CN101478109A - Optical thin-film structure used for laser crystal and preparation thereof - Google Patents
Optical thin-film structure used for laser crystal and preparation thereof Download PDFInfo
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- CN101478109A CN101478109A CNA2009100451147A CN200910045114A CN101478109A CN 101478109 A CN101478109 A CN 101478109A CN A2009100451147 A CNA2009100451147 A CN A2009100451147A CN 200910045114 A CN200910045114 A CN 200910045114A CN 101478109 A CN101478109 A CN 101478109A
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Abstract
The invention relates to an optical thin film structure used for laser crystals, and a preparation method thereof. The invention is characterized in that a hard film buffer layer is added between the conventional complex film systems of media/metal used for laser crystals, plays a role in increasing the binding force of the media-metal complex film systems and improving the anti-laser radiation injury threshold of the complex film systems, and meets the development requirements of a high-power laser. The film of the buffer layer is prepared through the thermal evaporation of electron beams. During the growth process, TiN grains and a cleaned supporting base are arranged in a vacuum growth cabinet; the growth cabinet is vacuumized; electron beams are used for irradiating the TiN grains; a given amount of nitrogen or nitrogen ions is introduced into the vacuum cabinet; and the film of the TiN buffer layer is deposited on the supporting base. The TiN buffer layer can significantly improve the binding force of the complex film systems and the anti-laser radiator injury threshold. The optical thin film structure is very theoretically and practically significant for the high-power lasers developing quickly.
Description
Technical field
The present invention relates to a kind of optical thin-film structure that is used for laser crystal and preparation method thereof, relate to a kind of resilient coating technology that is used for the medium/metal composite film system of laser crystal or rather, be a kind ofly to utilize the titanium nitride membrane resilient coating to improve medium/metal film to bind with joint efforts method with threshold for resisting laser damage, preparation method's utilization be the electron beam evaporating deposition technique.Belong to semi-conducting material, field of photovoltaic materials.
Background technology
Laser is as a kind of important photoelectric device, it is the basis that constitutes all kinds of photon informations or energy system, simultaneously be again the core devices that constitutes active photoelectricity weapon, now be widely used in numerous areas such as optical communication, optical information processing, laser processing, medical science and military science.Since nineteen sixty, first laser came out, for decades, especially enter after 21st century, the fast development of laser technology and application, it has developed into a typical cross discipline, is dissolved in diverse discipline research and the applied technical field.In emerging optical communication, optical-fiber network technology and traditional ray machine power technology, laser adds resultant super brightness, ultrashort pulse with monochromaticjty, correlation and the directivity of its uniqueness, bring deep effect to Science and Technology, follow the emergence of opto-electronics, laser science and technology will become the soul technology of opto-electronics gradually in continuous maturation and development.And in the development course of laser, solid state laser has occupied the leading position of development always.Particularly in the eighties in 20th century, semiconductor laser that occurs and the diode pumped solid state laser (Diode-PumpedSolid-State Lasers (DPSSL)) that occurs on this basis be because advantage such as its volume is little, in light weight, efficient is high, stable performance, good reliability and life-span are long, becomes in the photoelectricity industry the tool field of development prospect gradually.
Two most important directions of modern laser development: (1) microminiaturization, be mainly used in laser acquisition (as anti-terrorism sharp weapon detection of explosives and chemical warfare agent), accelerate network traffic etc., (2) high powerization is mainly used in military fields such as laser processing, modern space laser weapon and laser-produced fusion.Developing rapidly to the laser film field of diode pumping solid laser proposed higher challenge, and the quality of laser film quality will directly influence every performance of laser.For the laser of high-average power, the heat accumulation that high-power laser generation produced becomes and limits the important technology bottleneck that it further develops.Effectively the interconnection technique of cooling source and cooling source and laser internal heat aggregation zone has become the approach that breaks through this bottleneck.And the water cooling source is widely adopted owing to its unrivaled superiority, and the part of connection cooling source and LASER HEAT aggregation zone is widely used the metal of good heat-transfer.Therefore the matching problem between metallic film and the dielectric film (being mainly oxide based high-reflecting film or antireflective film) becomes the problem that must consider.And usually between the two crystal structure and charge characteristic etc. differs greatly, and has the serious stress mismatch between the interface, is easy to produce the aliquation and the obscission of film.Therefore how to solve the stress mismatch problem of medium/metal film system, strengthen adhesion between them, guarantee that simultaneously metal film is that thermal conductance and certain degree of hardness become technical matters that need to be resolved hurrily in order to the vibration of resisting high power laser light.
