CN108441959A - Mix Cerium aluminate gadolinium lutetium garnet crystal preparation method - Google Patents
Mix Cerium aluminate gadolinium lutetium garnet crystal preparation method Download PDFInfo
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- CN108441959A CN108441959A CN201810347605.6A CN201810347605A CN108441959A CN 108441959 A CN108441959 A CN 108441959A CN 201810347605 A CN201810347605 A CN 201810347605A CN 108441959 A CN108441959 A CN 108441959A
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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
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Abstract
The invention discloses one kind mixing Cerium aluminate gadolinium lutetium garnet crystal and preparation method thereof, and chemical formula is：Ce3xLu3(1‑x‑y)Gd3yAl5O12Growth processing step is as follows：Using the Frequency Induction Heating Czochralski grown crystal, heater is Iridium Crucible, is weighed in proportion after raw material is fired：Raw material is matched through claiming, grind be mixed it is even after through isostatic pressing machine briquet, at a high temperature of 1300 DEG C sintering solid phase reaction occurs, the raw material sintered is placed in drying box and preserves；Insulation cover and thermal insulation material are done with zirconium oxide and aluminium oxide respectively, observation panel is sealed with jewel piece, inert gas shielding, about 1950 DEG C of crystal growth temperature, 0.1~5mm/h of pull rate, 5~30rpm of crystal rotation is used inside growth course burner hearth.The present invention has many advantages, such as that crystal growth is at low cost, it is outstanding to be easy preparation large scale, high-concentration dopant easy to implement and scintillation properties.
Description
Technical field
The present invention relates to scintillation crystal, especially one kind mixing Cerium aluminate gadolinium lutetium Ce3xLu3(1-x-y)Gd3yAl5O12High temperature flickers
Crystal and preparation method thereof.
Background technology
Inorganic scintillation crystal be it is a kind of can be by high-energy photon (X/ gamma-rays) or the energy of particle (electronics, proton, neutron etc.)
Amount is converted into being easy to the crystalline state energy transfer medium of ultraviolet/visible light of detection.The detector extensive use that scintillation crystal is made
It is checked in high-energy physics, nuclear physics, nuclear medical imaging diagnosis (XCT, PET etc.), geological prospecting, astronomical Space Physics and safety
Look into equal fields.With nuclear detection and the rapid development of the relevant technologies, application field is still constantly being expanded.Different application field pair
Scintillation crystal proposes increasingly higher demands, and the scintillation crystals such as traditional NaI (Tl), BGO, PWO can no longer meet high property
The requirement of energy scintillation detector.
The development trend of scintillation crystal is centered on the performances such as height output, fast-response, high density, by following at present
Several channels carry out the exploratory development of novel scintillation crystal, improve and improve crystal property：1) by the codope of different ions,
The deficiency for improving existing scintillation crystal improves its scintillation properties, such as photoyield；2) by optimizing crystal growth formula, technique
And Study on Engineering Technology, reduce crystal growth cost and growth difficulty；3) it is dodged by crystalline mi defect, codope and crystal
Correlation between bright performance reduces and inhibits to be harmful to point defect, and the radiationless transition reduced in scitillation process turns energy
The loss changed.Cerium ion-doped silicate and aluminate is two type high temp inorganic scintillators being concerned in recent years.
Cerium ion-doped high temperature inorganic scintillation crystal belongs to extrinsic scintillator, the Ce of doping3+Ion is as crystal
The centre of luminescence, luminescence mechanism are made of following 3 processes：A) scintillation crystal absorbs high-energy ray or particle first, thus
A large amount of electron hole pair is generated in lattice；B) a large amount of high-energy electron hole to by Electron Electron, Electron-phonon it
Between interaction carry out relaxation, eventually become the thermalized electron hole pair with energy gap energy, the electron hole of thermalization
To transferring energy to Ce again3+The centre of luminescence；c)Ce3+The transition luminescence that ion passes through 5d-4f.
