CN1203965C - Surface processing method of titanium-doped sapphire crystal laser rod - Google Patents

Surface processing method of titanium-doped sapphire crystal laser rod Download PDF

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Publication number
CN1203965C
CN1203965C CN 03116635 CN03116635A CN1203965C CN 1203965 C CN1203965 C CN 1203965C CN 03116635 CN03116635 CN 03116635 CN 03116635 A CN03116635 A CN 03116635A CN 1203965 C CN1203965 C CN 1203965C
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laser
acid etching
titanium
sapphire crystal
laser bar
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CN 03116635
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CN1460573A (en
Inventor
彭观良
周圣明
李红军
王静雅
周国清
杭寅
徐军
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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  • Laser Beam Processing (AREA)
  • Grinding And Polishing Of Tertiary Curved Surfaces And Surfaces With Complex Shapes (AREA)

Abstract

A surface processing method for the Ti-doped sapphire crystal laser rod includes orienting Ti sapphire crystal, cutting to obtain blank, coarse and fine grinding, end machining, and chemical-mechanical polishing, and features acid etching and surface heat treatment. Tests show that the laser rod processed by the method can obtain a clean surface with smooth and flat atomic scale and complete crystal lattice, and the film deposited on the very smooth and flat substrate has a very high laser damage threshold value, thereby being beneficial to improving the output power of a laser.

