CN102230218A - Preparation method of ytterbium-doped lithium lutetium fluoride crystal - Google Patents
Preparation method of ytterbium-doped lithium lutetium fluoride crystal Download PDFInfo
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- CN102230218A CN102230218A CN201110151751XA CN201110151751A CN102230218A CN 102230218 A CN102230218 A CN 102230218A CN 201110151751X A CN201110151751X A CN 201110151751XA CN 201110151751 A CN201110151751 A CN 201110151751A CN 102230218 A CN102230218 A CN 102230218A
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- 239000013078 crystal Substances 0.000 title claims abstract description 61
- WVCSLTZAWJBKBL-UHFFFAOYSA-J lithium;lutetium(3+);tetrafluoride Chemical compound [Li+].[F-].[F-].[F-].[F-].[Lu+3] WVCSLTZAWJBKBL-UHFFFAOYSA-J 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 11
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 11
- 230000007423 decrease Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 208000005156 Dehydration Diseases 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 18
- 229910052697 platinum Inorganic materials 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 206010013786 Dry skin Diseases 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000005281 excited state Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910004261 CaF 2 Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 241001424413 Lucia Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 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 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
A preparation method of ytterbium-doped lutetium lithium fluoride crystals is provided, which is characterized in that high-quality ytterbium-doped lutetium lithium fluoride laser crystals are grown by a Bridgman method under the conditions of no vacuum, no pressurization and no atmosphere ventilation. The invention has the characteristics of simple and convenient process, simple equipment and low growth cost.
Description
Technical field
The present invention relates to the preparation method of laser crystal material, especially a kind of preparation method of ytterbium doping lithium lutetium fluoride crystal.
Background technology
Laser technology has just obtained the development of advancing by leaps and bounds since the invention of first laser apparatus, and has obtained application widely in fields such as industry, medical treatment, information science, biotechnology and military affairs.Along with the raising of laser power, superlaser can be used for the aspects such as cutting, boring, welding and surface treatment of multiple material.The superlaser Push Technology of studying at present utilizes ground-launched laser to give the propelling agent energy supply of rocket engine, forms high temperature and high pressure gas or plasma body, produces rocket thrust.High energy laser system also can be used for to the energy supply of space orbit satellite, to prolong satellite life; Can also collect sun power in the space, be converted into laser energy, carry out the energy directional transmission earthward, be converted to heat energy or electric energy again and use.
Adopt all solid state laser of diode-end-pumped owing to had that volume is little, efficient is high, characteristics such as long and light velocity quality of life-span number are widely studied, and wherein superpower macro-energy solid statelaser is the important directions that solid statelaser develops.Yb
3+Ion is the simplest active ions of level structure, and electronic configuration is [Xe] 4f
13, two electronic states are only arranged, ground state
2F
7/2And excited state
2F
5/2, about 10000cm of being separated by
-1, higher excited state in the 5d configuration, with
2F
5/2At a distance of about 10000cm
-1, at ultraviolet band.This just makes Yb
3+Have and advantage such as do not have excited state absorption, supreme conversion, can realize high-dopant concentration, quantum yield height and fluorescence lifetime are long and as the active ions of high energy laser material.Have in the world all to have used on many high power laser systems and mix the Yb laserable material, as the Mercury (Yb:S-FAP) of the U.S., Polaris (Yb:Glass), the French Lucia (Yb:YAG) etc. of Germany.U.S. Mercury laser aid adopts the Yb:S-FAP crystal, and the Yb:S-FAP crystal technique of large-size high-quality just obtained breaking through in recent years, and it has influenced the progress of Mercury always.The Yb:S-FAP crystal of Mercury can grow into φ 120mm at present, and its laser output is at 60J/10Hz/l ω, and expectation can arrive 100J/10Hz/l ω very soon.Have only 2w/mk but Yb:S-FAP crystal thermal conductivity is too low, be unfavorable for system thermal management and repetition operation, fluorescence lifetime 1.14ms shows slightly less than normal.
In recent years, the crystal of fluoride of mixing Yb received people's very big concern.Compare with oxide compound, fluoride-based material all has very high transmitance from deep ultraviolet to infrared very wide scope; Its low specific refractory power has reduced its non-linear effect that produces when laser pumping; Low phonon energy has reduced the probability of the nonradiative transition of adjacent energy inter-stage, and has long fluorescence lifetime, thereby helps energy storage.Wherein best example is exactly CaF
2And LiYF
4Crystal of fluoride is with LiYF
4Belong to the LiLuF of tetragonal system structure together
4Crystal receives much concern recently, with Yb:CaF
2Crystal is compared Yb:LiLuF
4Not only have the fluorescence lifetime close (2.5ms), and have bigger emission cross section with it; With LiYF
4Compare LiLuF
4Crystal has lower phonon energy (440cm
-1), because Lu ion and Yb ion have close ionic radius and quality, not only can realize high-concentration dopant simultaneously, and the variation of crystalline thermal conductivity is very little before and after mixing, therefore study Yb:LiLuF
4Laser crystals is significant to the development high-energy laser.
