelength laser catoptrons.
Background technology
Since nineteen sixty, laser instrument occurred, due to its exclusive monochromaticity, consistance, the characteristic that collimation etc. are not replaced, it is widely applied in military, processing, medical treatment and field of scientific study.Be usually used in the aspects such as laser ranging, laser guidance, laser boring and cutting, air detection, laser remote sensing, ophthalmologic operation.According to the difference of purposes, often need different optical maser wavelength, as needed for different lesions the laser selecting different wave length in laser surgey, to ensure to excise effect.Compare with traditional single wavelength laser instrument, multiple-wavelength laser to can be implemented on a laser instrument simultaneously or alternately exports the laser of multiple wavelength, so both eliminate the expense purchasing multi-station laser economically, turn reduce and take up room, reduce Operation and Maintenance cost.
The realization that multiwavelength laser exports, except carrying out, except the mode of He Ne laser, also can being realized the frequency conversion of laser by nonlinear optical effect to the multiple wavelength lasers produced in same operation material.1064nm, 532nm, 355nm and 266nm four-wavelength laser implementation procedure is: the laser that can be 1064nm by wavelength by frequency doubling technology converts the green glow that wavelength is 532nm to, the ultraviolet light that wavelength is 266nm can be obtained again by frequency multiplication, the laser mixing of wavelength to be the laser of 1064nm and wavelength be 532nm, can obtain the laser of third harmonic 355nm.
The development of multiple-wavelength laser it is also proposed higher requirement to its core parts catoptron, and four-wavelength laser described above requires that catoptron all has higher reflectivity, low absorption and high anti-damage performance at four wavelength places.These optical properties are by chemical cleaning, ion beam sputtering prerinse, high reverse--bias coatings optimization design utilize the integrated use that ion beam spatters the series of physicals such as deposition techniques rete, aftertreatment and chemical means to realize.
Summary of the invention
(1) technical matters that will solve
The technical problem to be solved in the present invention is: the preparation method how providing a kind of four wavelength laser catoptrons.
(2) technical scheme
For solving the problems of the technologies described above, the invention provides a kind of preparation method of four wavelength laser catoptrons, it comprises the steps:
Step S1: processing substrate; Use chemistry and physical cleaning disposal route, chemical treatment is carried out to substrate, and then utilizes ultrasound wave to clean, processed rear centrigugal swing dryer and dried; Chemical reagent comprises hydrochloric acid, ammoniacal liquor, hydrogen peroxide and deionized water;
Step S2: adopt the method for ion beam sputtering to prepare rete by ion beam sputtering device, described ion beam sputtering device comprises radio-frequency ion source, substrate frame and target; Sputtering source is 16cm ion gun, and the setting range of its ion beam pressure, ion beam current is 300V ~ 1300V and 150mA ~ 650mA.
Step S3: substrate prerinse; Presedimentary background vacuum is drawn into and is not more than 1 × 10
-3pa, uses 12cm assisting ion source to base-plate cleaning 5 ~ 10min under low current and lower pressure, with the surface adhesion force of the impurity and enhanced film and substrate of effectively removing substrate surface before thin film deposition;
Step S4: target prerinse; Before thin film deposition, 16cm plasma sputter source is used first to clean quartzy target 60 ~ 200s, then clean metal hafnium target 1500 ~ 5000s;
Step S5: film structure: Choice of substrate materials quartz, operating angle is 45 °, high refractive index layer Material selec-tion HfO
2, low-index film Material selec-tion SiO
2, concrete film structure is:
Sub/5.89H 3.58L 5.91H 3.56L 5.82H 3.52L 6.17H 3.22L 6.32H2.98L 6.54H 2.85L 6.46H 2.94L 6.46H 3.81L 5.43H 3.79L 2.47H 0.72L2.24H 4.03L 1.98H 0.91L 2.47H 3.88L 1.95H 0.96L 2.38H 3.90L 2.14H1.06L 2.07H 4.48L 1.34H 1.21L 2.98H 3.55L 1.16H 1.36L 2.92H 3.56L1.07H 1.47L 2.77H 1.05L 0.92H 1.67L 0.93H 2.91L 1.31H 1.22L 0.99H1.62L 0.75H 3.33L 1.00H 1.42L 0.91H/Air, wherein H, L represent the high refractive index layer HfO of 1/4 wave optical thickness respectively
2with low-index film SiO
2;
Step S6: aftertreatment: heating rate is not more than 5 DEG C/min, when temperature rises to 300 DEG C, the retention time is 12 ~ 20 hours;
Wherein, target is highly purified metal hafnium target, its Φ 360mm, purity >99.95%; And ultraviolet quartz target, its Φ 360mm, purity >99.995%, during work, target plane normal and ion beam incidence direction are 45 °; For improving the thickness evenness of film, work rest adopts planetary rotation structure; Oxygen is passed into vacuum chamber target surface by outside, the adjustable extent 0 ~ 50sccm of oxygen flow, the purity >99.999% of oxygen.