Description

The method of surface finish of ti sapphire crystal laser bar
Technical field
The present invention relates to the crystal laser rod, particularly a kind of method of surface finish of ti sapphire crystal laser bar, comprise technical process such as the directed cutting of crystalline, corase grind, correct grinding, chemically machinery polished, acid etching, surface heat processing, and relevant surperficial acid etching and heat treatment process parameter and the etching chemical agent prescription that adopted.
Background technology
Ti sapphire crystal is internationally recognized best broadband tunable laser crystalline material, it has gain bandwidth, big characteristics such as peak gain cross section, high-quantum efficiency, high heat conductance, high laser-damaged threshold value and Heat stability is good, is ultrafast, superpower femtosecond laser and high power tunable laser system good vibration and amplification medium.
Along with the develop rapidly of superpower, ultrafast, superpower femtosecond laser technology, more and more higher to the requirement of titanium gem crystal laser damage threshold.Body damage threshold (the GW/cm of titanium gem crystal 2) general specific surface rete damage threshold (300~500MW/cm 2) a high order of magnitude, therefore, the raising of plane of crystal rete damage threshold is crucial, and plane of crystal rete damage threshold depends on the processing and the coating technique of plane of crystal.
Formerly in the technology, solid laser rod as the operation material of laser apparatus, as ruby laser rod, YAG laser bar, mix titanium precious stone laser rod or the like, its processing usually only depends on mechanical mill and polishing process to finish (referring to Gao Honggang, Cao Jianlin, Zhu Yong, Chen Chuantian, physics, 2000 10 phases, 610 pages), the easy so inferior surface (Subsurface) of causing is damaged, and is difficult to obtain high-quality optical surface.Sub-surface damage is hidden under the upper layer after the polishing, be difficult for realizing, but sub-surface damage can increase the scattering of light on surface, makes the resisting laser damage ability drop of this optical element of laser bar itself.In addition, optical thin film is as key components in the laser optical element, and it is bearing the vital role that produces and transmit laser.The laser damage threshold of optical thin film directly has influence on the output size of energy of lasers, is one of bottleneck factor of limit laser device raising output rating.The optical thin film threshold for resisting laser damage is relevant with multiple factor, comprises substrate processing and cleaning parameters, coating process parameter and Coating Materials etc.The laser damage threshold of optical thin film depends on the calibration rule of its roughness, and depend on the roughness of substrate on the roughness certain degree of film, glossing has determined size, what and the defects property of substrate surface defective, and these processes all can form the absorption defective of film and substrate interface.So at the above-mentioned laser bar substrate surface deposition optical thin film that has sub-surface damage, the laser damage threshold of optical thin film also can be lower.(obeying the people, Ma Ping referring to Hu Jianping, Qiu, optical technology, the 27th the 6th phase of volume of November calendar year 2001,507 pages).
Therefore, how to improve optical material, particularly the resisting laser damage ability of laser bar substrate and optical thin film to satisfy the requirement of high power laser system, has become an of great value research topic.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the shortcoming of above-mentioned existing laser bar processing technology. a kind of method of surface finish of titanium gem crystal laser bar is provided.
Technical solution of the present invention is:
A kind of method of surface finish of ti sapphire crystal laser bar comprises iron gem crystal orientation, cuts into the laser bar blank, cylinder corase grind and correct grinding, end face processing, chemically machinery polished, it is characterized in that also will handling through acid etching and surface heat.
Described acid etching is through the titanium gem stick after the polishing, drops into H 2SO 4: H 3PO 4=3: 1 (volume ratio) mixed solution, 100~400 ℃ of temperature, acid etching 5~30 minutes.
It is to use deionized water rinsing 5 minutes through the titanium gem stick behind the acid etching, the titanium gem stick to be placed 1360 ± 20 ℃ environment again that described surface heat is handled, and constant temperature is 1~3 hour under the hydrogen atmosphere condition.
The present invention compares with technology formerly, its key is to have introduced acid etching and surface heat treatment process, advantage is acid etching and surface heat treatment process have been removed the machinery that produces in the polishing process on the laser bar surface a sub-surface damage, and remove various contaminations, thereby obtain the clean surface of smooth smooth, the lattice perfection of atom level, be deposited on this very smooth smooth suprabasil film and have very high laser-damaged threshold value, help the raising of laser output power, help obtaining superpower laser.
Description of drawings
Fig. 1 is the concrete process flow sheet of the method for surface finish of titanium gem crystal laser bar of the present invention.
Embodiment:
Titanium gem crystal Ti: Al 2O 3(doping content 0.35wt%Ti 2O 3), its crystal blank is by the process flow sheet of the method for surface finish of titanium gem crystal laser bar of the present invention as shown in Figure 1.The concrete preparation process of the method for surface finish of titanium gem crystal laser bar of the present invention is as follows:
<1〉directed cutting: titanium gem crystal according to the size of completion back laser bar, is reserved the process redundancy about 0.4~0.6mm more earlier through directed, cuts into tetragonal prism bodily form blank.
<2〉cylinder corase grind and correct grinding: with the cylinder blank with 120~180 #Silicon carbide or norbide abrasive material are worn into the crystal blank cross section on request and are four directions or cylindrical on rough grinding machine, require tapering and out of roundness error at ± 0.01mm.
