CN1477239A - Growth method of composite laser crystal - Google Patents
Growth method of composite laser crystal Download PDFInfo
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- CN1477239A CN1477239A CNA031415288A CN03141528A CN1477239A CN 1477239 A CN1477239 A CN 1477239A CN A031415288 A CNA031415288 A CN A031415288A CN 03141528 A CN03141528 A CN 03141528A CN 1477239 A CN1477239 A CN 1477239A
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- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 230000012010 growth Effects 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 3
- 239000000758 substrate Substances 0.000 claims abstract description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 30
- 239000010931 gold Substances 0.000 claims description 30
- 229910052737 gold Inorganic materials 0.000 claims description 30
- 230000006798 recombination Effects 0.000 claims description 26
- 238000005215 recombination Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 18
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002178 crystalline material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 239000006193 liquid solution Substances 0.000 abstract 2
- 238000002109 crystal growth method Methods 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000004973 liquid crystal related substance Substances 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
A growth method of composite laser crystal is characterized in that a hydrothermal method is adopted to directly grow YAG crystals at two ends of a doped YAG laser single crystal to form a composite laser crystal material. The YAG liquid crystal growth method is characterized in that a high-pressure kettle and a matched resistance furnace are adopted, the temperature of a growth area and a dissolution area in a reaction cavity is proper through reasonable temperature field design, the YAG liquid solution with high temperature and high pressure reaches a certain supersaturation degree, and when the solution in a container generates convection due to the temperature difference between the upper part and the lower part, the saturated YAG liquid solution in a high-temperature area is sent to two interfaces of a substrate seed wafer of a YAG laser single crystal in a low-temperature area to grow a YAG body single crystal with a certain thickness. The invention can directly grow Nd: YAG (or Yb: YAG) and YAG together, the crystal lattice is not mismatched, and two kinds of grown YAG/Nd: YAG (or Yb: YAG)/YAG crystals have no obvious boundary, and have good crystal integrity and good repeatability.
Description
Technical field
The present invention relates to the recombination laser crystal, particularly a kind of recombination laser crystalline growth method.Be specifically related at Nd: (or Yb: YAG) monocrystalline two ends growths YAG is combined into recombination laser crystalline material: YAG/Nd: YAG (or Yb: YAG)/YAG to YAG.
Background technology
Nd: YAG is a present the most frequently used class solid laser medium, and YAG matrix hardness height, optical quality is good, thermal conductivity is high, and Nd: YAG has the laser activity of high gain, low threshold value, is good concussion and amplification medium.
Same is the Yb of matrix with YAG: the YAG crystal, owing to have good optics, thermodynamics and mechanical property, chemical stability is good, has high-quantum efficiency, can carry out the characteristics such as doping of higher concentration, becomes and mixes Yb
3+Outstanding person in the laserable material.
Along with the development of superpower, intensity laser technology and semiconductor laser diode (LD) pump technology, more and more higher to the requirement of laser medium crystalline laser damage threshold.People such as G.E.Devlin had reported with flame method at Cr: Al in 1962
2O
3Al on every side grows
2O
3(referring to the 1st phase of Appl.Opt., 1962 the 11st page).Human guided mode methods such as V.N.Kurlov were at Ti: Al in 1998
2O
3Al on every side grows
2O
3(referring to the 191st phase of Journal of CrystalGrowth, 1998 the 520th page).People such as R.Weber proposed at Nd in 1998: the composite structure of the pure YAG crystal bar of YAG laser bar two ends optical cement, because pure YAG crystal is not to pump light or concussion photoabsorption, effective heat-eliminating medium, reduce heat effect and thermal lensing effect, in addition at pure YAG rod two ends plated film, the laser damage threshold that improves rete there is positive effect, thereby improved laser activity greatly, reduced laser threshold (referring to IEEE JournAl of Quantum Electronics, the 6th phase, the 34th the volume, 1998 the 1064th page).People such as D.Ehrentraut in 2002 have reported with improved crystal pulling method in pure YAG pipe growth inside Yb doped YAG (referring to JournAl of CrystAl the 242nd phase of Growth, 2002 years the 375th page).
