CN105332056A - Divalent metal cation and cerium co-doped lutetium aluminum garnet crystal for laser illumination and preparation method thereof - Google Patents
Divalent metal cation and cerium co-doped lutetium aluminum garnet crystal for laser illumination and preparation method thereof Download PDFInfo
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- CN105332056A CN105332056A CN201510773767.2A CN201510773767A CN105332056A CN 105332056 A CN105332056 A CN 105332056A CN 201510773767 A CN201510773767 A CN 201510773767A CN 105332056 A CN105332056 A CN 105332056A
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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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
Abstract
The invention discloses a divalent metal cation and cerium co-doped lutetium aluminum garnet crystal for laser illumination and a preparation method thereof. The chemical formula of the crystal is M3xCe3yLu3(1-x-y) Al5O12. The growing technology of the crystal includes the following steps that growth is performed through a medium-frequency induction heating pulling method, a heating body is an iridium crucible, raw materials are pressed by an isostatic press into blocks after being weighed, mixed and evenly ground, and sintering is performed at the high temperature of 1300 DEG C so that a solid phase reaction can occur; zirconia and alumina are used for preparing a heat-preserving cover, inert gas is adopted in a hearth in the growing process for protection, the growth temperature of the crystal is about 1970 DEG C, the pulling speed is 0.1-5 mm/h, and the rotating speed of the crystal is 5-30 rpm. The scintillation crystal has the outstanding advantages that high-concentration doping can be easily achieved and the crystal light yield is high, and the made crystal can serve as a core material of a laser illumination system.
Description
Technical field
The present invention relates to scintillation crystal, particularly laser illuminator a kind of divalent cation and cerium ion mixes LuAG (M altogether
3xce
3ylu
3 (1-x-y)al
5o
12) high temperature scintillation crystal and preparation method thereof.
Background technology
Inorganic scintillation crystal is a kind of crystalline state energy transfer medium that the energy transformation of high-energy photon or particle can be become be easy to ultraviolet/visible light detected.The detector that scintillation crystal is made is widely used in the fields such as high energy physics, nuclear physics, nuclear medical imaging diagnosis (XCT, PET etc.), geological prospecting, astronomical Space Physics and safety random check.Along with the develop rapidly of nuclear detection and correlation technique, its Application Areas is still in continuous expansion.Different application field proposes more and more higher requirement to scintillation crystal, and traditional scintillation crystal detectors such as NaI (Tl), BGO, PWO cannot meet the requirement of high-performance scintillation detector.
The development trend of current scintillation crystal is centered by the performances such as height output, fast-response, high-density, the exploratory development of novel scintillation crystal is carried out by following several channel, improve and improve crystal property: 1) by the codoped of different ions, improve the deficiency of existing scintillation crystal, improve its scintillation properties, as photoyield etc.; 2) by optimizing crystal growth formula, technique and Study on Engineering Technology etc., crystal growth cost and growth difficulty is reduced; 3) by crystalline mi defect, mutual relationship between codoped and Scintillation Properties, reduce and suppress harmful point defect, reducing radiationless transition in scitillation process to the loss of energy transformation.Cerium ion-doped silicate and aluminate are the two type high temp inorganic scintillators paid close attention to very in the industry in recent years.
Cerium ion-doped high temperature inorganic scintillation crystal belongs to extrinsic scintillator, the Ce of doping
3+ion is as the luminescence center of crystal, and its luminescence mechanism is made up of following 3 processes: a) first scintillation crystal absorbs energetic ray or particle, thus in lattice, produce a large amount of electron-hole pairs; B) relaxation is carried out to by the interaction between Electron Electron, Electron-phonon in a large amount of high-energy electron holes, and finally become the thermalized electron hole pair with energy gap energy, the electron-hole pair of thermalization transfers energy to Ce again
3+luminescence center; C) Ce
3+ion is by the transition luminescence of 5d-4f.Research shows, the oxide crystal that major part grows is owing to growing under an inert atmosphere, because anoxic can produce Lacking oxygen point defect, Lacking oxygen defect produces material impact to the optical property of oxide crystal, in the interaction process of photon and crystal, Lacking oxygen becomes electron trap or causes excitation energy loss by additional channel, thus the radiationless transition produced is the major cause { JournalofAppliedPhysics99 suppressing crystallo-luminescence efficiency, 113518 (2006) }, therefore the oxide crystal grown under most of oxygen-free environment, for improving its performance, all need later stage aerobic anneal.