Summary of the invention
The object of the present invention is to provide a kind of optical thin-film structure that is used for laser crystal and preparation method thereof, stress mismatch problem between the film resilient coating that increases one deck hard between medium-metal composite film system with solution medium/metal composite film is, and the threshold for resisting laser damage of raising metal film system or rather.What stress mismatch was introduced between solution medium/metal (Pt) compound film system usually is metal titanium membrane, but because the hardness and the threshold for resisting laser damage of Titanium film are too low, is not suitable in the superpower laser.What the present invention used is to have the buffer layer thin film that better stress coupling is all arranged with medium and metal composite film system, and not only the hardness of film is very high, can keep out the vibration of high power laser light.For with the high metal composite film of thermal conductivity coupling resilient coating commonly used be TiN, AlN or SiC, in order to narrate conveniently, be that example illustrates it with the TiN resilient coating below, must be pointed out, the technical process of TiN resilient coating also is applicable to resilient coatings such as SiC or AlN, is that concrete parameter slightly changes.
A kind of method that improves superpower laser with the medium/adhesion of metal composite film system and the resilient coating of threshold for resisting laser damage of the present invention, the target of electron beam melting is a titanium nitride particles, and the deposition of titanium nitride membrane is carried out in the electron beam vacuum deposition system.Its process is: the substrate that will plate dielectric film is put into the ultra high vacuum thin film growth chamber, under certain pressure and temperature atmosphere, utilize electron beam system with the titanium nitride particles fusion and make on the dielectric film of its hydatogenesis to the substrate holder, and then the metallic film of the high heat conductance of on titanium nitride membrane, then growing, for example Pt or Au, finishing medium/metal composite film is deposition process.
Method of the present invention:
1 coating materials is prepared.The coating materials that needs are coated with (have certain purity, for example 99.99% etc.) is prepared into graininess shapes such as cylinder by a certain size by methods such as vacuum-sinterings, is convenient to absorb the electron beam melting evaporation and grows into film.
2 substrates are prepared.Substrate type can be divided into common slide, (a kind of optical transmission is glass preferably, and it consists of: SiO for optics glass k9 glass commonly used
2=69.13% B
2O
3=10.75% BaO=3.07%Na
2O=10.40% K
2O=6.29% As
2O
3=0.36%), quartz glass, monocrystalline substrate, Nd:YAG substrate or other need be coated with the substrate of multilayer dielectricity/metal composite thin film.For glass substrate, at first sonicated a quarter of an hour (repeating twice) is carried out on its surface with aqueous slkali, utilize absolute ethyl alcohol ultrasonic a quarter of an hour (repeating twice) then, use deionized water ultrasonic a quarter of an hour at last; For monocrystalline substrate, at first remove the oxide layer on surface with 1:1 hydrofluoric acid, and then with acetone, ethanol and deionized water rinsing successively.The preprocess method of other substrates can be with reference to relevant patent or document.The substrate of handling well places vacuum desiccator standby.