The composite laser material of above-mentioned technology formerly, significant disadvantages is arranged: (1) forms by optical coupled agent or directly superimposed (optical cement): because the mismatch of optical coupled agent and single crystal, and there is significantly boundary between pure crystal and doped crystal, makes optical loss big; (2) composite single crystal of crystal pulling method, flame method and guided mode method direct growth, crystal mass is poor, has defectives such as a large amount of bubbles and wrap, and it is low to grow into power, not practical application in device so far.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the defective of above-mentioned technology formerly, a kind of recombination laser crystalline growth method is provided, make the recombination laser crystalline material of being grown have not mismatch of lattice, do not have sharp interface, the characteristics of the very little and good reproducibility of optical loss.
Technical solution of the present invention is;
A kind of recombination laser crystalline growth method is characterized in that adopting hydrothermal method directly at the two ends of doping YAG laser monocrystalline growth YAG crystal, forms the recombination laser crystalline material.
Described doping YAG laser monocrystalline is Nd: YAG, this Nd: the YAG doping content is for O.2-3mol%.
Described recombination laser crystalline growth method, be to adopt autoclave and supporting with it resistance furnace, by the design of rational temperature, make the temperature of interior vitellarium of reaction chamber and dissolve area suitable, make the YAG aqueous solution of High Temperature High Pressure reach certain degree of supersaturation, when the solution in the container produced convection current owing to the temperature difference between the top and the bottom, the saturated YAG aqueous solution of high-temperature zone was sent to the certain thickness YAG body monocrystalline of growth on two interfaces of substrate seed wafer of YAG laser monocrystalline of cold zone.
The growing apparatus of the composite laser material that the present invention is used is that the high temperature and high pressure kettle of a tyre stay-warm case and supporting with it temperature difference well formula resistance furnace are formed, described high temperature and high pressure kettle comprises: vitellarium, dissolve area, steel cap and steel still, the internal chamber wall of this steel still is provided with the gold lining, the trapezoidal seed crystal frame that uses the gold silk to make, the seed wafer that cuts by certain orientation couples together with the gold silk and is fixed on the seed crystal frame, and gold lining inner chamber has mineralizer and H
2The mixing solutions of O, YAG or Y
2O
3With Al
2O
3The mixture culture material is positioned at dissolve area, and baffle plate with holes is arranged at culture material top.
The step that present method comprises is as follows:
1. at first the YAG crystal or the Al of some amount and particle diameter melt method for growing
2O
3With Y
2O
3Mixture powder (Al
2O
3Content is 0.60-0.85wt%) agglomerate puts into the dissolve area of gold sleeve;
2. add alkali-metal mineralizer 7 and H by the compactedness of the 55%-75% percentage ratio of the shared autoclave free volume of solution in the autoclave (compactedness refer to pack under the room temperature)
2The O mixing solutions.
3. the trapezoidal seed crystal frame that uses the gold silk to make, the Nd that cuts by certain orientation: the YAG seed wafer couples together with the gold silk and is fixed on the seed crystal frame;
4. the seed crystal frame is slowly put into gold bushing pipe and good seal and put into autoclave more together, again the autoclave envelope is thoroughly also slowly put into resistance furnace;
5. resistance furnace heats up, adjust temperature and pressure, control the required temperature and the temperature difference, reach the autoclave reaction chamber internal and external equilibrium temperature of design, and being under the constant temperature growth, growth cycle is according to YAG/Nd: the YAG gauge in the YAG/YAG matrix material requires to decide;
6. stay-warm case is opened in blowing out, and autoclave proposes burner hearth.Take out the seed crystal frame, take out crystal, the solution of plane of crystal is cleaned, obtain YAG/Nd: YAG/YAG recombination laser crystal with warm water.
Described doping YAG laser monocrystalline is Yb: YAG, and this Yb: the YAG doping content is 0.2-50mol%, and described seed wafer is Yb: YAG, that obtain at last then is YAG/Yb: YAG/YAG recombination laser crystal.
The present invention compares with technology formerly, on the one hand, compares Nd with formerly technical optics couplant or directly superimposed (optical cement): YAG (or Yb: YAG) with the YAG direct growth together, do not have lattice mismatch, do not have sharp interface, optical loss is very little.On the other hand, compare with the composite single crystal of crystal pulling method formerly, flame method and the growth of guided mode method, and the YAG/Nd of Hydrothermal Growth: YAG (or Yb: YAG)/there is not obviously boundary between two kinds of crystal of YAG, perfection of crystal is good, good reproducibility.Suitable batch of the present invention is produced, and satisfies the market requirement in macro-energy, the manufacturing of high power laser device.
