CN104357899A - Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals - Google Patents
Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals Download PDFInfo
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- CN104357899A CN104357899A CN201410671892.8A CN201410671892A CN104357899A CN 104357899 A CN104357899 A CN 104357899A CN 201410671892 A CN201410671892 A CN 201410671892A CN 104357899 A CN104357899 A CN 104357899A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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Abstract
The invention discloses a kyropoulos method-based preparation method of large-size Yb-YAG laser crystals. The kyropoulos method-based preparation method comprises the steps of charging, melting, seeding, necking, shouldering, constant-diameter growing, cooling and annealing. During shouldering, the rotating speed of the crystals is zero; the crystals do not rotate during shouldering and at various stages afterwards. The pulling rate is controlled within the range of 0.05-0.3mm/h; the weight increase rate is controlled within the range of 10-250g/h, and the shouldering process is completed until the diameter of the crystals grows to the desired diameter. During constant-diameter growing, the heating power is adjusted so that the weight of the crystals increases evenly at the increase rate of 250-900g/h until the weight stops increasing, and at the moment, the crystal growth is terminated. The Yb: YAG laser crystals grown by use of the kyropoulos method-based preparation method has outstanding advantages such as large size, low defect density, no core, high utilization rate and low cost, and capable of meeting the requirements of a large-size high-power laser device on the large-size Yb: YAG laser crystals.
Description
Technical field
The present invention relates to laser crystal growth technological improvement, specifically refer to a kind of diameter
Φthe kyropoulos preparation method of the large scale ytterbium doped Yttrium aluminium garnet laser crystal (hereinafter referred to as Yb:YAG) of more than 180mm, belongs to technical field of crystal growth.
Background technology
Under the promotion of the large laser engineerings such as inertial confinement fusion (such as: the national portfire NIF of European high power laser light energy research mechanism HiPER, U.S.'s lawrence livermore laboratory), laser diode-pumped Yb:YAG crystal laser is that development is efficient, a main direction of studying of high power solid state laser.Wherein as the Yb:YAG crystal of core gain medium except there is excellent optics, calorifics and mechanical property, it also has following advantage compared with traditional Nd:YAG crystal: near 940nm, have wider absorption band (18nm), effectively can be coupled with InGaAs laser diode; Quantum defect little (~ 8.6%), the material thermal load that radiationless relaxation causes is low, is only 1/3 of Nd:YAG crystal; Fluorescence lifetime long (951 μ s), is more than 3 times of Nd:YAG crystal, is conducive to energy storage; Without concentration quenching effect; Without excited state absorption and upconversion mechanism.At present, European high power laser light energy research mechanism has planned to adopt diode pumping Yb:YAG crystal laser to obtain the superlaser of more than 100kJ level, and its target is that progressively improving laser power finally realizes laser-produced fusion igniting.On similar large scale laser instrument, all need large-sized Yb:YAG laser crystals.
