CN105297136A - Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof - Google Patents
Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and a preparation method thereof. The crystal has a chemical formula of Ce3xLu3(1-x-y)Gy3yAl5O12. The crystal is grown by using an intermediate-frequency induction heating Czochralski method; a heat-generating body is an iridium crucible; raw materials are weighed, batched, ground and uniformly mixed, then the obtained mixture is briquetted with an isostatic pressing machine, and sintering is carried out at a high temperature so as to allow the briquetted mixture to undergo a solid phase reaction; zirconia and alumina are separately used as insulation covers; the interior of a hearth is protected by inert gas in the process of growing; crystal growth temperature is about 1950 DEG C; a pulling rate is 0.1 to 5 mm/h; and a crystal rotating speed is 5 to 30 rpm. The preparation method has the advantages of low crystal growth cost, easiness in preparation of large-size crystal, realization of high-concentration doping, excellent scintillation property, etc.; and the prepared crystal can be used as a core material for development of a laser illumination system.
Description
Technical field
The present invention relates to scintillation crystal, particularly one mixes Cerium aluminate gadolinium lutetium Ce
3xlu
3 (1-x-y)gy
3yal
5o
12high 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 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, 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 received much concern 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 3 processes below: 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.
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 inorganic 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.The silicic acid lutetium (LSO) of Ce ion doping and yttrium luetcium silicate crystal (LYSO) 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.
At present, mainly there are following two shortcomings in Ce:YAG crystal: 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 huge, 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.
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 Ce being mainly used in laser illuminator
3xlu
3 (1-x-y)gy
3yal
5o
12high temperature scintillation crystal and preparation method thereof, this crystal can realize greater concn Ce
3+ion doping, and there is higher density and flicker cut-off energy, be a kind of high temperature scintillator crystal materials of excellent performance.Simultaneously because Gy instead of matrix Y element as main matrix element, high-purity Gy
2o
3cost of material is lower than Y
2o
3raw material, thus reduce crystal growth cost.
Technical solution of the present invention is as follows:
Be mainly used in a high temperature scintillation crystal for laser illuminator, feature is that this is mixed cerium LGAG crystal and adopts melt method for growing, and its chemical formula is:
Ce
3xLu
3(1-x-y)Gy
3yAl
5O
12
In formula, x=0.001 ~ 0.1, y=0.8 ~ 0.9, x is dopant ion Ce
3+, it replaces the Gy in LGAG parent lattice
3+ion.
Mix a preparation method for Cerium aluminate gadolinium lutetium scintillation crystal, the method comprises the following steps:
1. composition of raw materials:
Ce
3xlu
3 (1-x-y)gy
3yal
5o
12crystal adopts CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(5N) and Al
2o
3(5N) raw material, in molar ratio 6x:3 (1-x-y): 3y:5 prepares burden, and wherein the span of x, y is respectively x=0.001 ~ 0.1, y=0.8 ~ 0.9;
2. melt method for growing Ce is adopted
3xlu
3 (1-x-y)gy
3yal
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.By x, y molar ratio weighing CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(5N) and Al
2o
3(5N) raw material, wherein 5N represents that the purity of raw material is 59, namely 99.999%, raw material fully mixes the block material that rear isostatic pressing machine is pressed into desired size, then loads 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, and the block material sintered is taken out encapsulation, put into loft drier for subsequent use, adopt the above-mentioned single crystal of melt method for growing:
Described melting method is crystal pulling method, and described crucible is Iridium Crucible, and seed crystal is the pure YAG 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 YAG 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 YAG 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 Ce is grown with above raw material and technique
3xlu
3 (1-x-y)gy
3yal
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 540nm, and fall time is about 75ns, Ce
3+concentration 0.1at% ~ 8at%, under high-energy ray irradiation, photon yield can reach 8000 ~ 20000Ph/MeV.
Ce
3xlu
3 (1-x-y)gy
3yal
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 Ce
3+doping content is the Ce of 1.0at%
0.03: Lu
0.27gy
2.7al
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 CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(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 1mm/h, and rotating speed is 18rpm, controls the growth of crystal Raised key axis, and 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 Ce:LGAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 2: Czochralski grown Ce
3+doping content is the Ce of 2.0at%
0.06: Lu
0.24gy
2.7al
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 CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(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 1mm/h, and rotating speed is 18rpm, controls the growth of crystal Raised key axis, and 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 Ce:LGAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 3: Czochralski grown Ce
3+doping content is the Ce of 3.0at%
0.09: Gy
0.21y
2.7al
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 CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(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 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 Ce:LGAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 4: Czochralski grown Ce
3+doping content is the Ce of 5.0at%
0.15: Gy
0.15y
2.7al
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 CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(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 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 Ce:LGAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Embodiment 5: Czochralski grown Ce
3+doping content is the Ce of 8.0at%
0.24: Lu
0.06gy
2.7al
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 CeO
2(5N), Lu
2o
3(about 5N), Gy
2o
3(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 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 Ce:LGAG crystal being of a size of Φ 50*100mm, crystal is 1200g heavily about.
Claims (3)
1. laser illuminator is with mixing a Cerium aluminate gadolinium lutetium garnet crystal, it is characterized in that: molecular formula Ce
3xlu
3 (1-x-y)gy
3yal
5o
12, x=0.001 ~ 0.1 in formula, y=0.8 ~ 0.9, x is the doping of Ce ion, and y is the content of matrix Gy ion, and Ce ion enters LGAG crystal and replaces Lu ion site.
2. the laser illuminator preparation method mixing Cerium aluminate gadolinium lutetium garnet crystal, is characterized in that processing step is as follows:
(1) Frequency Induction Heating Czochralski grown Ce is adopted
3xlu
3 (1-x-y)gy
3yal
5o
12crystal, heating element is Iridium Crucible, and raw material weighs in following formula ratio after roasting:
6xCeO
2+3(1-x-y)Lu
2O
3+3yGy
2O
3+5Al
2O
3=2Ce
3xLu
3(1-x-y)Gy
3yAl
5O
12+(3x/2)O
2↑
Wherein x is the volumetric molar concentration of doped Ce ion in melt, and in crystal, the doping content of Ce ion is then the product of x and segregation coefficient;
(2) raw material is through claiming to join, and grinds the even rear packaging that is mixed, and is pressed into cylindric and under the high temperature of 1300 DEG C, sinters generation solid state reaction with isostatic pressed, is placed in loft drier and saves backup after the raw material sintered encapsulation;
(3) do stay-warm case and lagging material with zirconium white and aluminum oxide respectively, seal porthole with jewel sheet, adopt protection of inert gas, growth temperature about 1950 DEG C, pull rate 0.1 ~ 5mm/h, crystal rotation 5 ~ 30rpm, growth Ce
3xlu
3 (1-x-y)gy
3yal
5o
12crystal.
3. the laser illuminator according to claim 2 preparation method mixing Cerium aluminate gadolinium lutetium garnet crystal, it is characterized in that, raw materials used purity is: CeO
2:>=99.999%, Lu
2o
3:>=99.995%, Gy
2o
3:>=99.999%, Al
2o
3:>=99.999%.
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| 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 |
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Application publication date: 20160203 |