At present to Yb:LiLuF
4Crystal technique all is the method for preparing crystal of fluoride of habitually practising, and no matter is to adopt crystal pulling method or descent method, the raw material that all needs to feed high-purity gas and adopt the spectroscopically pure level, even also will grow fluoridizing under the atmosphere.This just makes this crystal growth technique equipment bulky complex (large-scale vacuum crystal growing furnace and gas purifying equipment); The high request of raw material and gas purity has caused the crystal growth cost to improve greatly.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ytterbium doping lithium lutetium fluoride crystal, the characteristics of this method are under common air atmosphere, adopt the method for chemical reaction deoxidation to prepare ytterbium doping lithium lutetium fluoride crystal, it is easy to have technology, and equipment is simple, the low characteristics of growth cost.。
Technical solution of the present invention is as follows:
A kind of preparation method of ytterbium doping lithium lutetium fluoride crystal, its characteristics are that this method comprises the following steps:
1. select for use purity greater than 99.99% LiF, LuF
3And YbF
3, prepare burden by the proportioning of following equation in selected x value back,
LiF+xYbF
3+(1-x)LuF
3=Yb
x:LiLu
(1-x)F
4
X=0.1~35mol.% wherein forms the raw material of ytterbium doping lithium lutetium fluoride crystal after mixing;
2. described raw material, is added the 0.05-0.1g reductor and mixes after 4~6 hours through 200~300 ℃ of dehydrations, put into wall thickness and be the tight sealing behind the end crucible that has of 0.15~0.3mm;
3. described crucible is placed under the decline stove air atmosphere, temperature is 900~960 ℃ a high-temperature zone melt 4~6 hours, crucible descends with 0.5~1.2mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 25~40 ℃/cm, is cooled to room temperature with 20~40 ℃/h speed behind the growth ending.
Described reductor is carbon dust, rubber or CF
4
The technique effect of the technology of the present invention
First successfully under air atmosphere, adopt chemical deoxy technology in the world, utilize Bridgman-Stockbarge method for growing to go out diameter greater than 40mm, length high-quality Yb:LiLuF greater than 100mm
4Crystal.The characteristics of the present invention and conventional growth method are:
(1) condition of needing no vacuum, logical any atmosphere and pressurization;
(2) need not the bulky complex growth apparatus;
(3) technology is easy, and equipment is simple, the growth cost is low.
Description of drawings
The furnace construction synoptic diagram that Fig. 1 the inventive method adopts
Among the figure: the 1-pulling apparatus, 2-aluminum oxide insulation cover, the 3-alumina tube, the 4-high-temperature zone, 5-platinum bar, 6-heats thermal source, the 7-platinum crucible, the 8-melt, the 9-temperature-control heat couple, 10-monitors thermopair, 11-cold zone, 12-crystal.
Fig. 2 is the room temperature absorption spectrum of the invention process example 2 growing crystals
Fig. 3 is the room temperature fluorescence spectrum of the invention process example 2 growing crystals
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
The stove that the inventive method adopts drives the variable gear group with motor and realizes regulating constant rate of speed decline, and the stove high-temperature zone adopts four silication carbon-points as heating member, and cold zone does not have heating unit.Temperature regulating device adopts platinum-rhodium thermocouple, and the inner lining material of stove is an alumina bubble brick, and concrete structure as shown in Figure 1.The furnace construction synoptic diagram that Fig. 1 the inventive method adopts is among the figure: 1-pulling apparatus, 2-aluminum oxide insulation cover, 3-alumina tube, 4-high-temperature zone, 5-platinum bar, 6-heats thermal source, 7-platinum crucible, 8-melt, the 9-temperature-control heat couple, 10-monitors thermopair, 11-cold zone, 12-crystal.Growing crystal adopts platinum as crucible material, be processed into end crucible according to the required size and dimension of crystal, the crucible height generally exceeds about 1/4th than powder height, and wall thickness is 0.15-0.3mm, the volume that depends on crystal growth, crucible are disposable use.
