CN1552956A - Method for growing cerium-doped yttrium aluminum garnet crystal - Google Patents

Method for growing cerium-doped yttrium aluminum garnet crystal Download PDF

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CN1552956A
CN1552956A CNA2003101226172A CN200310122617A CN1552956A CN 1552956 A CN1552956 A CN 1552956A CN A2003101226172 A CNA2003101226172 A CN A2003101226172A CN 200310122617 A CN200310122617 A CN 200310122617A CN 1552956 A CN1552956 A CN 1552956A
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crystal
cerium
ceo
aluminum garnet
yttrium aluminum
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CN1259464C (en
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曾雄辉
徐军
赵广军
李红军
何晓明
庞辉勇
介明印
王静雅
张连翰
杭寅
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Abstract

A process for growing Ce-doped yttrium aluminium garnet features that a certain amount of Sc is added to the raw material for growing Ce-doped yttrium aluminium garnet2O3Or Lu2O3The molar ratio of the raw material formula is as follows: al 2O3∶Y2O3∶CeO2+A2O3X is more than or equal to 0.1 percent and less than or equal to 10.0 percent, and y is more than or equal to 0.1x and less than or equal to x; a. the2O3Is Sc2O3Or Lu2O3. The invention can improve the Ce greatly3+And Y3+The large radius fit between the crystal lattices causes lattice distortion, reduces dislocation density and improves the scintillation performance of the yttrium aluminum garnet crystal.