(3) beneficial effect
The present invention realizes 1064nm, 532nm, 355nm and 266nm tetra-preparation of wavelength place high reflectivity mirror by the integrated use of a series of chemistry, physical means, specifically comprises the processes such as chemical cleaning, ion beam sputtering prerinse, four wavelength high reverse--bias film design, ion beam sputtering alternating deposit multilayer height low-index film, aftertreatment.In the present invention, rete design only have employed high low-refraction bi-material, and Film preparation process only needs primary depositing to complete.Four wave mirror prepared by this method have reflectivity high, absorb little, and higher anti-laser damage performance, can meet the application requirement of multiple wavelength output laser.
Accompanying drawing explanation
Fig. 1 is four wave mirror preparation method process flow diagrams.
Fig. 2 is ion beam sputter depositing system schematic.
Fig. 3 is four wave mirror Film Design curve maps.
Fig. 4 is post-processing temperature time plot.
Fig. 5 is four wave mirror test curve figure.
Embodiment
For making object of the present invention, content and advantage clearly, below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.
For solving the problem of prior art, the invention provides a kind of preparation method of four wavelength laser catoptrons, as shown in Figure 1, it comprises the steps:
Step S1: processing substrate; Use chemistry and physical cleaning disposal route, chemical treatment is carried out to substrate, and then utilizes ultrasound wave to clean, processed rear centrigugal swing dryer and dried; Chemical reagent comprises hydrochloric acid, ammoniacal liquor, hydrogen peroxide and deionized water;
Step S2: adopt the method for ion beam sputtering to prepare rete by ion beam sputtering device, described ion beam sputtering device comprises radio-frequency ion source, substrate frame and target; Consult Fig. 2.Sputtering source is 16cm ion gun, and the setting range of its ion beam pressure, ion beam current is 300V ~ 1300V and 150mA ~ 650mA.
Step S3: substrate prerinse; Presedimentary background vacuum is drawn into and is not more than 1 × 10
-3pa, before thin film deposition, use 12cm assisting ion source is to base-plate cleaning 5 ~ 10min under low current and lower pressure, effectively can remove the impurity of substrate surface and the surface adhesion force of enhanced film and substrate;
Step S4: target prerinse; Before thin film deposition, 16cm plasma sputter source is used first to clean quartzy target 60 ~ 200s, then clean metal hafnium target 1500 ~ 5000s;
Step S5: film structure: Choice of substrate materials quartz, operating angle is 45 °, high refractive index layer Material selec-tion HfO
2, it is a kind of common high laser damage threshold membraneous material, and have fabulous chemical stability and thermal stability, it can near ultraviolet to infrared band through wave band; Low-index film Material selec-tion SiO
2, it all has extremely low absorption and good stability at wider wave band; Concrete film structure is:
Sub/5.89H 3.58L 5.91H 3.56L 5.82H 3.52L 6.17H 3.22L 6.32H2.98L 6.54H 2.85L 6.46H 2.94L 6.46H 3.81L 5.43H 3.79L 2.47H 0.72L2.24H 4.03L 1.98H 0.91L 2.47H 3.88L 1.95H 0.96L 2.38H 3.90L 2.14H1.06L 2.07H 4.48L 1.34H 1.21L 2.98H 3.55L 1.16H 1.36L 2.92H 3.56L1.07H 1.47L 2.77H 1.05L 0.92H 1.67L 0.93H 2.91L 1.31H 1.22L 0.99H1.62L 0.75H 3.33L 1.00H 1.42L 0.91H/Air, wherein H, L represent the high refractive index layer HfO of 1/4 wave optical thickness respectively
2with low-index film SiO
2;
Step S6: aftertreatment: heating rate is not more than 5 DEG C/min, when temperature rises to 300 DEG C, the retention time is 12 ~ 20 hours;
Wherein, target is highly purified metal hafnium target, its Φ 360mm, purity >99.95%; And ultraviolet quartz target, its Φ 360mm, purity >99.995%, during work, target plane normal and ion beam incidence direction are 45 °; For improving the thickness evenness of film, work rest adopts planetary rotation structure; Oxygen is passed into vacuum chamber target surface by outside, the adjustable extent 0 ~ 50sccm of oxygen flow, the purity >99.999% of oxygen.