<3〉end face processing: W40, W20, W10 norbide face off on steel disk are successively used in the processing of titanium precious stone laser rod both ends of the surface.In process of lapping, to note measuring end face squareness.
<4〉chemically machinery polished: chemically machinery polished is to drip the process that the accurate in advance chemical corrosion liquid of preparing polishes crystal on the polishing pad.Polishing workpiece and polishing pad are done relative movement and friction, finish polishing simultaneously under the help of grinding slurry (title polishing fluid) that contains chemical mordant.
<5〉acid etching:, drop into H through the titanium gem stick after the above-mentioned polishing 2SO 4: H 3PO 4=3: 1 (volume ratio) mixed solution, 100~400 ℃ of temperature, acid etching 5~30 minutes.Purpose is to remove the sub-surface damage of the machinery that produces on the laser bar surface in the polishing process, and removes various contaminations, thereby obtains the clean surface of smooth smooth, the lattice perfection of atom level.
<6〉surface heat is handled: in order further to eliminate because the surface stress that technology produced and the cut of front, obtain the planarized surface of atom level level, so will use deionized water rinsing 5 minutes through the titanium gem stick behind the acid etching, the titanium gem stick placed 1360 ± 20 ℃ environment, constant temperature is 1~3 hour in hydrogen atmosphere, carries out surface heat and handles.
Be an embodiment below.The concrete preparation process of the method for surface finish of titanium gem crystal laser bar is as follows:
<1〉directed cutting: the titanium gem crystal both ends of the surface cut into (6 ± 0.5) * (6 ± 0.5) * (15 ± 0.5) mm tetragonal prism bodily form blank perpendicular to (0001) face.
<2〉cylinder corase grind and correct grinding: the cylinder blank is used 120 and 180 respectively #The norbide abrasive material is worn into the crystal blank cross section on request on rough grinding machine be cylindrical Φ 6 * (15 ± 0.5) mm, requires tapering and out of roundness error at ± 0.01mm.
<3〉end face processing: W40, W20, W10 norbide face off on steel disk are successively used in the processing of titanium precious stone laser rod both ends of the surface.In process of lapping, to note measuring end face squareness.
<4〉chemically machinery polished: polishing workpiece and polishing pad are done relative movement and friction, finish polishing simultaneously under the help of grinding slurry (title polishing fluid) that contains chemical mordant.The polishing condition that the present invention adopts:
Polished die rotating speed: 50 rev/mins
Polishing workpiece stationary installation rotating speed: 50 rev/mins
Polishing workpiece stationary installation swinging distance: 30mm (can regulate as required)
Polishing workpiece stationary installation hunting frequency: 15 round trips of per minute
Polishing fluid: the W0.1 diamond grinds mould cream, uses H 2SO 4: H 3PO 4The dilution of=3: 1 (volume ratio) mixed solution is mixed well
Polishing fluid flow: 200ml/min (can regulate as required)
Be applied to the load on the titanium precious stone laser rod: 400g/cm 2(3.9 * 10 4Pa) (can regulate as required)
Temperature: 25 ℃ of room temperatures
Polish results is checked glazed surface (two planar end surfaces of titanium precious stone laser rod) with the scratch detection instrument under these conditions, does not find cut, and polishing effect is good.
<5〉acid etching:, drop into H through the titanium gem stick after the above-mentioned polishing 2SO 4: H 3PO 4=3: 1 (volume ratio) mixed solution, 300 ℃ of temperature, acid etching 20 minutes.
<6〉surface heat is handled: will use deionized water rinsing 5 minutes through the titanium gem stick behind the acid etching, and carry out surface heat again and handle.The titanium gem stick is placed 1360 ℃ environment, and annealing constant temperature is 1 hour in hydrogen atmosphere, and recording roughness is RMS=0.10nm.
<7〉resisting laser damage: the anti-reflection film (AR) that the pumping both ends of the surface of laser bar is plated 808nm.The laser damage threshold of film is measured by Nd: the output of YAG Q-switched pulse laser, the laser output mode is TE 00, wavelength is 1064nm, pulsewidth (FWHM) was 10 nanoseconds.The laser damage threshold that records film (is 20Jcm -2) than control group through conventional technology (from technology<1〉to<4 〉, but lack<5 and<6〉two steps) laser damage threshold of the laser bar that makes (is 12Jcm -2) be significantly increased.
Test shows that different surface heat treatment condition can bring up planarized surface in various degree, wherein, the titanium gem stick placed 1360 ± 20 ℃ environment, the result of constant temperature after 1~3 hour in hydrogen atmosphere, the surface is the most smooth, has obtained higher roughness.This kind surface heat treatment process parameters optimal.The laser bar substrate surface shows that with the check of atomic power micro-(AFM) photo the titanium jewel under 1360 ℃ of conditions of constant temperature, was annealed 1 hour in hydrogen atmosphere, recording roughness is RMS=0.10nm.
Behind the processing step through the front, carry out the test of plated film and resisting laser damage.Pumping end surface plating anti-reflection film to laser bar.The laser damage threshold of film is measured and is undertaken by the 1-ON-1 mode, is standard with international standard ISO11254, measures zero damage probability laser damage threshold.Testing laser is by Nd: the output of YAG Q-switched pulse laser, the laser output mode is TE 00, wavelength is 1064nm, pulsewidth (FWHM) was 10 nanoseconds.The laser damage threshold that records film than control group through conventional technology (from technology<1〉to<4 〉, but lack<5 and<6〉two steps) laser damage threshold of the laser bar that makes is significantly increased.Its reason is that acid etching and surface heat treatment process removed the sub-surface damage of the machinery that produces in the polishing process on the laser bar surface, and remove various contaminations, thereby obtain the clean surface of smooth smooth, the lattice perfection of atom level, strengthened the bonding force between film and the substrate, the absorption defective of film and substrate interface obtains reducing, and has very high laser-damaged threshold value so be deposited on this very smooth smooth suprabasil film.