Description

Mix the growth method of the yag crystal of cerium
Technical field:
The present invention relates to yag crystal, particularly a kind of preparation method who mixes the yag crystal of cerium.
Background technology
Mix the yttrium aluminum garnet (Ce of cerium 3+: YAG) crystal has the luminous efficiency height, decay of luminescence is fast, and thermomechanical property is good, peak luminous wavelength is with advantages such as the photomultiplier commonly used and the reception sensitive wavelength of silicon photo diode match, is the fast decay scintillation material of high comprehensive performance.Ce 3+: the YAG single crystal is suitable for surveying light charged particle, especially Ce such as alpha-particle, electronics and β ray 3+: the YAG scintillation detector is widely used in fields such as electron microscope, β and X ray counting, electronics and x-ray imaging screens.
People such as Polish scholar M.Moszy ń ski had studied Ce in 1994 3+: the flicker character of YAG, result of study show it can replaced C sI (Tl) and BGO be used for light charged particle and survey, and because its high-melting-point and deliquescence characteristic not, be more suitable in using (" Properties of YAG:Ce scintillator " is published in Nuclear Instruments andMethods in Physics Research A 345 (1994) 461-467) at high temperature and moist environment midium or long term.People such as Polish scholar T.Ludziejewski were to having the Ce of different cerium doping contents in 1997 3+: the YAG crystal has been done further research, they think that the optimal cerium doping content that is applied to scintillation crystal is (" Investigation of some scintillation properties of YAG:Ce crystals " is published in Nuclear Instruments and Methods in Physics Research A 398 (1997) 287-294) about 1mol%Ce.
But because Ce 3+Radius be 103.4Pm, and Y 3+Radius be 88Pm, so from the angle of ionic radius coupling, Ce 3+Can cause bigger lattice distortion after mixing, undoubtedly, the generation of this lattice distortion can be introduced more point defect, thereby reduce the crystalline scintillation properties in crystal.And can not carry out the doping of higher concentration.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of growth method of mixing the yttrium aluminum garnet of cerium, makes in the technology formerly because the Ce that mixes 3+And Y 3+Between bigger ionic radius mismatch and the lattice distortion problem that causes improves, thereby reduce dislocation desity, improve the scintillation properties of yag crystal.
Sc 3-And Lu 3+Ionic radius all be about 84.8pm, so, can improve lattice distortion to a certain extent if in yag crystal, mix Sc (or Lu) and Ce altogether according to suitable proportioning.And because scandium and lutetium all are a kind of neutral component, so mix a spot of scandium or lutetium does not have any influence to the crystalline scintillation properties.
Technical solution of the present invention is as follows:
A kind of growth method of mixing the yttrium aluminum garnet of cerium is characterized in mixing a certain amount of Sc in the prescription of raw material 2O 3Or Lu 2O 3, to improve because Ce 3+And Y 3+Between bigger radius mismatch and the lattice distortion that causes, thereby reduce dislocation desity, improve the crystalline scintillation properties.
Composition of raw materials of the present invention is:
Al 2O 3: Y 2O 3: CeO 2: A 2O 3=5: 3 (1-x-y): 6x: 3y are 0.1%≤x≤10.0% wherein, 0.1x≤y≤x; A 2O 3Be Sc 2O 3Or Lu 2O 3
The device that the yag crystal of cerium is mixed in used crystal pulling method (Czochralski) growth of the present invention is common Frequency Induction Heating single crystal growing furnace.It comprises parts such as iridium crucible, vacuum system, Medium frequency induction generator power and temperature control system.
The present invention mixes the growth method of the yttrium aluminum garnet of cerium, comprises that following concrete steps are:
1. at span 0.1%≤x of x and y≤10.0%, 0.1x≤y≤x selectes the value of x, y, and by each raw material Y of following composition of raw materials molar ratio weighing 2O 3, Sc 2O 3Or Lu 2O 3, Al 2O 3, CeO 2:
Al 2O 3∶Y 2O 3∶CeO 2∶A 2O 3＝5∶3(1-x-y)∶6x∶3y
0.1%≤x≤10.0% wherein, 0.1x≤y≤x; A 2O 3Be Sc 2O 3Or Lu 2O 3
2. with the raw material Y of above-mentioned weighing 2O 3, Sc 2O 3(or Lu 2O 3), A1 2O 3, CeO 2, after mechanical mixture is even, use swager at 20-50kg/cm 2Pressure under be pressed into cake;
3. at 1000-1650 ℃ of sintering 10-20h;
4. use Czochralski grown crystal: shove charge vacuumizes fills high pure nitrogen, and growth is prepared in the fusing that heats up: pull rate is 0.5-3mm/h, and speed of rotation is 10-20rpm;
5. behind the grown crystal, slowly be down to room temperature, take out crystal.
Advantage of the present invention: owing to adopted Sc 2O 3Or Lu 2O 3And CeO 2The method of mixing altogether according to a certain ratio, thus can improve to a great extent because Ce 3+And Y 3+Between the adaptive and lattice distortion that causes of bigger radius, thereby reduce dislocation desity, improve the scintillation properties of yag crystal.
Embodiment:
Embodiment 1:
In this example, x=0.1%, y=0.01%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.9967: 5: 0.006: 0.0003 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 20kg/cm 2Pressure under briquet then, in 1000 ℃ of sintering 10h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up: pull rate is 1mm/h, and rotary speed is 10rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 2.
X=0.1% in this example, y=0.1%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.994: 5: 0.006: 0.003 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 50kg/cm 2Pressure under briquet, then in 1650 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 3mm/h, and speed of rotation is 20rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 3.
X=0.1% in this example, y=0.05%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.9955: 5: 0.006: 0.0015 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1300 ℃ of sintering 15h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 4.
X=2% in this example, y=0.2%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.934: 5: 0.12: 0.006 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 30kg/cm 2Pressure under briquet then in 1400 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 5.
X=2% in this example, y=1%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.91: 5: 0.12: 0.03 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 35kg/cm 2Pressure under briquet then in 1350 ℃ of sintering 18h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 16rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 6.
X=2% in this example, y=2%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.88: 5: 0.12: 0.06 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 45kg/cm 2Pressure under briquet then in 1450 ℃ of sintering 12h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 7.
X=6% in this example, y=0.6%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.802: 5: 0.36: 0.018 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 50kg/cm 2Pressure under briquet then in 1300 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 8.
X=6% in this example, y=3%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.73: 5: 0.36: 0.09 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1550 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 9.
X=6% in this example, y=6%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.64: 5: 0.36: 0.18 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 30kg/cm 2Pressure under briquet then in 1650 ℃ of sintering 14h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 13rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 10.
X=10% in this example, y=1%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.67: 5: 0.6: 0.03 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1350 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 11.
X=10% in this example, y=5%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.55: 5: 0.6: 0.15 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 45kg/cm 2Pressure under briquet then in 1550 ℃ of sintering 15h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 13rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 12.
X=10% in this example, y=10%.So with Y 2O 3, Al 2O 3, CeO 2, Sc 2O 3High pure raw material was according to 2.4: 5: 0.6: 0.3 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 35kg/cm 2Pressure under briquet then in 1450 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Sc 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 13.
X=0.1% in this example, y=0.01%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.9967: 5: 0.006: 0.0003 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 20kg/cm 2Pressure under briquet then in 1000 ℃ of sintering 10h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 10rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 14.
X=0.1% in this example, y=0.1%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.994: 5: 0.006: 0.003 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 50kg/cm 2Pressure under briquet then in 1650 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 3mm/h, and speed of rotation is 20rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 15.
X=0.1% in this example, y=0.05%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.9955: 5: 0.006: 0.0015 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1300 ℃ of sintering 15h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 16.
X=2% in this example, y=0.2%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.934: 5: 0.12: 0.006 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 30kg/cm 2Pressure under briquet then in 1400 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 17.
X=2% in this example, y=1%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.91: 5: 0.12: 0.03 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 35kg/cm 2Pressure under briquet then in 1350 ℃ of sintering 18h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 2mm/h, and speed of rotation is 16rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 18.
X=2% in this example, y=2%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.88: 5: 0.12: 0.06 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 45kg/cm 2Pressure under briquet then in 1450 ℃ of sintering 12h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 19.
X=6% in this example, y=0.6%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.802: 5: 0.36: 0.018 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 50kg/cm 2Pressure under briquet then in 1300 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 20.
X=6% in this example, y=3%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.73: 5: 0.36: 0.09 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1550 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 21.
X=6% in this example, y=6%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.64: 5: 0.36: 0.18 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 30kg/cm 2Pressure under briquet then in 1650 ℃ of sintering 14h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 1mm/h, and speed of rotation is 13rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 22.
X=10% in this example, y=1%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.67: 5: 0.6: 0.03 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 40kg/cm 2Pressure under briquet then in 1350 ℃ of sintering 20h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 12rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 23.
X=10% in this example, y=5%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.55: 5: 0.6: 0.15 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 45kg/cm 2Pressure under briquet then in 1550 ℃ of sintering 15h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 13rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.
Embodiment 24.
X=10% in this example, y=10%.So with Y 2O 3, Al 2O 3, CeO 2, Lu 2O 3High pure raw material was according to 2.4: 5: 0.6: 0.3 mole proportioning weighing, gross weight is 1Kg.After mechanical mixture is even, use swager at 35kg/cm 2Pressure under briquet then in 1450 ℃ of sintering 16h, shove charge vacuumizes fills high pure nitrogen, growth is prepared in the fusing that heats up.Pull rate is 0.5mm/h, and speed of rotation is 14rpm.Behind the grown crystal, slowly be down to room temperature, take out crystal.The crystal water white transparency is complete, and quality is better.Than not mixing altogether Lu 2O 3Same concentration cerium-doped yttrium aluminum garnet scintillation crystal, dislocation density reduces, the passage of scintillation light output performance improves 5%-20%.