The main method of current growth Yb:YAG crystal has crystal pulling method (Czochralski method), temperature gradient method (TGT) and Horizontal Bridgman method.Wherein crystal pulling method is modal high melting point crystal growth method, it have process of growth observable, fast growth, without advantages such as parasitic nucleation.The limitation of Czochralski grown large size Yb:YAG crystal is: the fusing point of Yb:YAG crystal about 1950 DEG C, and the fusing point of iridium is 2440 DEG C, and uses iridium crucible that the maximum critical temperature of any damage can not be caused to be 2300 DEG C.Due to large radial symmetry gradient (difference of the melt temperature of sidewall of crucible and its middle), and large radial symmetry gradient is necessary to the crystal preparing optical quality, thus very difficult from iridium crucible long large diameter Yb:YAG crystal in next life by crystal pulling method; Be there is core in germ nucleus by another significant drawbacks of Czochralski grown Yb:YAG crystal, cause the utilization ratio of crystal to reduce.Although improve crystal pulling method technology existing, such as, described in Chinese patent 101338453A, be heated by resistive molybdenum crucible and realize plane interface growth Yb:YAG crystal, the crystal diameter obtained still only has 35 ~ 50mm.Horizontal Bridgman method is different from crystal pulling method, and it is loaded by raw material in the boat type crucible of molybdenum, treat raw material melt after in hot-zone slow mobile crucible, move to cold-zone from hot-zone and make raw material solidification and crystallization.Crystalline size and the shape of the method growth are determined by crucible, usual crystal slabbing, document [M.Arzakantsyan, N.Ananyan, et al, Growth of large 90 mm diameter Yb:YAG single crystals with Bagdasarov method. Optical Materials Express, 2012,2 (9): 1219-1225] report the Yb:YAG laser crystals having grown diameter 90mm.Temperature gradient method is the patent obtained in 1985, is mainly used to growth gem crystal (101705516A Chinese patent), and does not also obtain sufficiently high optical quality in growth garnet crystal, and the Yb:YAG crystalline size adopting this method to grow is to the maximum
Φ75mm × 45mm [X.D. Xu, Z.W. Zhao, et al, Comparison of Yb:YAG crystals grown by Cz and TGT method, Journal of Crystal Growth, 2003,257 (3-4): 297-300].The above method except having any problem in acquisition large size Yb:YAG crystal, and crystal quality is also because of the intrinsic feature of method and existing defects, such as: the crystal that temperature gradient method grows with Horizontal Bridgman method contacts all the time with sidewall of crucible, easy parasitic nucleation, also can cause crystal stress at temperature-fall period because thermal contraction is inconsistent, even cause crystal cleavage; And the crystal of Czochralski grown is often because thermograde is excessive, the defects such as crystal dislocation are more, affect laser activity.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide a kind of large size Yb-YAG laser crystals kyropoulos preparation method, present method can be greater than the Yb-YAG laser crystals of 180mm by growth diameter.
To achieve these goals, the technical solution used in the present invention is as follows:
Large size Yb-YAG laser crystals kyropoulos preparation method, present method Yb:YAG crystal growth carries out in High Temperature Furnaces Heating Apparatus, the body of heater of this High Temperature Furnaces Heating Apparatus there is water coolant access port, the thermal insulation layer of ring-type is provided with in body of heater, be provided with in thermal insulation layer and place the pallet of crucible, bell is provided with seed rod, seed rod upper end and weight sensor, lifts motor and is connected with rotating machine, Yb-YAG laser crystals preparation process is as follows
(1) shove charge: loaded in tungsten crucible by block for the Yb:YAG prepared pre-crystallized raw material, then crucible is placed on pallet, and load onto seed crystal, shove charge is complete, High Temperature Furnaces Heating Apparatus is evacuated to≤5 × 10
-3pa; In the pre-crystallized raw material of Yb:YAG, the doping content of Yb ion is the arbitrary value within the scope of 0.1 ~ 50.0 at.%;
(2) material: open heating power supply, to be increased on raw material fusing point 5 ~ 10 DEG C by crucible temperature; After raw material all melts, regulate heating power to make melt convection form stable, then keep 1 ~ 5h;
(3) seeding: open lift motor, slowly decline seed rod, and seed crystal lower end is contacted with bath surface, controls seeding temperature and seed crystal is neither grown also do not melt;
(4) necking down: after seeding welding, observes knot dish situation, judges that whether cold heart position is at crucible center, if not at crucible center, then rotate seed crystal by rotating machine and make the position of dish to crucible central growth, knot dish diameter is less than 3cm; Knot dish position behind crucible center, then adopts the mode of manually lift to reach the object of necking down, and lift 1 ~ 3mm, the overall height of neck is 2 ~ 4cm at every turn; After adjusting power, enter shouldering process;
(5) shouldering: during shouldering, the rotating speed of crystal is zero, and shouldering and later each stage thereof, crystal does not rotate; Casting speed control within the scope of 0.05 ~ 0.3mm/h, weight gain rate controls within the scope of 10 ~ 250g/h, treats that crystal diameter grows to required diameter, namely completes shouldering process;
(6) isodiametric growth: regulate heating power, crystal weight is evenly increased, and advancing the speed is 250 ~ 900g/h, until weight no longer increases, now crystal growth terminates;
(7) cool: in process of cooling, initial rate of temperature fall is 10 ~ 30 DEG C/h, close heating power supply when temperature is 200 ~ 400 DEG C, then be filled with argon gas, to increase spontaneous rate of temperature fall, until crystal is cooled to room temperature;
(8) anneal: take out crystal from High Temperature Furnaces Heating Apparatus after, then crystal is put into retort furnace at O
2+ N
2anneal under atmosphere or air atmosphere, if O
2+ N
2atmosphere, then O
2concentration is 0.1 ~ 30%, and annealing temperature is 1200 ~ 1350 DEG C, and constant temperature time is 30 ~ 48h, and temperature rise rate is 40 ~ 50 DEG C/h, and rate of temperature fall is 20 ~ 30 DEG C/h.