The high-temperature oxide scintillation crystal of Ce ion doping as: Ce:YAG, Ce:LSO, Ce:GSO, Ce:YAP, Ce:LuAP etc. be come across the end of the eighties in last century-a collection of novel scintillator crystal materials at the beginning of the nineties.With traditional NaI:Tl, BGO, BaF
2the low melting points such as PWO (being no more than 1500 DEG C) inorganic scintillation crystal is compared, the high-temp oxide crystal of Ce ion doping is with High Light Output (being about the 2-10 of BGO crystal doubly) and fast decay (being about the 1/5-1/20 of BGO crystal) characteristic, therefore, the scintillation crystal of this kind of excellent property causes the great attention of scientific circles.Silicic acid lutetium (LSO) crystal of Ce ion doping and yttrium luetcium silicate (LYSO) crystal receive much concern because of the important application in computer tomography (CT scanner) system in medical science PET (positron emission tomography) machine and industrial sector.US4958080 describes the Lu of cerium dopping
2siO
5crystal preparation, patent US6624420 describes Ce
2x(Lu
1-yy
y)
2 (1-x)siO
5crystal preparation, patent US6437336 relates to Lu
2 (1-x)m
2xsi
2o
7prepared by crystalloid, wherein M is Ce elements at least partly.This kind of scintillator all jointly has the high stopping power to energy-rich radiation, causes the strong light emission of quickly light pulse.
Yttrium aluminum garnet (Y
3al
5o
12or YAG) monocrystalline is excellent laser host material and optical window material.1992, Ce:YAG is suggested and causes people's broad interest as scintillation material, the people such as Moszynski and Ludziejewski have carried out comparatively systematic research respectively at 1994 and the scintillation properties to Ce:YAG crystal in 1997, and point out that Ce:YAG crystal has excellent scintillation properties.Ce:YAG crystal has fast decay (78ns) and at 550nm band emission fluorescence, can well be coupled with silicon photo diode, the field such as low-yield gamma-rays, alpha-particle detection during it can be applied to, at present, the commercialization of Ce:YAG high temperature scintillation crystal, is mainly used in the display unit of scanning electron microscope (SEM).
As everyone knows, the most proven technique realizing white light LEDs is on blue light wafer, smear the yellow Ce:YAG fluorescent material of one deck, make blue light become white light with yellow light mix, but its colour rendering index is relatively low.At present, scientist is putting forth effort the illumination utilizing semiconductor laser of research.There is " light efficiency decline " problem, high brightness in blue led, more difficultly raises the efficiency.And there is not this problem in laser apparatus, " compared with LED illumination, laser illuminator can realize very high efficiency ".Therefore Shuji Nakamura is estimated, laser illuminator replaces LED illumination in the future.In laser illuminator, the YAG monocrystalline of Ce ion doping is the best materials that current known auxiliary blue light laser diode realizes luminance brightness white light.
There is following shortcoming as scintillation crystal in Ce:YAG: 1) due to Ce
3+(R
ce=1.03nm) ion enters the less Y of substitution ion radius after YAG lattice
3+(R
y=0.89nm), because ionic radius difference is larger, Ce ion segregation coefficient in YAG lattice very little (~ 0.1), cause the skewness of Ce ion in crystal on the one hand, make Ce:YAG crystal be difficult to realize high-concentration dopant simultaneously, on the other hand because ionic radius difference is comparatively large, cause crystalline structure stress comparatively large, crystal easily ftractures; 2) less (the about 4.55g/cm of Ce:YAG crystalline density
3) cause cut-off energy during its detection energetic ray less, there is certain limitation when high-energy gamma X-ray detection X; 3) because crystal grows under an inert atmosphere, can because anoxic produce Lacking oxygen, Lacking oxygen becomes electron trap or causes excitation energy loss by additional channel, thus reduces the photoyield of crystal.