3 film growths.Specifically be divided into following several steps:
(1) needs are coated with coating materials and clean after substrate place vacuum chamber, the different coating materials of multilayer film place respectively among the different crucibles;
(2) utilize mechanical pump and turbomolecular pump that vacuum chamber is taken out vacuum to 5 * 10 privately
-4-10
-5Below the Pa;
(3) utilize the programed temperature heated substrate temperature required, be generally room temperature to 800 ℃ to testing;
(4) open plasma source, utilize N
2Plasma source carries out cleaning before the plated film to substrate, removes surface contaminant, strengthens the adhesion of substrate and film simultaneously, utilizes baffle plate that substrate is blocked then, prevents pollution;
(5) unlocking electronic beam control system, pre-thermionic electron beam certain hour, for example 5 minutes, coating materials was arrived in the position of focused beam, and definite electron beam then, the fritting coating materials, the rotating crucible position is carried out fritting respectively to different coating materials then;
(6) open film-thickness monitoring (quartz crystal oscillator control or optics control etc.), set the thickness that needs, strengthen beam power, feed a certain amount of required gas (O for example to deposition velocity to required value
2Deng) treat that the stable substrate baffle plate of opening of deposition process begins plated film, the rotating crucible plating second layer was successively to last one deck after first tunic had plated;
(7) deposition finishes, and turns off electron beam control power supply, extraneous gas, is cooled to room temperature, and vacuum breaker takes out institute's growing film, last molecular pump and mechanical pump.
4 for further improving film and sink to the bottom adhesion or improve performances such as crystallinity, can be at high temperature to the film heat treatment of annealing, look 400-1000 ℃ of backing material and required raising performance annealing region, annealing time is 0.5-24 hour.
The test of 5 threshold for resisting laser damage.Laser test system mainly partly is made up of laser generation system, laser optical path, CCD photographic system etc.In the test with the laser radiation film of certain energy density, with the 2Hz frequency, the 20ns pulse duration, 100 subpulses are testing standard, and same energy density sample different parts test 10 times, is determined damage probability, be abscissa then with the energy density, damage probability is the ordinate mapping, and extrapolation test curve to damage probability is the zero damage probability point that the intersection point of zero point and abscissa is defined as film, is the threshold for resisting laser damage of film.
This shows feature of the present invention:
1. in order to solve the adaptive problem of stress of medium/metal composite film system, between medium and metallic film, introduced the resilient coating good, thereby solved the aliquation and the obscission of medium/metal composite film system with they matchings; The thickness of described buffer layer thin film is 50～200nm;
2. also promptly for the Pt/Ti high with thermal conductivity ... what metal composite film system coupling adopted is the titanium nitride resilient coating, if can adopt other nitride or carbide resilient coating the most, for example AlN or SiC etc. in order to mate other metal film systems; Described dielectric layer is SiO
2, TiO
2, Si
3N
4Deng material;
3. specifically in order to improve the threshold for resisting laser damage of medium/metal composite film system, utilize titanium nitride membrane to substitute Titanium film resilient coating commonly used, improved the hardness and the threshold for resisting laser damage of compound film system;
Because the lower slightly and Titanium film of the thermal conductivity of titanium nitride membrane, therefore in order to cool off in the heat that superpower laser the is produced source that is cooled fast, the thickness of titanium nitride membrane can not be too thick, on titanium nitride membrane, then deposit one deck thermal conductivity preferred metal titanium film system, both can improve the hardness and the threshold for resisting laser damage of compound film system, can also guarantee that the thermal conductivity of metal film system was taken away in the source that is cooled heat that superpower laser produces in time simultaneously;
4. be to be the laser crystal example with Nd:YAG among the present invention, same this structure also is applicable to the YAG crystal of other element dopings, Cr:YAG for example, and Yb:YAG etc., and in the laser crystal of other matrix in the structure, for example: Cr, Ti:Al
2O
3, Nd:YVO
4, Nd:GGG, Yb:BOYS, Yb:KYW laser crystal etc.;
5. be medium/titanium nitride/metal composite film system, in other film systems, can adopt the resilient coating technology equally, for example for the very thin one deck titanium nitride resilient coating of can on monocrystalline substrate, growing earlier at epitaxial growth magnesia film on the silicon substrate;
In sum, the beneficial effect that had compared with prior art of the present invention:
Prior art mainly is to introduce Titanium film resilient coating between medium/metal (Pt) compound film system, it can solve the stress mismatch problem between medium/metal composite film system to a certain extent, but because the hardness and the threshold for resisting laser damage of Titanium film are lower, be used for the damage that superpower laser just is easy to generate film, thereby cause the damage of whole laser system performance.And the present technique employing is to introduce the titanium nitride membrane resilient coating between medium/metal composite film system, titanium nitride membrane and dielectric film and Titanium film all have good matching, simultaneously because the hardness of titanium nitride membrane and threshold for resisting laser damage are all high a lot of than Titanium film, so just solved the film damage problem of compound film system in superpower laser, thereby improved the performance of high power laser system.
