CN1203965C - Surface processing method of titanium-doped sapphire crystal laser rod - Google Patents
Surface processing method of titanium-doped sapphire crystal laser rod Download PDFInfo
- 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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- China
- Prior art keywords
- laser
- acid etching
- titanium
- sapphire crystal
- laser bar
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Links
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 10
- 239000010980 sapphire Substances 0.000 title claims abstract description 10
- 238000003672 processing method Methods 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000005498 polishing Methods 0.000 claims abstract description 22
- 238000005530 etching Methods 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000010936 titanium Substances 0.000 claims description 33
- 239000010437 gem Substances 0.000 claims description 31
- 229910001751 gemstone Inorganic materials 0.000 claims description 31
- 229910052719 titanium Inorganic materials 0.000 claims description 31
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000758 substrate Substances 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 13
- 230000003287 optical effect Effects 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 239000010409 thin film Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 4
- 238000007517 polishing process Methods 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010979 ruby Substances 0.000 description 1
- 229910001750 ruby Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- 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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116635 CN1203965C (en) | 2003-04-25 | 2003-04-25 | Surface processing method of titanium-doped sapphire crystal laser rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116635 CN1203965C (en) | 2003-04-25 | 2003-04-25 | Surface processing method of titanium-doped sapphire crystal laser rod |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1460573A CN1460573A (en) | 2003-12-10 |
| CN1203965C true CN1203965C (en) | 2005-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03116635 Expired - Fee Related CN1203965C (en) | 2003-04-25 | 2003-04-25 | Surface processing method of titanium-doped sapphire crystal laser rod |
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| Country | Link |
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Families Citing this family (12)
| 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 |
-
2003
- 2003-04-25 CN CN 03116635 patent/CN1203965C/en not_active Expired - Fee Related
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| CN1460573A (en) | 2003-12-10 |
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