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
The present embodiment provides a kind of four wave mirror preparation methods, and it is by chemical cleaning, ion beam sputtering prerinse, four wavelength high reverse--bias Film Design utilize the multi-wavelength point place high reflectance dielectric film catoptron that the integrated use that ion beam spatters the series of physicals such as deposition techniques rete, aftertreatment and chemical means obtains.
The method specifically comprises the steps:
1) processing substrate: successively carry out MOS grade hydrochloric acid, ammoniacal liquor and hydrogen peroxide, deionized water three cleanings (cleaning solution temperature is 95 DEG C) respectively, recycling supersonic wave cleaning machine carries out ultrasonic cleaning to it, ultrasonic frequency is 3000kHz, ultrasonic time 10 ~ 15min, finally dry with centrigugal swing dryer, rotating speed is 5000 ~ 6000 revs/min;
2) before thin film deposition with 12cm auxiliary source under low current and lower pressure (50mA/350V) to base-plate cleaning 10min;
3) 16cm plasma sputter source (ion beam voltage 1250V, ion beam current 650mA) clean metal hafnium target 900s is used;
4) select quartz as base material in the present invention, operating angle is 45 °, high refractive index layer Material selec-tion HfO2, low-index film Material selec-tion SiO2.Concrete film structure is: Sub/5.89H 3.58L 5.91H 3.56L 5.82H 3.52L 6.17H 3.22L 6.32H2.98L 6.54H 2.85L 6.46H 2.94L 6.46H 3.81L 5.43H 3.79L 2.47H 0.72L2.24H 4.03L 1.98H 0.91L 2.47H 3.88L 1.95H 0.96L 2.38H 3.90L2.14H1.06L 2.07H 4.48L 1.34H 1.21L 2.98H 3.55L 1.16H 1.36L 2.92H 3.56L1.07H 1.47L 2.77H 1.05L 0.92H 1.67L 0.93H 2.91L 1.31H 1.22L 0.99H1.62L 0.75H 3.33L 1.00H 1.42L 0.91H/Air, wherein H, L represents high refractive index layer HfO2 and the low-index film SiO2 of 1/4 wave optical thickness respectively,
5) aftertreatment: heating rate is not more than 3 DEG C/min, when temperature rises to 300 DEG C, the retention time is 12 ~ 20 hours.