Described crucible is cylindric, and crucible upper inner diameter is greater than 2 ~ 20% of bottom inner diameter, crucible bottom internal diameter >=200mm.
The direction of the seed crystal that present method uses is [111] direction or [100] direction.
Present method has certain similarity compared with crystal pulling method, all has process of growth observable; The defect that seed crystal extends to crystals can be reduced by necking down technique; Crystal does not contact with crucible, without parasitic nucleation, can not cause the advantages such as stress during cooling.In addition, present method also has the following advantage not available for crystal pulling method:
1, can growth diameter
Φthe large size Yb:YAG crystal of more than 180mm, crystalline size is close with crucible diameter.
2, thermograde little (≤10 DEG C/cm) during crystal growth, can obtain the high-quality Yb:YAG crystal of low-dislocation-density, and under little thermograde, there will not be the reason of constitutional supercooling to be Yb
3+the segregation coefficient of ion in YAG crystal is close to 1.0.
3, after entering the isodiametric growth stage, crystal does not rotate, pulling rate extremely slow (not higher than 0.3mm/h), and avoid the fluctuation of the solid-liquid interface caused because of mechanical vibration, make growth interface more stable, crystal quality is higher.
4, growth interface is convex tapered to melt, and growth die area is little.
5, growth cost of the present invention is lower than crystal pulling method.
In sum, adopt the Yb:YAG crystal of kyropoulos growth, there is the outstanding advantages such as size is large, defect concentration is low, coreless (or core is little), utilization ratio is high, cost is low, the demand of large-scale device of high power laser to large size Yb:YAG crystal can be met.Meanwhile, the popularization of this technology, also has obvious economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the raw stove schematic diagram of bubble of growth Yb:YAG crystal.
In figure, 1-water coolant access port, 2-body of heater, 3-thermal insulation layer, 4-crucible, 5-heating electrode, 6-seed rod, 7-YAG seed crystal, 8-support bar.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Kyropoulos growth Yb:YAG crystal of the present invention, it carries out in High Temperature Furnaces Heating Apparatus, and High Temperature Furnaces Heating Apparatus structure as shown in Figure 1.The body of heater 2 of High Temperature Furnaces Heating Apparatus has water coolant access port 1, is provided with tungsten crucible 4 in body of heater 2, crucible 4 is arranged on a pallet, and pallet is supported by the support bar 8 being arranged on burner hearth center.Have thermal insulation layer 3 between crucible and body of heater, bell is provided with seed rod 6, seed rod 6 upper end and weight sensor, lifts motor and is connected with rotating machine, and YAG seed crystal 7 is equipped with in seed rod 6 lower end.Label 5 is heating electrode.The present invention carries out according to the following steps:
(1) shove charge: block for the Yb:YAG prepared pre-crystallized raw material is loaded in tungsten crucible, then crucible fork truck is hung on the pallet in the raw stove burner hearth of bubble, then load onto stay-warm case, seed crystal and bell successively.Finally be evacuated to≤5 × 10
-3pa.