Summary of the invention
In order to solve the deficiency of above-mentioned Ce:YAG scintillation crystal, the object of the present invention is to provide a kind of M being mainly used in laser illuminator
3xce
3ylu
3 (1-x-y)al
5o
12high temperature scintillation crystal and preparation method thereof, the Lu ion that in this crystal, Ce ionic replacement ionic radius is larger, thus greater concn Ce can be realized
3+ion doping, and there is higher density and flicker cut-off energy; In addition, because Lacking oxygen is+divalent, divalent cation (Ca is mixed
2+, Mg
2+, Ba
2+deng), by charge compensation, on the basis of oxygen atmosphere annealing, oxygen vacancy concentration can be reduced further, thus improve the equation of light volume of crystal further, prepare the high-density crystalline material that scintillation properties is more excellent.
Technical solution of the present invention is as follows:
Be mainly used in a high temperature scintillation crystal for laser illuminator, feature is that the LuAG crystal that this divalent cation and cerium ion are mixed altogether adopts melt method for growing, and its chemical formula is:
M
3xCe
3yLu
3(1-x-y)Al
5O
12
In formula, x=0.0001 ~ 0.001, y=0.01 ~ 0.08, wherein M is divalent metal (Ca
2+, Mg
2+, Ba
2+deng), x is the doping of M ion, and y is the doping of Ce ion, and Ce ion enters LuAG crystal and replaces Lu ion site.
Divalent cation and cerium ion mix a preparation method for LuAG scintillation crystal altogether, and the method comprises the following steps:
1. composition of raw materials:
M
3xce
3ylu
3 (1-x-y)al
5o
12crystal adopts MO (4N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) as initial feed, and 6x:6y:3 (1-x-y) in molar ratio: 5 prepare burden, and wherein the span of x, y is respectively x=0.0001 ~ 0.001, y=0.01 ~ 0.08;
2. melt method for growing M is adopted
3xce
3ylu
3 (1-x-y)al
5o
12scintillation crystal:
First by predrying in atmosphere for each high pure oxide powder, removing planar water, drying material temperature degree is 1000 DEG C.Weigh MO (4N), CeO in molar ratio
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material (N represents the purity of raw material), raw material is after fully mixing, the block material of required specification and size is pressed into isostatic pressing machine, then load in alumina crucible, put in retort furnace and sinter, within 10 hours, from room temperature to 1300 DEG C, constant temperature was cooled to room temperature through 10 hours after 10 hours, the block material sintered is taken out encapsulation, puts into loft drier for subsequent use.
Described melting method is crystal pulling method, and described crucible is Iridium Crucible, and seed crystal is the pure LuAG single crystal rod in <111> or <100> direction, and crystal growth is in high-purity Ar or high-purity N
2carry out in atmosphere.Pull rate is 0.1 ~ 5mm/h, and speed of rotation is 5 ~ 30rpm.
Described melting method is falling crucible method, and described crucible material adopts high purity graphite, and crucible bottom can not put seed crystal, or puts into the pure LuAG seed crystal described in above-mentioned crystal pulling method, and crystal growth is in high-purity Ar or high-purity N
2carry out in atmosphere.Crucible fall off rate is 0.1 ~ 1.5mm/h.
Described melting method is temperature gradient method, and crucible material adopts high purity graphite, and crucible bottom can not put seed crystal, or puts into the pure LuAG seed crystal described in above-mentioned crystal pulling method, and crystal growth is in high-purity Ar or high-purity N
2carry out in atmosphere.Crystal is made to carry out segmentation cooling growing crystal with the rate of temperature fall that growth velocity is 1 ~ 50 DEG C/h.
Technique effect of the present invention:
High-quality M is grown with above raw material and technique
3xce
3ylu
3 (1-x-y)al
5o
12crystal, crystal is yellow, and outward appearance is good, has excellent optics and physical and chemical performance.Main glow peak is positioned at about 530nm, and fall time is about 75ns, Ce
3+concentration 1at% ~ 6at%, under high-energy ray irradiation, photon yield can reach 9000 ~ 20000Ph/MeV.
M
3xce
3ylu
3 (1-x-y)al
5o
12crystal can with the detection equipment efficient coupling such as silicon photo diode, can be applicable to the fields such as high energy physics, nuclear physics, nuclear medical imaging diagnosis (XCT, PET), geological prospecting, astronomical Space Physics and safety random check.
Embodiment
Below by concrete enforcement, the invention will be further described, but should not limit the scope of the invention with this.