The preparation method of ytterbium doping lithium lutetium fluoride crystal of the present invention comprises the following steps:
1. select for use purity greater than 99.99% LiF, LuF
3And YbF
3, prepare burden by the proportioning of following equation in selected x value back,
LiF+xYbF
3+(1-x)LuF
3=Yb
x:LiLu
(1-x)F
4
X=0.1~35mol.% wherein forms the raw material of ytterbium doping lithium lutetium fluoride crystal after mixing;
2. described raw material, is added the 0.05-0.1g reductor and mixes after 4~6 hours through 200~300 ℃ of dehydrations, put into wall thickness and be the tight sealing behind the end crucible that has of 0.15~0.3mm;
3. described crucible being placed decline stove temperature is 900~960 ℃ high-temperature zone melt 4~6 hours, crucible descends with 0.5~1.2mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 25~40 ℃/cm, is cooled to room temperature with 20~40 ℃/h speed behind the growth ending.Described reductor is carbon dust, rubber or CF
4
Be specific embodiment below:
Embodiment 1:LiYb
0.001Lu
0.999F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.001Lu
0.999F
4Through 200 ℃ of 6 hours dewatered dryings, add the 0.05g carbon dust and mix as reductor after the batch mixes, adding is of a size of in φ 30 * 150 point end platinum crucibles, and crucible is sealed.Described crucible placed described crucible is placed decline stove temperature is 900 ℃ high-temperature zone melt 5 hours, crucible descends with 1.2mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 25 ℃/cm, is cooled to room temperature with 20 ℃/h speed behind the growth ending.
Embodiment 2:LiYb
0.05Lu
0.95F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.05Lu
0.95F
4Batch mixes is after 250 ℃ of 5 hours dewatered dryings, and adds 0.05g rubber and mix as reductor, puts into and is of a size of φ 40 * 40 * 180 flat platinum crucibles, crucible wall thickness 0.2mm.Put into pure LiLuF
4Crystal seals crucible as seed crystal.Described crucible placed described crucible is placed decline stove temperature is 920 ℃ high-temperature zone melt 6 hours, crucible descends with 0.8mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 30 ℃/cm, is cooled to room temperature with 30 ℃/h speed behind the growth ending.Crystal take out the back along a to being processed into 10 * 10 * 1mm
3Sample carry out spectrum test, absorption spectrum as shown in Figure 2, fluorescence spectrum is as shown in Figure 3.
Embodiment 3:LiYb
0.1Lu
0.9F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.1Lu
0.9F
4Batch mixes is after 300 ℃ of 4 hours dewatered dryings, and adds 0.05g CF
4Mix as reductor, put into and be of a size of φ 30 * 180 point end platinum crucibles, put into pure LiLuF
4Crystal seals crucible as seed crystal.Described crucible placed described crucible is placed decline stove temperature is 960 ℃ high-temperature zone melt 4 hours, crucible descends with 1mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 30 ℃/cm, is cooled to room temperature with 25 ℃/h speed behind the growth ending.
Embodiment 4:LiYb
0.2Lu
0.8F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.2Lu
0.8F
4Batch mixes is after 250 ℃ of 6 hours dewatered dryings, and adds the 0.1g carbon dust and mix as reductor, puts into and is of a size of φ 40 * 40 * 220 flat platinum crucibles, crucible wall thickness 0.25mm, pure LiLuF
4Crystal seals crucible as seed crystal.Described crucible placed described crucible is placed decline stove temperature is 940 ℃ high-temperature zone melt 5 hours, crucible descends with 0.5mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 40 ℃/cm, is cooled to room temperature with 35 ℃/h speed behind the growth ending.
Embodiment 5:LiYb
0.3Lu
0.7F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.3Lu
0.7F
4Batch mixes is after 200 ℃ of 5 hours dewatered dryings, and adds 0.1g rubber and mix as reductor, puts into and is of a size of φ 40 * 220 point end platinum crucibles, and crucible is sealed.Described crucible placed described crucible is placed decline stove temperature is 950 ℃ high-temperature zone melt 4 hours, crucible descends with 0.7mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 40 ℃/cm, is cooled to room temperature with 40 ℃/h speed behind the growth ending.
Embodiment 6:LiYb
0.35Lu
0.65F
4Crystal growth
With YbF
3, LiF and LuF
3Press the crystalline structural formula LiYb of present embodiment
0.35Lu
0.65F
4Batch mixes is after 200 ℃ of 5 hours dewatered dryings, and adds 0.1g CF
4Mix as reductor, put into and be of a size of φ 30 * 150 point end platinum crucibles, crucible is sealed.Described crucible placed described crucible is placed decline stove temperature is 960 ℃ high-temperature zone melt 4 hours, crucible descends with 1mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 30 ℃/cm, is cooled to room temperature with 25 ℃/h speed behind the growth ending.