(2) material: open heating power supply, to be increased on raw material fusing point 5 ~ 10 DEG C by crucible temperature.After raw material all melts, regulate heating power to make melt convection form stable, then keep 1 ~ 5h.
(3) seeding: open lift motor, slowly decline seed rod, and seed crystal lower end is contacted with bath surface, if seed crystal neither grows when also not melting, temperature is best seeding temperature.
(4) necking down: after seeding welding, by observing knot dish situation, judge that whether cold heart position is at crucible center, determine whether that rotating seed crystal by rotating machine makes the position of dish to crucible central growth, knot dish diameter is as far as possible little, and diameter is less than 3cm, determine that dish position is behind crucible center, start to adopt the mode of manually lift to reach the object of necking down, lift at 1 ~ 3mm, the overall height of neck is 2 ~ 4cm at every turn.After adjusting power, enter shouldering process.
(5) shouldering: casting speed control within the scope of 0.05 ~ 0.3mm/h, weight gain rate controls within the scope of 10 ~ 250g/h, treats that crystal diameter grows to required diameter, namely completes shouldering process.
(6) isodiametric growth: regulate heating power, crystal weight is evenly increased, and advancing the speed is 250 ~ 900g/h, until weight no longer increases.
(7) cool: in process of cooling, initial rate of temperature fall is 10 ~ 30 DEG C/h, close heating power supply when temperature is 200 ~ 400 DEG C, then be filled with high-purity argon gas, to increase spontaneous rate of temperature fall, until crystal is cooled to room temperature.
(8) anneal: take out crystal from High Temperature Furnaces Heating Apparatus after, then crystal is put into retort furnace at O
2+ N
2(O
2concentration is 0.1 ~ 30%) to anneal under atmosphere or air atmosphere, annealing temperature is 1200 ~ 1350 DEG C, and constant temperature time is 30 ~ 48h, and temperature rise rate is 40 ~ 50 DEG C/h, and rate of temperature fall is 20 ~ 30 DEG C/h.
In above-mentioned steps (1), in the pre-crystallized raw material of Yb:YAG, the doping content of Yb ion can be the arbitrary value within the scope of 0.1 ~ 50.0 at.%.The weight of raw material is 36 ~ 100kg, and this is relevant with crucible size with the doping content of Yb ion.
In above-mentioned steps (1), tungsten crucible is cylindric, and crucible upper inner diameter is greater than 2 ~ 20% of bottom inner diameter, and crucible bottom internal diameter is 200mm or larger.
The direction of the seed crystal used in above-mentioned steps (3) is [111] direction or [100] direction.
In above-mentioned steps (5), the rotating speed of crystal is zero, and pulling rate is lower than 0.3mm/h, or pulling rate is zero.
Below provide two embodiments to help to understand the present invention further.
Embodiment 1:
In the tungsten crucible cross pre-crystallized high-purity block Yb:YAG raw material 37kg loading ethanol wash, carry out shove charge.Yb in raw material
3+the concentration of ion is 2.0at.%, and tungsten crucible upper inner diameter is 230mm, and lower inner diameter is 200mm, and interior height is 325mm.After installing stove, burner hearth is evacuated to 5 × 10
-3during Pa, carry out resistive heating intensification by the speed of 6kW/h, until raw material all melts, observe in melt when having stable liquid fluid line, insulation 1h.Slow adjustment YAG seed crystal makes its lower end drop to 5mm place above melt liquid level, and the geometric centre relative deviation of seed crystal center and crucible is not more than 10mm, and observes seed crystal head and whether have melting phenomenon, if there is melting phenomenon, temperature is too high, need reduce heating power.YAG seed crystal is immersed in melt, regulate heating power, seed crystal is neither grown up also non-fusible, namely complete seeding process.Reduce heating power 1kW, when seed crystal head knot dish diameter is about 2cm, manually lift seed rod carries out necking down, and each lift is highly 2mm, cocondensation neck 10 times.After necking down, pull rate is adjusted to 0.3mm/h, and regulates heating power, make weight respectively by 30g/h(0 ~ 500g), 70g/h(500g ~ 2kg), 120g/h(2 ~ 4kg) mode increase, until when crystal diameter is about 190mm, namely complete shouldering.And then enter the isodiametric growth stage by the speed of 350g/h, now pulling rate is set to 0.07mm/h, and after waiting crystal mass no longer to increase, crystal growth terminates.Whole process of growth is carried out under vacuo.Then regulate heating power, lower the temperature by the speed of 30 DEG C/h, when in-furnace temperature is 300 DEG C, close heating power supply, then pass into high-purity Ar gas, make the pressure in burner hearth equal with normal atmosphere, after 48h, take out crystal boule.The Yb:YAG crystal boule diameter taken out from the raw stove of bubble is 190mm, because Yb
2+the colour center that ion causes exists, and crystal is light blue.