Embodiment 2
The present embodiment provides a kind of four wave mirror preparation methods, comprises the following steps:
1) chemical cleaning is carried out to quartz base plate to be coated, successively carry out MOS grade hydrochloric acid, ammoniacal liquor and hydrogen peroxide, deionized water three cleanings (cleaning solution temperature is 95 DEG C) respectively, recycling supersonic wave cleaning machine carries out ultrasonic cleaning to it, ultrasonic frequency is 3000kHz, ultrasonic time 12min, finally dry with centrigugal swing dryer, rotating speed is 6000r/min;
2) coating machine parameter is set: 16cm ion gun is as plasma sputter source, and its ion beam pressure is 1250V, and electric current is 650mA; 12cm ion gun is as auxiliary source only for the cleaning of substrate, and its ion beam pressure is 350V, and electric current is 50mA;
3) target is highly purified metal hafnium target (Φ 360mm, purity >99.95%) and ultraviolet quartz target (Φ 360mm, purity >99.995%), during work, target plane normal and ion beam incidence direction are 45 °; Work rest uses planetary rotation structure.Oxygen is passed into vacuum chamber target surface by outside, and oxygen flow is chosen as 40sccm (the purity >99.999% of oxygen);
4) when background vacuum is drawn into 3 × 10-4Pa, with 12cm auxiliary source by step 3) parameter that sets carries out cleaning 10min to substrate;
5) before thin film deposition, 16cm plasma sputter source is used by step 3) parameter that sets first cleans quartzy target 120s, then clean metal hafnium target 4000s;
6) ion beam sputtering (using 16cm ion gun) technique is adopted to deposit following film system successively:
Sub/5.89H 3.58L 5.91H 3.56L 5.82H 3.52L 6.17H 3.22L 6.32H2.98L 6.54H 2.85L 6.46H 2.94L 6.46H 3.81L 5.43H 3.79L 2.47H 0.72L2.24H 4.03L 1.98H 0.91L 2.47H 3.88L 1.95H 0.96L 2.38H 3.90L 2.14H1.06L 2.07H 4.48L 1.34H 1.21L 2.98H 3.55L 1.16H 1.36L 2.92H 3.56L1.07H 1.47L 2.77H 1.05L 0.92H 1.67L 0.93H 2.91L 1.31H 1.22L 0.99H1.62L 0.75H 3.33L 1.00H 1.42L 0.91H/Air, wherein H, L represents high refractive index layer HfO2 and the low-index film SiO2 of 1/4 wave optical thickness respectively, accompanying drawing 2 is theoretical reflectance rate curve,
7) element having plated high-reflecting film is put into baking box, the time that setting rises to 200 DEG C from room temperature is 2 hours, and the time being warming up to 300 DEG C from 200 DEG C is 2 hours, and keeps 15 hours at 300 DEG C, then lower the temperature voluntarily in an oven, temperature time curve accompanying drawings 3;
8) use spectrophotometer measurement spectral reflectivity, 1064nm, 532nm, 355nm and 266nm tetra-wavelength points place reflectivity be respectively 99.7%, 99.2%, 97.7% and 96.8%, accompanying drawings 4.
To sum up, 1064nm, 532nm, 355nm and 266nm tetra-wavelength points place all to realize high reflectance, by traditional design, preparation method, rete is thicker, preparation difficulty larger.Test result of the present invention shows, under 45 ° of test angle, the reflectivity that the reflectivity at 1064nm and 532nm place all reaches more than 99%, 355nm and 266nm place also reaches about 97%.Achieve catoptron and be separated taking into account of multi-wavelength point place's high reflectance.Result as shown in Figure 5.
By implementing such scheme, achieve 1064nm, 532nm, 355nm and 266nm tetra-preparation of wavelength place high reflectivity mirror, in the present invention, rete design only have employed high low-refraction bi-material, and Film preparation process only needs primary depositing to complete.Multi-wavelength point place catoptron prepared by the present invention may be used for multiple-wavelength laser.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and distortion, these improve and distortion also should be considered as protection scope of the present invention.
Claims (2)
1. a preparation method for four wavelength laser catoptrons, it is characterized in that, it comprises the steps:
Step S1: processing substrate; Use chemistry and physical cleaning disposal route, chemical treatment is carried out to substrate, and then utilizes ultrasound wave to clean, processed rear centrigugal swing dryer and dried; Chemical reagent comprises hydrochloric acid, ammoniacal liquor, hydrogen peroxide and deionized water;
Step S2: adopt the method for ion beam sputtering to prepare rete by ion beam sputtering device, described ion beam sputtering device comprises radio-frequency ion source, substrate frame and target; Sputtering source is 16cm ion gun, and the setting range of its ion beam pressure, ion beam current is 300V ~ 1300V and 150mA ~ 650mA.