The high-temperature oxide scintillation crystal of Ce ion dopings is such as：Ce:YAG、Ce:LSO、Ce:GSO、Ce:YAP、Ce:LuAP
Etc. being a collection of novel inorganic scintillator crystal materials for coming across the beginning of the nineties at the end of the eighties in last century-.With traditional NaI:Tl, BGO,
BaF2, the low melting points such as PWO (be no more than 1500 DEG C) inorganic scintillation crystal compares, and the high-temp oxide crystal of Ce ion dopings has both
There are High Light Output (about 2-10 times of BGO crystal) and fast decaying (the about 1/5-1/20 of BGO crystal) characteristic, it is therefore, this kind of
The scintillation crystal of function admirable causes the great attention of scientific circles.The silicic acid lutetium (LSO) and yttrium luetcium silicate crystal of Ce ion dopings
(LYSO) because of the computer tomography (CT scan in medicine PET (positron emission tomography) machine and industrial department
Instrument) important application in system and be concerned.US4 958 080 describes the Lu of cerium dopping2SiO5Prepared by crystal, patent US6
624 420 describe Ce2x(Lu1-yYy)2(1-x)SiO5Prepared by crystal, patent US6 437 336 is related to Lu2(1-x)M2xSi2O7Class is brilliant
Prepared by body, wherein M is at least partly Ce elements.This kind of scintillator all jointly has the high stopping power to energy-rich radiation,
Cause the strong light emission of very fast light pulse.
Yttrium-aluminium-garnet (Y3Al5O12Or YAG) monocrystalline is excellent laser host material and optical window material.1992
Year, Ce:YAG is suggested as scintillation material and causes people's broad interest, and Moszynski and Ludziejewski et al. are respectively
In 1994 and 1997 to Ce:The scintillation properties of YAG crystal have carried out more systematic research, and point out Ce:YAG crystal has
There are excellent scintillation properties.Ce:YAG crystal has fast decaying (78ns) and emits fluorescence in 550nm wave bands, with two pole of silicon light
Pipe can couple well so that it can be applied to the fields such as middle low energy gamma-rays, alpha-particle detection, currently, Ce:YAG high temperature
Scintillation crystal has been commercialized, and is mainly used for the display unit of scanning electron microscope (SEM).
Currently, Ce:YAG crystal is primarily present following two disadvantages：1) due to Ce3+(RCe=1.03nm) ion enters YAG
The smaller Y of substitution ion radius after lattice3+(RY=0.89nm), since ionic radius difference is larger, Ce ions are in YAG lattices
Segregation coefficient very little (~0.1) on the one hand leads to Ce ions being unevenly distributed in crystal, while making Ce:YAG crystal is difficult to
Realize that high-concentration dopant causes crystal structure stress larger, crystal is easy out on the other hand since ionic radius difference is huge
It splits；2)Ce:Smaller (the about 4.55g/cm of YAG crystalline densities3) cause cut-off energy when its detection high-energy ray smaller, in high energy
There is certain limitation when measuring gamma-ray detection.
Invention content
In order to solve above-mentioned Ce:The deficiency of YAG scintillation crystals, the purpose of the present invention is to provide one kind being used for high-energy ray
The Ce of detection3xLu3(1-x-y)Gd3yAl5O12High temperature scintillation crystal and preparation method thereof, the crystal can realize higher concentration Ce3+From
Son doping, and be a kind of high temperature scintillator crystal materials haveing excellent performance with higher density and flicker cut-off energy.While by
In Gd as main matrix element instead of matrix Y element, high-purity Gd2O3Cost of material is less than Y2O3Raw material, to reduce
Crystal growth cost.