Description of drawings
For further specifying technology contents of the present invention, be described in detail as follows below in conjunction with example and accompanying drawing, wherein:
Accompanying drawing 1 is respectively the laser damage photo of Ti and TiN buffer layer thin film, and wherein (a) is the laser damage photo that does not have the Ti metallic film of TiN resilient coating, (b) is the laser damage photo of TiN resilient coating.
Embodiment
Below by the introduction of specific embodiment, further specify substantive distinguishing features of the present invention and obvious improvement.
Being prepared as follows in detail of embodiment 1 TiN buffer layer thin film:
1 raw material is prepared.Using the raw material of preparation TiN film in this experiment is that high-purity (4N) electron beam evaporation is grains dedicated.
2 substrates are prepared.Selecting ordinary optical K9 glass in the present embodiment for use is substrate.At first substrate is put into NaOH solution ultrasonic a quarter of an hour, repeated twice, then ultrasonic a quarter of an hour in absolute ethyl alcohol, repeat twice, at last at deionized water for ultrasonic a quarter of an hour.Place vacuum drying chamber standby the substrate of handling well then.
3 film growths.Be divided into following several steps:
(1) with special-purpose 4N rank TiN particle of ready electron beam evaporation and SiO
2Medium coating materials and cleaned K9 substrate place vacuum chamber, and adjusting target to substrate distance is 50cm;
(2) start mechanical pump and molecular pump vacuum chamber is taken out vacuum to 2 * 10 privately
-4Below the Pa;
(3) adopt temperature programmed control, substrate is heated to 200 ℃, heating rate is 15 ℃/min;
(4) open plasma source, utilize N
2Plasma source carries out cleaning before the plated film to substrate, removes surface contaminant, strengthens the adhesion of substrate and film simultaneously, utilizes baffle plate that substrate is blocked then, prevents pollution;
(5) unlocking electronic bundle thermal evaporation control system, pre-thermionic electron guns 5min, the position of focused beam, and definite electron beam then is to coating materials, and the rotating crucible position is to SiO then
2Carry out fritting respectively with TiN;
(6) open film-thickness monitoring (quartz crystal oscillator control or optics control etc.), set thickness and be respectively 200nm and 100nm, strengthen the electron beam line, treat that the stable substrate baffle plate of opening of deposition process begins to plate SiO to 40mA
2Film feeds N then
2, the rotating crucible position begins evaporation TiN resilient coating to the TiN coating materials;
(7) deposition finishes, and turns off electron beam control power supply, extraneous gas, is cooled to room temperature, and vacuum breaker takes out institute's growing film, last molecular pump and mechanical pump.
The concrete Comparative Examples of implementing:
Being prepared as follows in detail of metal Ti film:
1 raw material is prepared.Using the raw material of preparation Ti film in this experiment is that high-purity (4N) electron beam evaporation is grains dedicated.
2 substrates are prepared.Selecting ordinary optical K9 glass in the present embodiment for use is substrate.At first substrate is put into NaOH solution ultrasonic a quarter of an hour, repeated twice, then ultrasonic a quarter of an hour in absolute ethyl alcohol, repeat twice, at last at deionized water for ultrasonic a quarter of an hour.Place vacuum drying chamber standby the substrate of handling well then.