Yb:YAG crystal boule obtained above is put into retort furnace, in air atmosphere by the ramp to 1250 DEG C of 50 DEG C/h, then constant temperature 48h, then be cooled to room temperature by the rate of temperature fall of 25 DEG C/h, finally take out crystal, crystal water white transparency.
Embodiment 2:
In the tungsten crucible cross pre-crystallized high-purity block Yb:YAG raw material 41kg loading ethanol wash, carry out shove charge.Yb in raw material
3+the concentration of ion is 30.0at.%, and tungsten crucible upper inner diameter is 230mm, and lower inner diameter is 200mm, and interior height is 325mm.After installing stove, burner hearth is evacuated to 5 × 10
-3during Pa, carry out resistive heating intensification by the speed of 6kW/h, until raw material all melts, observe in melt when having stable liquid fluid line, insulation 1h.Slow adjustment YAG seed crystal makes its lower end drop to 5mm place above melt liquid level, and the geometric centre relative deviation of seed crystal center and crucible is not more than 10mm, and observes seed crystal head and whether have melting phenomenon, if there is melting phenomenon, temperature is too high, need reduce heating power.YAG seed crystal is immersed in melt, regulate heating power, seed crystal is neither grown up also non-fusible, namely complete seeding process.Reduce heating power 1kW, when seed crystal head knot dish diameter is about 2cm, manually lift seed rod carries out necking down, and each lift is highly 2mm, cocondensation neck 10 times.After necking down, pull rate is adjusted to 0.3mm/h, and regulates heating power, make weight respectively by 35g/h(0 ~ 560g), 80g/h(560g ~ 2.3kg), 135g/h(2.3 ~ 4.5kg) mode increase, until when crystal diameter is about 190mm, namely complete shouldering.And then enter the isodiametric growth stage by the speed of 400g/h, now pulling rate is set to 0.07mm/h, and after waiting crystal mass no longer to increase, crystal growth terminates.Whole process of growth is carried out under vacuo.Then regulate heating power, lower the temperature by the speed of 30 DEG C/h, when in-furnace temperature is 300 DEG C, close heating power supply, then pass into high-purity Ar gas, make the pressure in burner hearth equal with normal atmosphere, after 48h, take out crystal boule.The Yb:YAG crystal boule diameter taken out from the raw stove of bubble is 190mm, because Yb
2+the colour center that ion causes exists, and crystal is light blue.
Yb:YAG crystal boule obtained above is put into retort furnace, in air atmosphere by the ramp to 1250 DEG C of 50 DEG C/h, then constant temperature 48h, then be cooled to room temperature by the rate of temperature fall of 25 DEG C/h, finally take out crystal, crystal water white transparency.