Technical solution of the invention is as follows：
A kind of high temperature scintillation crystal for high energy ray detector, feature are that this is mixed cerium LGAG crystal and uses melt method
Growth, chemical formula are：
Ce3xLu3(1-x-y)Gd3yAl5O12
In formula, x=0.001~0.1, y=0.8~0.9, x are Doped ions Ce3+, replace in LGAG parent lattices
Gd3+Ion.
A kind of preparation method for mixing Cerium aluminate gadolinium lutetium scintillation crystal, this method include the following steps：
1. composition of raw materials：
Ce3xLu3(1-x-y)Gd3yAl5O12Crystal uses CeO2(5N)、Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) is former
Expect, in molar ratio 6x:3(1-x-y):3y:5 carry out dispensing, and the value range of wherein x, y are respectively x=0.001~0.1, y=
0.8~0.9；
2. using melt method for growing Ce3xLu3(1-x-y)Gd3yAl5O12Scintillation crystal：
First by each high pure oxide powder predrying in air, absorption water is removed, baking material temperature is 1000 DEG C.By x, y
Molar ratio weighing CeO2(5N)、Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material, wherein 5N indicate that the purity of raw material is 5
A 9, i.e., 99.999%, raw material are pressed into the block of required size with isostatic pressing machine, are then charged into oxidation after being sufficiently mixed uniformly
It in aluminium crucible, puts into Muffle furnace and is sintered, 10 hours from room temperature to 1300 DEG C, dropped after 10 hours of constant temperature through 10 hours
It warms to room temperature, the block sintered is taken out and is encapsulated, it is spare to be put into drying box, using the above-mentioned monocrystal of melt method for growing：
The melt method is czochralski method, and the crucible is Iridium Crucible, and seed crystal is<111>Or<100>Direction it is pure
YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.Pull rate is 0.1~5mm/h, rotary speed 5
~30rpm.
The melt method is Bridgman-Stockbarger method, and the crucible material uses high purity graphite, crucible bottom that can not put
Seed crystal, or the pure YAG seed crystals described in above-mentioned czochralski method are put into, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.Earthenware
Crucible fall off rate is 0.1~1.5mm/h.
The melt method is temperature gradient method, and crucible material uses high purity graphite, crucible bottom that can not put seed crystal, or
The pure YAG seed crystals described in above-mentioned czochralski method are put into, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.Make crystal with life
The rate of temperature fall that long rate is 1~50 DEG C/h carries out segmented cooling and grows crystal.The technique effect of the present invention：
It grown the Ce of high quality with the above raw material and technique3xLu3(1-x-y)Gd3yAl5O12Crystal, crystal are yellow, appearance
Well, there are excellent optics and physical and chemical performance.Main glow peak is located at 540nm or so, die-away time about 75ns, Ce3+Concentration
0.1at%~8at%, under high-energy ray irradiation, photon yield is up to 8000~20000Ph/MeV.
Ce3xLu3(1-x-y)Gd3yAl5O12Crystal can be applied to height with the detecting devices efficient coupling such as silicon photo diode
It can physics, nuclear physics, nuclear medical imaging diagnosis (XCT, PET), geological prospecting, the astronomical necks such as Space Physics and safety random check
Domain.
Specific implementation mode
Below by specific implementation, the invention will be further described, but should not be limited the scope of the invention with this.
Embodiment 1：Czochralski grown Ce3+Doping concentration is the Ce of 1.0at%0.03:Lu0.27Gd2.7Al5O12Scintillation crystal
First by the predrying appropriate in air of each high pure oxide powder, absorption water, the calcination at 1000 DEG C are removed
10h, then by CeO2(5N), Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material carries out weighing dispensing according to molar ratio.
Isostatic pressing machine briquet is used after mixing, is put in iridium crucible, using Czochralski grown crystal, seed crystal is<111>Direction
Pure YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.The pull rate of crystal is 1mm/h, and rotating speed is
18rpm, control crystal Raised key axis growth, it is roasting that all crystal growths all pass through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials →
Crystal seed → sow → necking down → shouldering → isodiametric growth → puies forward the processes such as de- and cooling.Entire growth cycle about 7 days.Grow ruler
The very little yellow Ce for Φ 50*100mm:LGAG crystal, crystal weigh about 1200g.