Embodiment 1: Czochralski grown Ca ion doping concentration is 0.05at%, Ce
3+doping content is the Ca of 1.0at%
0.0015ce
0.03lu
2.9685al
5o
12scintillation crystal.
First that each high pure oxide powder is suitable predrying in atmosphere, removing planar water, calcination 10h at 1000 DEG C, then by Ca (5N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material carries out weigh batching according to mol ratio.Mix rear isostatic pressing machine briquetting, be put in iridium crucible, adopt Czochralski grown crystal, seed crystal is the pure YAG single crystal rod in <111> direction, and crystal growth is in high-purity Ar or high-purity N
2carry out in atmosphere.The pull rate of crystal is 0.5 ~ 1mm/h, rotating speed is 18rpm, control the growth of crystal Raised key axis, all crystals growth is all through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials → roasting crystal seed → sow → necking down → shouldering → isodiametric growth → put forward the processes such as de-and cooling.Whole growth cycle about 7 days.Grow the yellow Ca:Ce:LuAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 2: Czochralski grown Ca ion doping concentration is 0.05at%, Ce
3+doping content is the Ca of 2.0at%
0.0015ce
0.06lu
2.9385al
5o
12scintillation crystal.
First that each high pure oxide powder is suitable predrying in atmosphere, removing planar water, calcination 10h at 1000 DEG C, then by Ca (5N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material carries out weigh batching according to mol ratio.Mix rear isostatic pressing machine briquetting, be put in iridium crucible, adopt Czochralski grown crystal, seed crystal is the pure YAG single crystal rod in <111> direction, and crystal growth is in high-purity Ar or high-purity N
2carry out in atmosphere.The pull rate of crystal is 0.5 ~ 1mm/h, rotating speed is 18rpm, control the growth of crystal Raised key axis, all crystals growth is all through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials → roasting crystal seed → sow → necking down → shouldering → isodiametric growth → put forward the processes such as de-and cooling.Whole growth cycle about 7 days.Grow the yellow Ca:Ce:LuAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 3: Czochralski grown Ca ion doping concentration is 0.05at%, Ce
3+doping content is the Ca of 3.0at%
0.0015ce
0.09lu
2.9085al
5o
12scintillation crystal.
First that each high pure oxide powder is suitable predrying in atmosphere, removing planar water, calcination 10h at 1000 DEG C, then by Ca (5N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material carries out weigh batching according to mol ratio.Mix rear isostatic pressing machine briquetting, be put in iridium crucible, adopt Czochralski grown crystal, seed crystal is the pure YAG single crystal rod in <111> direction, and crystal growth is at high-purity Ar or N
2carry out in atmosphere.The pull rate of crystal is 0.5 ~ 1mm/h, rotating speed is 18rpm, control the growth of crystal Raised key axis, all crystals growth is all through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials → roasting crystal seed → sow → necking down → shouldering → isodiametric growth → put forward the processes such as de-and cooling, whole growth cycle about 7 days.Grow the faint yellow Ca:Ce:LuAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 4: Czochralski grown Ca ion doping concentration is 0.05at%, Ce
3+doping content is the Ca of 3.0at%
0.0015ce
0.12lu
2.8785al
5o
12scintillation crystal.
First that each high pure oxide powder is suitable predrying in atmosphere, removing planar water, calcination 10h at 1000 DEG C, then by Ca (5N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material carries out weigh batching according to mol ratio.Mix rear isostatic pressing machine briquetting, be put in iridium crucible, adopt Czochralski grown crystal, seed crystal is the pure YAG single crystal rod in <111> direction, and crystal growth is at high-purity Ar or N
2carry out in atmosphere.The pull rate of crystal is 0.5 ~ 1mm/h, rotating speed is 18rpm, control the growth of crystal Raised key axis, all crystals growth is all through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials → roasting crystal seed → sow → necking down → shouldering → isodiametric growth → put forward the processes such as de-and cooling, whole growth cycle about 7 days.Grow the faint yellow Ca:Ce:LuAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 5: Czochralski grown Ca ion doping concentration is 0.05at%, Ce
3+doping content is the Ca of 6.0at%
0.0015ce
0.18lu
2.8185al
5o
12scintillation crystal.