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (4)
1. large size Yb-YAG laser crystals kyropoulos preparation method, it is characterized in that: present method Yb:YAG crystal growth carries out in High Temperature Furnaces Heating Apparatus, the body of heater of this High Temperature Furnaces Heating Apparatus there is water coolant access port, the thermal insulation layer of ring-type is provided with in body of heater, be provided with in thermal insulation layer and place the pallet of crucible, bell is provided with seed rod, seed rod upper end and weight sensor, lifts motor and is connected with rotating machine, Yb-YAG laser crystals preparation process is as follows
(1) shove charge: loaded in tungsten crucible by block for the Yb:YAG prepared pre-crystallized raw material, then crucible is placed on pallet, and load onto seed crystal, shove charge is complete, High Temperature Furnaces Heating Apparatus is evacuated to≤5 × 10
-3pa;
(2) material: open heating power supply, to be increased on raw material fusing point 5 ~ 10 DEG C by crucible temperature; After raw material all melts, regulate heating power to make melt convection form stable, then keep 1 ~ 5h;
(3) seeding: open lift motor, slowly decline seed rod, and seed crystal lower end is contacted with bath surface, controls seeding temperature and seed crystal is neither grown also do not melt;
(4) necking down: after seeding welding, observes knot dish situation, judges that whether cold heart position is at crucible center, if not at crucible center, then rotate seed crystal by rotating machine and make the position of dish to crucible central growth, knot dish diameter is less than 3cm; Knot dish position behind crucible center, then adopts the mode of manually lift to reach the object of necking down, and lift 1 ~ 3mm, the overall height of neck is 2 ~ 4cm at every turn; After adjusting power, enter shouldering process;
(5) shouldering: during shouldering, the rotating speed of crystal is zero, and casting speed control within the scope of 0.05 ~ 0.3mm/h, weight gain rate controls within the scope of 10 ~ 250g/h, treats that crystal diameter grows to required diameter, namely completes shouldering process;
(6) isodiametric growth: regulate heating power, crystal weight is evenly increased, and advancing the speed is 250 ~ 900g/h, until weight no longer increases, now crystal growth terminates;
(7) cool: in process of cooling, initial rate of temperature fall is 10 ~ 30 DEG C/h, close heating power supply when temperature is 200 ~ 400 DEG C, then be filled with argon gas, to increase spontaneous rate of temperature fall, until crystal is cooled to room temperature;
(8) anneal: take out crystal from High Temperature Furnaces Heating Apparatus after, then crystal is put into retort furnace at O
2+ N
2anneal under atmosphere or air atmosphere, if O
2+ N
2atmosphere, then O
2concentration is 0.1 ~ 30%, and annealing temperature is 1200 ~ 1350 DEG C, and constant temperature time is 30 ~ 48h, and temperature rise rate is 40 ~ 50 DEG C/h, and rate of temperature fall is 20 ~ 30 DEG C/h.
2. large size Yb-YAG laser crystals kyropoulos preparation method according to claim 1, is characterized in that: described crucible is for cylindric, and crucible upper inner diameter is greater than 2 ~ 20% of bottom inner diameter, crucible bottom internal diameter >=200mm.
3. large size Yb-YAG laser crystals kyropoulos preparation method according to claim 1, is characterized in that: the direction of the seed crystal that present method uses is [111] direction or [100] direction.
4. large size Yb-YAG laser crystals kyropoulos preparation method according to claim 1, is characterized in that: in the pre-crystallized raw material of Yb:YAG, the doping content of Yb ion is the arbitrary value within the scope of 0.1 ~ 50.0 at.%.
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| PCT/CN2015/077069 WO2016078321A1 (en) | 2014-11-21 | 2015-04-21 | Method for preparing large size yb-yag laser crystal through kyropoulos method |
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| CN110067025A (en) * | 2018-01-20 | 2019-07-30 | 河北胤丞光电科技有限公司 | A kind of preparation method of the YAG crystal of high-output power |
| CN108531979A (en) * | 2018-04-25 | 2018-09-14 | 上海翌波光电科技股份有限公司 | A kind of crystal manufacture stove and crystal manufacturing process |
| CN112296511A (en) * | 2020-09-30 | 2021-02-02 | 北京德弦科技有限公司 | Method for processing, reading and detecting miniature mark of gem and processing device |
| CN114836821A (en) * | 2021-02-01 | 2022-08-02 | 浙江大学杭州国际科创中心 | Growth method of low dislocation density gallium oxide bulk single crystal |
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| WO2016078321A1 (en) | 2016-05-26 |
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