Embodiment 2:Czochralski grown Ce3+Doping concentration is the Ce of 2.0at%0.06:Lu0.24Gd2.7Al5O12Scintillation crystal.
First by the predrying appropriate in air of each high pure oxide powder, absorption water, the calcination at 1000 DEG C are removed
10h, then by CeO2(5N), Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material carries out weighing dispensing according to molar ratio.
Isostatic pressing machine briquet is used after mixing, is put in iridium crucible, using Czochralski grown crystal, seed crystal is<111>Direction
Pure YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.The pull rate of crystal is 1mm/h, and rotating speed is
18rpm, control crystal Raised key axis growth, it is roasting that all crystal growths all pass through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials →
Crystal seed → sow → necking down → shouldering → isodiametric growth → puies forward the processes such as de- and cooling.Entire growth cycle about 7 days.Grow ruler
The very little yellow Ce for Φ 50*100mm:LGAG crystal, crystal weigh about 1200g.
Embodiment 3：Czochralski grown Ce3+Doping concentration is the Ce of 3.0at%0.09:Gd0.21Y2.7Al5O12Scintillation crystal.
First by the predrying appropriate in air of each high pure oxide powder, absorption water, the calcination at 1000 DEG C are removed
10h, then by CeO2(5N), Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material carries out weighing dispensing according to molar ratio.
Isostatic pressing machine briquet is used after mixing, is put in iridium crucible, using Czochralski grown crystal, seed crystal is<111>Direction
Pure YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.The pull rate of crystal is 1mm/h, and rotating speed is
18rpm, control crystal Raised key axis growth, it is roasting that all crystal growths all pass through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials →
Crystal seed → sow → necking down → shouldering → isodiametric growth → carries the processes such as de- and cooling, entire growth cycle about 7 days.Grow ruler
The very little yellow Ce for Φ 50*100mm:LGAG crystal, crystal weigh about 1200g.
Embodiment 4：Czochralski grown Ce3+Doping concentration is the Ce of 5.0at%0.15:Gd0.15Y2.7Al5O12Scintillation crystal.
First by the predrying appropriate in air of each high pure oxide powder, absorption water, the calcination at 1000 DEG C are removed
10h, then by CeO2(5N), Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material carries out weighing dispensing according to molar ratio.
Isostatic pressing machine briquet is used after mixing, is put in iridium crucible, using Czochralski grown crystal, seed crystal is<111>Direction
Pure YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.The pull rate of crystal is 1mm/h, and rotating speed is
18rpm, control crystal Raised key axis growth, it is roasting that all crystal growths all pass through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials →
Crystal seed → sow → necking down → shouldering → isodiametric growth → carries the processes such as de- and cooling, entire growth cycle about 7 days.Grow ruler
The very little yellow Ce for Φ 50*100mm:LGAG crystal, crystal weigh about 1200g.
Embodiment 5：Czochralski grown Ce3+Doping concentration is the Ce of 8.0at%0.24:Lu0.06Gd2.7Al5O12Scintillation crystal.
First by the predrying appropriate in air of each high pure oxide powder, absorption water, the calcination at 1000 DEG C are removed
10h, then by CeO2(5N), Lu2O3(about 5N), Gd2O3(5N) and Al2O3(5N) raw material carries out weighing dispensing according to molar ratio.