Description of drawings
Fig. 1 is the used growing apparatus diagrammatic cross-section of preparation recombination laser crystalline material.
Embodiment
See also Fig. 1 earlier, Fig. 1 is the growing apparatus of the used composite laser material of the present invention, is that the high temperature and high pressure kettle of a tyre stay-warm case and supporting with it temperature difference well formula resistance furnace 10 are formed.Its structure mainly comprises: vitellarium 1, dissolve area 2, steel cap 3, steel still 4.In order to prolong the life-span of autoclave, prevent the corrosion under High Temperature High Pressure of acidity or basic solution to the still internal chamber wall, use gold lining 5 to separate with the autoclave inwall as the protection lining.The trapezoidal seed crystal frame 6 that uses the gold silk to make, the seed wafer that cuts by certain orientation couple together with the gold silk and fixing on the top of the shelf, whenever next ladder frame can be hung tens of (deciding on seed crystal is big or small).Gold lining 5 inner chambers have mineralizer 7 and H
2The mixing solutions of O, YAG or Y
2O
3With Al
2O
3Mixture culture material 8 is positioned at dissolve area 2, and baffle plate with holes 9 is arranged at culture material 8 tops.
It is as follows that the present invention prepares recombination laser crystalline concrete steps:
<1〉at first the YAG crystal or the Al of some amount and particle diameter melt method for growing
2O
3With Y
2O
3Mixture powder (Al
2O
3Content is 0.60-0.85wt%) agglomerate puts into the dissolve area 2 of gold lining 5 bottoms.
<2〉add alkali-metal mineralizer 7 and H by the compactedness of the 55%-75% percentage ratio of the shared autoclave free volume of solution in the autoclave (compactedness refer to pack under the room temperature)
2The O mixing solutions.
<3〉the trapezoidal seed crystal frame 6 that uses the gold silk to make, the seed wafer that cuts by certain orientation couples together with the gold silk and fixes on the top of the shelf.
<4〉seed crystal frame 6 is slowly put into gold bushing pipe and good seal and put into autoclave more together, again the autoclave envelope is thoroughly also slowly put into resistance furnace 10.
<5〉resistance furnace 10 heats up, and adjusts temperature and pressure, controls the required temperature and the temperature difference, reaches the autoclave reaction chamber internal and external equilibrium temperature of design, and is in growth under the constant temperature.Growth cycle is according to YAG/Nd: YAG (or Yb: YAG)/ YAG gauge in the YAG matrix material requires to decide.
<6〉stay-warm case is opened in blowing out, and autoclave proposes burner hearth.Take out the seed crystal frame, take out crystal, the solution of seed crystal face is cleaned with warm water.
Embodiment 1:Nd: YAG and the growth of YAG recombination laser crystalline
Prepare Nd with above-mentioned hydrothermal growth method and concrete growth technique step: YAG.Selected Hydrothermal Growth stove device as shown in Figure 1, vitellarium 1, dissolve area 2, steel cap 3, steel still 4, cavity size Ф 38mm * 700mm, gold lining 5, lining inner cavity size Ф 30mm * 690mm, thickness of pipe 0.8mm, gold seed crystal frame 6 and YAG culture material 8.
<1〉directly be 4-8mm YAG crystal or Al with 100 gram particles
2O
3With Y
2O
3Mixture powder (Al
2O
3Content is 60-85wt%) agglomerate puts into the dissolve area 2 of gold lining 5 bottoms.
<2〉the mineralizer K for preparing again
2CO
3The mixing solutions of (concentration is 6mol/L) and water adds the mixing solutions of mineralizer and water respectively by 80%, 85%, 90% compactedness.
<3〉the trapezoidal seed crystal frame 6 that uses the gold silk to make, the Nd of 30 * 30 * 15mm that cuts by (111) direction: the polishing of YAG (Nd doping content 1mol%) seed wafer two ends optical grade, spile at the edge, connect aperture with the gold silk, and fixing on the top of the shelf.
<4〉the seed crystal frame is slowly put into gold lining 5, and good seal puts into autoclave more together, and slowly put into resistance furnace 10.