3 film growths.Be divided into following several steps:
(1) with special-purpose 4N rank Ti particle of ready electron beam evaporation and SiO
2Medium coating materials and cleaned K9 substrate place vacuum chamber, and adjusting target to substrate distance is 50cm;
(2) start mechanical pump and molecular pump vacuum chamber is taken out vacuum to 2 * 10 privately
-4Below the Pa;
(3) adopt temperature programmed control, substrate is heated to 200 ℃, heating rate is 15 ℃/min;
(4) open plasma source, utilize N
2Plasma source carries out cleaning before the plated film to substrate, removes surface contaminant, strengthens the adhesion of substrate and film simultaneously, utilizes baffle plate that substrate is blocked then, prevents pollution;
(5) unlocking electronic bundle thermal evaporation control system, pre-thermionic electron guns 5min, the position of focused beam, and definite electron beam then is to coating materials, and the rotating crucible position is to SiO then
2Carry out fritting respectively with the Ti coating materials;
(6) open film-thickness monitoring (quartz crystal oscillator control or optics control etc.), setting thickness is respectively 200nm and 100nm, strengthens the electron beam line to 40mA, treats that the stable substrate baffle plate of opening of deposition process begins to plate SiO
2Film, the rotating crucible position begins evaporation Ti metal film to the Ti coating materials then;
(7) deposition finishes, and turns off electron beam control power supply, extraneous gas, is cooled to room temperature, and vacuum breaker takes out institute's growing film, last molecular pump and mechanical pump.
Specific embodiment and the test of Comparative Examples threshold for resisting laser damage are compared:
Concrete test process is as follows: test frequency is defined as 2HZ, and laser pulse width is defined as 10ns, and each pulse test number of times is defined as 100 times, just the 50s clock time; By laser focusing system laser spots is focused on fixed-area size, for example 1cm
2, measure laser energy by oscilloscope, determine laser energy density then; Same energy density is tested 10 times at the sample different parts, determine damage probability, be abscissa then with the energy density, damage probability is the ordinate mapping, extrapolation test curve to damage probability is the zero damage probability point that the intersection point of zero point and abscissa is defined as film, is the threshold for resisting laser damage of film.
Test result shows: the threshold for resisting laser damage of the TiN buffer layer thin film threshold for resisting laser damage than metal TI film at least is high by 20%.
Experimental result contrast under two kinds of specific embodiments:
Come as can be seen from experimental result, adopted after the TiN resilient coating, the adhesion of film system has obtained enhancing, and the threshold for resisting laser damage of film improves greatly simultaneously, and this has considerable theory and realistic meaning for the development of modern superpower laser.
Claims (10)
1, a kind of optical thin-film structure that is used for laser crystal is characterized in that between the composite membrane of medium/metal increasing one deck hard buffer layer thin film, and described buffer layer thin film is the material that is complementary with the high metal composite film system of thermal conductivity.
2, by the described optical thin-film structure that is used for laser crystal of claim 1, it is characterized in that described buffer layer thin film is TiN, AlN or SiC, described metal film is Pt or Au.
3,, it is characterized in that described buffer layer thin film is TiN by claim 1 or the 2 described optical thin-film structures that are used for laser crystal.
4, by the described optical thin-film structure that is used for laser crystal of claim 3, the thickness that it is characterized in that described buffer layer thin film is 50-200nm.
5, by the described optical thin-film structure that is used for laser crystal of claim 3, it is characterized in that on cushion into film, depositing the layer of metal titanium film again, the heat that is beneficial to the superpower laser generation is in time taken away in the source of being cooled.
6, preparation is characterized in that as each described method that is used for the optical thin-film structure of laser crystal among the claim 1-4 preparation technology is:
At first, the substrate that has plated deielectric-coating is put into the ultra high vacuum thin film growth chamber, under certain pressure and temperature atmosphere, utilize electron beam system with the resilient coating particle fusion and make on the dielectric film of its hydatogenesis to the substrate holder, and then the metallic film of the high heat conductance of on titanium nitride membrane, then growing, finish the manufacturing process of medium/metal film syzygy.
7, by the described manufacture method that is used for the optical thin-film structure of laser crystal of claim 6, it is characterized in that:
(a) coating materials is prepared: the TiN resilient coating coating materials that needs are coated with is prepared into graininess shapes such as cylinder by vacuum sintering method, is convenient to absorb the electron beam melting evaporation and grows into film.