Claims (3)

1, a kind of method of surface finish of ti sapphire crystal laser bar comprises the titanium gem crystal orientation, cuts into the laser bar blank, cylinder corase grind and correct grinding, end face processing, chemically machinery polished, it is characterized in that also will handling through acid etching and surface heat.
2, the method for surface finish of ti sapphire crystal laser bar according to claim 1 is characterized in that described acid etching is that the input volume ratio is H the titanium gem stick after the process polishing 2SO 4: H 3PO 4In=3: 1 the mixed solution, 100~400 ℃ of temperature, acid etching 5~30 minutes.
3, the method for surface finish of ti sapphire crystal laser bar according to claim 1 and 2, it is characterized in that it is to use deionized water rinsing 5 minutes through the titanium gem stick behind the acid etching that described surface heat is handled, the titanium gem stick is placed 1360 ± 20 ℃ environment, constant temperature is 1~3 hour under the hydrogen atmosphere condition again.
CN 03116635 2003-04-25 2003-04-25 Surface processing method of titanium-doped sapphire crystal laser rod Expired - Fee Related CN1203965C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1301184C (en) * 2003-12-16 2007-02-21 汪开庆 Optical grinding machine and method for processing sapphire crystal substrate for semiconductor use
CN100346541C (en) * 2005-03-31 2007-10-31 中国工程物理研究院激光聚变研究中心 Edge covering method for large-diameter titanium-doped sapphire crystals
CN101404380A (en) * 2008-11-14 2009-04-08 福建华科光电有限公司 Production method for intracavity frequency doubling micro-chip laser device with two-piece structure
CN102166790A (en) * 2011-01-21 2011-08-31 苏州辰轩光电科技有限公司 Processing method for removing rough surface and scars of sapphire substrate
CN103522149A (en) * 2013-10-14 2014-01-22 无锡荣能半导体材料有限公司 Polishing processing method for crystal bar
CN103639850A (en) * 2013-12-13 2014-03-19 哈尔滨工业大学深圳研究生院 Crystal polishing method
CN103757707B (en) * 2014-01-21 2016-04-06 广东富源科技股份有限公司 A kind of complete processing of sapphire material mobile phone screen cover plate
CN104842225A (en) * 2015-04-22 2015-08-19 苏州爱彼光电材料有限公司 Wet processing method for large-dimension sapphire substrate surface
CN109551312A (en) * 2018-12-18 2019-04-02 福建福晶科技股份有限公司 A kind of surface Cold-forming process of Ti:Sapphire laser
CN110257919A (en) * 2019-05-21 2019-09-20 南京同溧晶体材料研究院有限公司 A kind of uniform diameter single crystal fiber processing method
CN110586568A (en) * 2019-08-29 2019-12-20 江苏吉星新材料有限公司 Cleaning method for sapphire substrate slice after grinding of boron carbide
CN110834264A (en) * 2019-11-27 2020-02-25 湖南大合新材料有限公司 Crystal polishing method

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