<5〉resistance furnace 10 heats up, and adjusts temperature and pressure.The dissolve area temperature is 400 ℃, and the vitellarium temperature is 360 ℃, 40 ℃ of the temperature difference; Operating pressure 172MPa; In the 10 ℃/h of heat-up rate, the autoclave internal and external temperature reaches balance, and the constant temperature growth is 15 days under this temperature.
<6〉stay-warm case is opened in cooling, blowing out, and autoclave proposition burner hearth takes out the crystal 5 piece, and every crystal is thick plate-like, Nd: YAG both ends of the surface YAG thickness all reaches 8mm. warm water plane of crystal solution, and crystal is sparkling and crystal-clear transparent, does not have cotton nothing and splits, and integrity is good.
With the YAG/Nd that is grown: make all solid state laser behind the cutting of YAG/YAG recombination laser crystalline material, round as a ball, processing, the plated film, laser threshold reduces by 10%, and the laser output efficiency improves 5%.This recombination laser crystal has wide application background.
Embodiment 2:Yb: YAG and the growth of YAG recombination laser crystalline
In step<3〉Nd: YAG seed wafer Yb: YAG replaced, other were with embodiment 1.
Claims (6)
1, a kind of recombination laser crystalline growth method is characterized in that adopting hydrothermal method directly at the two ends of doping YAG laser monocrystalline growth YAG crystal, forms the recombination laser crystalline material.
2, recombination laser crystalline growth method according to claim 1 is characterized in that described doping YAG laser monocrystalline is Nd: YAG, and this Nd: the YAG doping content is 0.2-3mol%.
3, recombination laser crystalline growth method according to claim 2, it is characterized in that adopting autoclave and supporting with it resistance furnace, by the design of rational temperature, make the temperature of interior vitellarium of reaction chamber and dissolve area suitable, make the YAG aqueous solution of High Temperature High Pressure reach certain degree of supersaturation, when the solution in the container produced convection current owing to the temperature difference between the top and the bottom, the saturated YAG aqueous solution of high-temperature zone was sent to the certain thickness YAG body monocrystalline of growth on two interfaces of substrate seed wafer of YAG laser monocrystalline of cold zone.
4, recombination laser crystalline growth method according to claim 3, the growing apparatus that it is characterized in that the composite laser material that the present invention is used is that the high temperature and high pressure kettle of a tyre stay-warm case and supporting with it temperature difference well formula resistance furnace (10) are formed, described high temperature and high pressure kettle comprises: vitellarium (1), dissolve area (2), steel cap (3) and steel still (4), the internal chamber wall of this steel still (4) is provided with gold lining (5), the trapezoidal seed crystal frame (6) that uses the gold silk to make, the seed wafer that cuts by certain orientation couples together with the gold silk and is fixed on the seed crystal frame (6), and gold lining (5) inner chamber has mineralizer (7) and H
2The mixing solutions of O, YAG or Y
2O
3With Al
2O
3Mixture culture material (8) is positioned at dissolve area (2), and baffle plate with holes (9) is arranged at culture material (8) top.
5, recombination laser crystalline growth method according to claim 4 is characterized in that the step that present method comprises is as follows:
1. at first the YAG crystal or the Al of some amount and particle diameter melt method for growing
2O
3With Y
2O
3Mixture powder (Al
2O
3Content is 0.60-0.85wt%) agglomerate puts into the dissolve area (2) of gold lining (5) bottom;
2. add alkali-metal mineralizer 7 and H by the compactedness of the 55%-75% percentage ratio of the shared autoclave free volume of solution in the autoclave (compactedness refer to pack under the room temperature)
2The O mixing solutions.
3. the trapezoidal seed crystal frame (6) that uses the gold silk to make, the Nd that cuts by certain orientation: the YAG seed wafer couples together with the gold silk and is fixed on the seed crystal frame (6);
4. seed crystal frame (6) is slowly put into gold bushing pipe (5) and good seal and put into autoclave more together, again the autoclave envelope is thoroughly also slowly put into resistance furnace (10);
5. resistance furnace (10) heats up, adjust temperature and pressure, control the required temperature and the temperature difference, reach autoclave (4) the reaction chamber internal and external equilibrium temperature of design, and being under the constant temperature growth, growth cycle is according to YAG/Nd: the YAG gauge in the YAG/YAG matrix material requires to decide;
6. stay-warm case is opened in blowing out, and autoclave (4) proposes burner hearth.Take out the seed crystal frame, take out crystal, the solution of plane of crystal is cleaned, obtain YAG/Nd: YAG/YAG recombination laser crystal with warm water.