First that each high pure oxide powder is suitable predrying in atmosphere, removing planar water, calcination 10h at 1000 DEG C, then by Ca (5N), CeO
2(5N), Lu
2o
3(about 5N) and Al
2o
3(5N) raw material carries out weigh batching according to mol ratio.Mix rear isostatic pressing machine briquetting, be put in iridium crucible, adopt Czochralski grown crystal, seed crystal is the pure YAG single crystal rod in <111> direction, and crystal growth is at high-purity Ar or N
2carry out in atmosphere.The pull rate of crystal is 0.3 ~ 1mm/h, rotating speed is 18rpm, control the growth of crystal Raised key axis, all crystals growth is all through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials → roasting crystal seed → sow → necking down → shouldering → isodiametric growth → put forward the processes such as de-and cooling, whole growth cycle about 7 days.Grow the faint yellow Ca:Ce:LuAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Claims (3)
1. laser illuminator divalent metal and cerium mix a lutetium aluminum carbuncle crystal altogether, it is characterized in that: molecular formula M
3xce
3ylu
3 (1-x-y)al
5o
12, x=0.0001 ~ 0.001 in formula, y=0.01 ~ 0.08, wherein M is divalent metal (Ca
2+, Mg
2+, Ba
2+deng), x is the doping of M ion, and y is the doping of Ce ion, and Ce ion enters LuAG crystal and replaces Lu ion site.
2. laser illuminator divalent metal and cerium mix a preparation method for lutetium aluminum carbuncle crystal altogether, it is characterized in that processing step is as follows:
(1) Frequency Induction Heating Czochralski grown M is adopted
3xce
3ylu
3 (1-x-y)al
5o
12crystal, heating element is Iridium Crucible, and raw material weighs in following formula ratio after roasting:
6xMO+6yCeO
2+3(1-x-y)Lu
2O
3+5Al
2O
3=2M
3xCe
3yLu
3(1-x-y)Al
5O
12+3(y-x)/2O
2↑
Wherein M is divalent metal (Ca
2+, Mg
2+, Ba
2+deng), x is the concentration of M ion of adulterating in melt, and y is the concentration of doped Ce ion in melt, and in crystal, the doping content of Ce ion is then the product of y and segregation coefficient;
(2) raw material is through claiming to join, and grinds the even rear packaging that is mixed, and be pressed into cylindric with isostatic pressed and under the high temperature of 1300 DEG C, sinter generation solid state reaction, packaged being placed in loft drier of the raw material sintered saves backup;
(3) lagging material is done with zirconium white and aluminum oxide respectively, by sapphire sheet as view port, growing crystal under protection of inert gas, growth temperature about 1970 DEG C, pull rate 0.1 ~ 5mm/h, crystal rotation 5 ~ 30rpm, growth M
3xce
3ylu
3 (1-x-y)al
5o
12crystal.
3. laser illuminator divalent metal according to claim 2 and cerium mix the preparation method of lutetium aluminum carbuncle crystal altogether, it is characterized in that, raw materials used purity is: MO>=99.99%, CeO
2:>=99.999%, Lu
2o
3:>=99.995%, Al
2o
3:>=99.999%.
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CN107502354A (en) * | 2017-10-11 | 2017-12-22 | 哈尔滨工业大学 | A kind of warm white LED fluorescent material and preparation method thereof |
CN107502354B (en) * | 2017-10-11 | 2020-11-06 | 哈尔滨工业大学 | Fluorescent powder for warm white LED and preparation method thereof |
CN108441960A (en) * | 2018-04-18 | 2018-08-24 | 苏州四海常晶光电材料有限公司 | Divalent metal is co-doped with lutetium aluminum carbuncle crystal preparation method with cerium |
CN108893779A (en) * | 2018-07-16 | 2018-11-27 | 苏州四海常晶光电材料有限公司 | A kind of calcium ions and magnesium ions and cerium co-doped yttrium aluminium garnet scintillation crystal and preparation method thereof |
CN111995397A (en) * | 2020-08-14 | 2020-11-27 | 中国科学院宁波材料技术与工程研究所 | Fluorescent ceramic and preparation method and application thereof |
CN112851124A (en) * | 2021-02-04 | 2021-05-28 | 中国科学院福建物质结构研究所 | Glass ceramic membrane composite material for laser illumination |
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