Isostatic pressing machine briquet is used after mixing, is put in iridium crucible, using Czochralski grown crystal, seed crystal is<111>Direction
Pure YAG monocrystal rods, crystal growth is in high-purity Ar or high-purity N2It is carried out in atmosphere.The pull rate of crystal is 1mm/h, and rotating speed is
18rpm, control crystal Raised key axis growth, it is roasting that all crystal growths all pass through shove charge → vacuumize → applying argon gas → temperature increasing for melting materials →
Crystal seed → sow → necking down → shouldering → isodiametric growth → carries the processes such as de- and cooling, entire growth cycle about 7 days.Grow ruler
The very little yellow Ce for Φ 50*100mm:LGAG crystal, crystal weigh about 1200g.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (3)
1. one kind mixing Cerium aluminate gadolinium lutetium garnet crystal, it is characterised in that：Molecular formula Ce3xLu3(1-x-y)Gd3yAl5O12, x=in formula
0.001~0.1, y=0.8~0.9, x are the doping of Ce ions, and y is the content of matrix Gd ions, and Ce ions enter LGAG crystalline substances
Body replaces Lu ion sites.
2. a kind of preparation method for mixing Cerium aluminate gadolinium lutetium garnet crystal, it is characterised in that processing step is as follows：
(1) Frequency Induction Heating Czochralski grown Ce is used3xLu3(1-x-y)Gd3yAl5O12Crystal, heater are Iridium Crucible, former
Expect it is fired after as the following formula ratio weighed：
6xCeO2+3(1-x-y)Lu2O3+3yGd2O3+5Al2O3=2Ce3xLu3(1-x-y)Gd3yAl5O12+(3x/2)O2↑
Wherein x is the molar concentration that Ce ions are adulterated in melt, and the doping concentration of Ce ions is then x and segregation coefficient in crystal
Product；
(2) raw material through claim match, grind be mixed it is even after packaging, with isostatic pressed be pressed into it is cylindric and at a high temperature of 1300 DEG C be sintered send out
Raw solid phase reaction is placed in drying box after the raw material encapsulation sintered and saves backup；
(3) insulation cover and thermal insulation material are done with zirconium oxide and aluminium oxide respectively, observation panel is sealed with jewel piece, using inert gas
Protection, about 1950 DEG C, 0.1~5mm/h of pull rate, 5~30rpm of crystal rotation of growth temperature grow Ce3xLu3(1-x-y)
Gd3yAl5O12Crystal.
3. the preparation method according to claim 2 for mixing Cerium aluminate gadolinium lutetium garnet crystal, characterized in that raw materials used
Purity is：CeO2:>=99.999%, Lu2O3:>=99.995%, Gd2O3:>=99.999%, Al2O3:>=99.999%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021031139A1 (en) * | 2019-08-21 | 2021-02-25 | 眉山博雅新材料有限公司 | Multi-component garnet-structured scintillation crystal growth method and equipment |
| CN112552038A (en) * | 2020-11-13 | 2021-03-26 | 浙江大学 | Green fluorescent composite ceramic and preparation method and application thereof |
| CN114958372A (en) * | 2021-12-09 | 2022-08-30 | 营口理工学院 | Preparation of GdAlO by reverse coprecipitation technology 3 Method for preparing Ce luminescent powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297136A (en) * | 2015-11-13 | 2016-02-03 | 孙雷 | Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof |
-
2018
- 2018-04-18 CN CN201810347605.6A patent/CN108441959A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297136A (en) * | 2015-11-13 | 2016-02-03 | 孙雷 | Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021031139A1 (en) * | 2019-08-21 | 2021-02-25 | 眉山博雅新材料有限公司 | Multi-component garnet-structured scintillation crystal growth method and equipment |
| CN112552038A (en) * | 2020-11-13 | 2021-03-26 | 浙江大学 | Green fluorescent composite ceramic and preparation method and application thereof |
| CN112552038B (en) * | 2020-11-13 | 2021-12-14 | 浙江大学 | Green fluorescent composite ceramic and preparation method and application thereof |
| CN114958372A (en) * | 2021-12-09 | 2022-08-30 | 营口理工学院 | Preparation of GdAlO by reverse coprecipitation technology 3 Method for preparing Ce luminescent powder |
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