6, according to claim 1 or 2 or 3 or 4 or 5 described recombination laser crystalline growth methods, it is characterized in that described doping YAG laser monocrystalline is Yb: YAG, this Yb: the YAG doping content is 0.2-50mol%, described seed wafer is Yb: YAG, that obtain at last then is YAG/Yb: YAG/YAG recombination laser crystal.
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Cited By (10)
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CN100358194C (en) * | 2006-03-07 | 2007-12-26 | 上海大学 | Method for preparing composite Ti:Al2O3 laser rod |
CN101103143B (en) * | 2005-01-12 | 2012-06-27 | 株式会社古屋金属 | Pressure vessel for growing single crystal |
CN102534790A (en) * | 2012-01-19 | 2012-07-04 | 山东大学 | Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof |
CN103436952A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Neodymium-doped yttrium aluminum garnet and pure yttrium aluminum garnet bonded growth method |
CN107815725A (en) * | 2017-12-11 | 2018-03-20 | 桂林百锐光电技术有限公司 | Hydrothermal crystallization device with alternation thermal field and the method using device growth crystal |
CN109280963A (en) * | 2018-08-24 | 2019-01-29 | 中国科学院合肥物质科学研究院 | A kind of composite plate laser crystal and its reverse mould method preparation method |
CN111424318A (en) * | 2020-06-10 | 2020-07-17 | 眉山博雅新材料有限公司 | Method for preparing doped YAG single crystal optical fiber |
CN112795987A (en) * | 2020-12-28 | 2021-05-14 | 北京雷生强式科技有限责任公司 | Preparation method of composite laser crystal |
CN113122908A (en) * | 2021-03-23 | 2021-07-16 | 桂林百锐光电技术有限公司 | Preparation method of composite YAG crystal |
CN114351244A (en) * | 2021-12-29 | 2022-04-15 | 北京雷生强式科技有限责任公司 | Temperature control mechanism, composite laser crystal growth system and preparation method of composite laser crystal |
-
2003
- 2003-07-11 CN CNA031415288A patent/CN1477239A/en active Pending
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101103143B (en) * | 2005-01-12 | 2012-06-27 | 株式会社古屋金属 | Pressure vessel for growing single crystal |
CN100358194C (en) * | 2006-03-07 | 2007-12-26 | 上海大学 | Method for preparing composite Ti:Al2O3 laser rod |
CN102534790A (en) * | 2012-01-19 | 2012-07-04 | 山东大学 | Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof |
CN102534790B (en) * | 2012-01-19 | 2014-11-05 | 山东大学 | Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof |
CN103436952A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Neodymium-doped yttrium aluminum garnet and pure yttrium aluminum garnet bonded growth method |
CN107815725B (en) * | 2017-12-11 | 2023-12-19 | 桂林百锐光电技术有限公司 | Hydrothermal crystallization device with alternating temperature field and method for growing crystals by using same |
CN107815725A (en) * | 2017-12-11 | 2018-03-20 | 桂林百锐光电技术有限公司 | Hydrothermal crystallization device with alternation thermal field and the method using device growth crystal |
CN109280963A (en) * | 2018-08-24 | 2019-01-29 | 中国科学院合肥物质科学研究院 | A kind of composite plate laser crystal and its reverse mould method preparation method |
US11136690B1 (en) | 2020-06-10 | 2021-10-05 | Meishan Boya Advanced Materials Co., Ltd. | Method for preparing doped yttrium aluminum garnet single crystal fiber by performing a cylindrical surface polishing operation and growing a cladding layer |
CN111424318A (en) * | 2020-06-10 | 2020-07-17 | 眉山博雅新材料有限公司 | Method for preparing doped YAG single crystal optical fiber |
CN112795987A (en) * | 2020-12-28 | 2021-05-14 | 北京雷生强式科技有限责任公司 | Preparation method of composite laser crystal |
CN113122908A (en) * | 2021-03-23 | 2021-07-16 | 桂林百锐光电技术有限公司 | Preparation method of composite YAG crystal |
CN114351244A (en) * | 2021-12-29 | 2022-04-15 | 北京雷生强式科技有限责任公司 | Temperature control mechanism, composite laser crystal growth system and preparation method of composite laser crystal |
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