(b) substrate is prepared: substrate is divided into common slide, optics glass k9 glass commonly used, quartz glass, monocrystalline substrate or Nd:YAG substrate; For glass substrate, at first secondary is repeated on its surface and carry out sonicated with aqueous slkali, utilize absolute ethyl alcohol to repeat twice ultrasonic then, use deionized water ultrasonic at last; For monocrystalline substrate, at first remove the oxide layer on surface with 1:1 hydrofluoric acid, and then with acetone, ethanol and deionized water rinsing successively; The substrate of handling well places vacuum desiccator standby;
(c) film growth: specifically be divided into following several steps:
1. the described substrate that is coated with after coating materials and step b clean of step a is placed vacuum chamber, the different coating materials of multilayer film place respectively among the different crucibles;
2. utilize mechanical pump and turbomolecular pump that vacuum chamber is taken out vacuum to 5 * 10 privately
-4-10
-5Below the Pa;
3. utilize the programed temperature heated substrate temperature required to testing;
4. open plasma source, utilize N
2Plasma source carries out cleaning before the plated film to substrate, removes surface contaminant, strengthens the adhesion of substrate and film simultaneously, utilizes baffle plate that substrate is blocked then, prevents pollution;
5. unlocking electronic beam control system, pre-thermionic electron beam, the position of focused beam, and definite electron beam then is to coating materials, the fritting coating materials, the rotating crucible position is carried out fritting respectively to different coating materials then;
6. open the quartz crystal oscillator control or the film-thickness monitoring of optics control, set the thickness that needs, strengthen beam power to deposition velocity to required value, feed needed gas, treat that the stable substrate baffle plate of opening of deposition process begins plated film, rotating crucible plating second layer resilient coating was successively to last one deck after the ground floor deielectric-coating had plated;
7. deposition finishes, and turns off electron beam control power supply, extraneous gas, is cooled to room temperature, and vacuum breaker takes out institute's growing film, last molecular pump and mechanical pump.
8, by the described manufacture method that is used for the optical thin-film structure of laser crystal of claim 7, the purity that it is characterized in that described TiN resilient coating is 4N.
9, by the described manufacture method that is used for the optical thin-film structure of laser crystal of claim 7, it is characterized in that prepared film is carried out annealing in process; The temperature of annealing in process is 400-100 ℃.
10,, it is characterized in that the annealing in process time is 0.5-24 hour by the described manufacture method that is used for the optical thin-film structure of laser crystal of claim 9.
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| CN102407624A (en) * | 2011-08-15 | 2012-04-11 | 西北核技术研究所 | Laser-irradiation-resistant diffuse reflection metal panel and manufacturing method thereof |
| CN103074593A (en) * | 2012-12-28 | 2013-05-01 | 中国科学院安徽光学精密机械研究所 | Method for improving flexible AZO (aluminum doped zinc oxide) film photoelectric property by excimer laser |
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| CN102407624B (en) * | 2011-08-15 | 2014-09-17 | 西北核技术研究所 | Laser-irradiation-resistant diffuse reflection metal panel and manufacturing method thereof |
| CN103074593A (en) * | 2012-12-28 | 2013-05-01 | 中国科学院安徽光学精密机械研究所 | Method for improving flexible AZO (aluminum doped zinc oxide) film photoelectric property by excimer laser |
| CN105575669A (en) * | 2016-03-05 | 2016-05-11 | 无锡南理工科技发展有限公司 | Dye-sensitized solar cell preparation method |
| CN106340793A (en) * | 2016-11-25 | 2017-01-18 | 中国工程物理研究院应用电子学研究所 | Large-area-fluorescence-absorption-based metalized transition layer structure for suppressing amplified spontaneous emission of batten |
| CN107254667A (en) * | 2017-06-06 | 2017-10-17 | 中国科学院半导体研究所 | Optical medium film, Al2O3, silicon-containing film, the preparation method of laser chamber facial mask |
| WO2020173065A1 (en) * | 2019-02-27 | 2020-09-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Optical film structure, and manufacturing method therefor and use thereof |
| CN109957763A (en) * | 2019-04-10 | 2019-07-02 | 深圳市旺鑫精密工业有限公司 | A kind of nanometer shallow layer manufacture craft applied to five gold surfaces |
| CN115094388A (en) * | 2022-07-08 | 2022-09-23 | 广东信大科技有限公司 | Heating pipe coating method and rose gold pipe and gold pipe prepared by same |
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