The foregoing description after tested, its absorption spectrum and fluorescence spectrum all have embodiment 2 similar results.It is easy that experiment shows that the present invention has technology, and equipment is simple, the low characteristics of growth cost.
Claims (2)
1. the preparation method of a ytterbium doping lithium lutetium fluoride crystal is characterized in that this method comprises the following steps:
1. select for use purity greater than 99.99% LiF, LuF
3And YbF
3, prepare burden by the proportioning of following equation in selected x value back,
LiF+xYbF
3+(1-x)LuF
3=Yb
x:LiLu
(1-x)F
4
X=0.1~35mol.% wherein forms the raw material of ytterbium doping lithium lutetium fluoride crystal after mixing;
2. described raw material, is added the 0.05-0.1g reductor and mixes after 4~6 hours through 200~300 ℃ of dehydrations, put into wall thickness and be the tight sealing behind the end crucible that has of 0.15~0.3mm;
3. described crucible is placed under the decline stove air atmosphere, temperature is 900~960 ℃ a high-temperature zone melt 4~6 hours, crucible descends with 0.5~1.2mm/h speed then, this moment, crystal solid-liquid interface place ± the interior thermograde of 0.5cm scope was 25~40 ℃/cm, is cooled to room temperature with 20~40 ℃/h speed behind the growth ending.
2. the preparation method of ytterbium doping lithium lutetium fluoride crystal according to claim 1 is characterized in that: described reductor is carbon dust, rubber or CF
4
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103194796A (en) * | 2013-03-22 | 2013-07-10 | 中国科学院上海光学精密机械研究所 | Infrared laser crystal in Ho-Pr codoping lutecium lithium fluoride, and preparation method thereof |
CN103774222A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Eu<3+>/Dy<3+>-doped NaYF4 monocrystal for white light LEDs (light-emitting diodes) and preparation method thereof |
CN103774211A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Terbium/ytterbium rare earth ion codoped lithium gadolinium lutetium fluoride upconversion luminescent crystal and preparation method thereof |
CN103820855A (en) * | 2014-02-20 | 2014-05-28 | 宁波大学 | Tb<3+>/Sm<3+> doped LiLuF4 monocrystal used for white light LED, and preparation method thereof |
CN104975345A (en) * | 2014-04-04 | 2015-10-14 | 上海硅酸盐研究所中试基地 | Method for growing cerium fluoride crystal by non-vacuum descent process |
-
2011
- 2011-06-08 CN CN201110151751XA patent/CN102230218A/en active Pending
Non-Patent Citations (2)
Title |
---|
A.S.YASYUKEVICH ET AL: "SPECTRAL KINETIC PROPERTIES OF Yb3+:Na4Y6F22 and Yb3+:LiLuF4 CRYSTALS", 《JOURNAL OF APPLIED SPECTROSCOPY》 * |
JIGANG YIN ET AL: "Crystal growth and spectroscopic characterization of Yb-doped and Yb, Na-codoped PbF2 laser crystals", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103194796A (en) * | 2013-03-22 | 2013-07-10 | 中国科学院上海光学精密机械研究所 | Infrared laser crystal in Ho-Pr codoping lutecium lithium fluoride, and preparation method thereof |
CN103774222A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Eu<3+>/Dy<3+>-doped NaYF4 monocrystal for white light LEDs (light-emitting diodes) and preparation method thereof |
CN103774211A (en) * | 2014-02-20 | 2014-05-07 | 宁波大学 | Terbium/ytterbium rare earth ion codoped lithium gadolinium lutetium fluoride upconversion luminescent crystal and preparation method thereof |
CN103820855A (en) * | 2014-02-20 | 2014-05-28 | 宁波大学 | Tb<3+>/Sm<3+> doped LiLuF4 monocrystal used for white light LED, and preparation method thereof |
CN103774222B (en) * | 2014-02-20 | 2016-06-08 | 宁波大学 | A kind of Eu for white light LEDs3+/Dy3+Doping NaYF4Monocrystal and preparation method thereof |
CN103820855B (en) * | 2014-02-20 | 2016-11-16 | 宁波大学 | A kind of Tb for white light LEDs3+/ Sm3+doping LiLuF4monocrystal and preparation method thereof |
CN104975345A (en) * | 2014-04-04 | 2015-10-14 | 上海硅酸盐研究所中试基地 | Method for growing cerium fluoride crystal by non-vacuum descent process |
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