Step S3: substrate prerinse; Presedimentary background vacuum is drawn into and is not more than 1 × 10
-3pa, uses 12cm assisting ion source to base-plate cleaning 5 ~ 10min under low current and lower pressure, with the surface adhesion force of the impurity and enhanced film and substrate of effectively removing substrate surface before thin film deposition;
Step S4: target prerinse; Before thin film deposition, 16cm plasma sputter source is used first to clean quartzy target 60 ~ 200s, then clean metal hafnium target 1500 ~ 5000s;
Step S5: film structure: Choice of substrate materials quartz, operating angle is 45 °, high refractive index layer Material selec-tion HfO
2, low-index film Material selec-tion SiO
2, concrete film structure is:
Sub/5.89H 3.58L 5.91H 3.56L 5.82H 3.52L 6.17H 3.22L 6.32H2.98L 6.54H 2.85L 6.46H 2.94L 6.46H 3.81L 5.43H 3.79L 2.47H 0.72L2.24H 4.03L 1.98H 0.91L 2.47H 3.88L 1.95H 0.96L 2.38H 3.90L 2.14H1.06L 2.07H 4.48L 1.34H 1.21L 2.98H 3.55L 1.16H 1.36L 2.92H 3.56L1.07H 1.47L 2.77H 1.05L 0.92H 1.67L 0.93H 2.91L 1.31H 1.22L 0.99H1.62L 0.75H 3.33L 1.00H 1.42L 0.91H/Air, wherein H, L represent the high refractive index layer HfO of 1/4 wave optical thickness respectively
2with low-index film SiO
2;
Step S6: aftertreatment: heating rate is not more than 5 DEG C/min, when temperature rises to 300 DEG C, the retention time is 12 ~ 20 hours.
2. the preparation method of four wavelength laser catoptrons as claimed in claim 1, is characterized in that, target is highly purified metal hafnium target, its Φ 360mm, purity >99.95%; And ultraviolet quartz target, its Φ 360mm, purity >99.995%, during work, target plane normal and ion beam incidence direction are 45 °; For improving the thickness evenness of film, work rest adopts planetary rotation structure; Oxygen is passed into vacuum chamber target surface by outside, the adjustable extent 0 ~ 50sccm of oxygen flow, the purity >99.999% of oxygen.
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Cited By (4)
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| CN108445567A (en) * | 2018-03-30 | 2018-08-24 | 苏州沛斯仁光电科技有限公司 | A kind of high-reflecting film and preparation method of high damage threshold |
| CN113671609A (en) * | 2021-07-27 | 2021-11-19 | 上海灵曼信息科技有限公司 | High laser damage threshold film and preparation method thereof |
| CN113721313A (en) * | 2021-08-11 | 2021-11-30 | 中国科学院上海光学精密机械研究所 | Method for realizing low-absorption low-heat distortion film |
| CN115980898A (en) * | 2023-03-21 | 2023-04-18 | 成都沃达惠康科技股份有限公司 | Multi-element multi-layer middle infrared high-reflection film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108445567A (en) * | 2018-03-30 | 2018-08-24 | 苏州沛斯仁光电科技有限公司 | A kind of high-reflecting film and preparation method of high damage threshold |
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| CN113721313A (en) * | 2021-08-11 | 2021-11-30 | 中国科学院上海光学精密机械研究所 | Method for realizing low-absorption low-heat distortion film |
| CN113721313B (en) * | 2021-08-11 | 2022-05-31 | 中国科学院上海光学精密机械研究所 | Method for realizing low-absorption low-heat distortion film |
| CN115980898A (en) * | 2023-03-21 | 2023-04-18 | 成都沃达惠康科技股份有限公司 | Multi-element multi-layer middle infrared high-reflection film and preparation method thereof |
| CN115980898B (en) * | 2023-03-21 | 2023-06-20 | 成都沃达惠康科技股份有限公司 | Multi-element multi-layer middle infrared high-reflection film and preparation method thereof |
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Application publication date: 20150204 |