Claims (3)

1, a kind of growing method of mixing the yttrium-aluminium-garnet of cerium, the key that it is characterized in that this method are in the composition of raw materials of growth cerium-doped yttrium aluminum garnet, mix a certain amount of Sc 2O 3Or Lu 2O 3, the mol ratio of its composition of raw materials is: Al 2O 3: Y 2O 3: CeO 2: A 2O 3=5: 3 (1-x-y): 6x: 3y are 0.1%≤x≤10.0% wherein, 0.1x≤y≤x; A 2O 3Be Sc 2O 3Or Lu 2O 3
2, growth method of mixing the yttrium aluminum garnet of cerium according to claim 1 is characterized in that comprising that following concrete steps are:
1. at span 0.1%≤x of x and y≤10.0%, 0.1x≤y≤x selectes the value of x, y, and presses each raw material Y of the following molar ratio weighing of composition of raw materials 2O 3, Sc 2O 3(or Lu 2O 3), Al 2O 3, CeO 2:
Al 2O 3∶Y 2O 3∶CeO 2∶A 2O 3＝5∶3(1-x-y)∶6x∶3y
0.1%≤x≤10.0% wherein, 0.1x≤y≤x; A 2O 3Be Sc 2O 3Or Lu 2O 3
2. with the raw material Y of above-mentioned weighing 2O 3, Sc 2O 3(or Lu 2O 3), Al 2O 3, CeO 2, after mechanical mixture is even, use swager at 20-50kg/cm 2Pressure under be pressed into cake;
3. at 1000-1650 ℃ of sintering 10-20h;
4. use Czochralski grown crystal: shove charge vacuumizes fills high pure nitrogen, and growth is prepared in the fusing that heats up: pull rate is 0.5-3mm/h, and speed of rotation is 10-20rpm;
5. behind the grown crystal, slowly be down to room temperature, take out crystal.
3, growth method of mixing the yttrium aluminum garnet of cerium according to claim 2, the device that it is characterized in that described Czochralski grown cerium-doped yttrium aluminum garnet crystal are common Frequency Induction Heating single crystal growing furnace.
CN 200310122617 2003-12-19 2003-12-19 Method for growing cerium-doped yttrium aluminum garnet crystal Expired - Fee Related CN1259464C (en)

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CN100447309C (en) * 2007-04-30 2008-12-31 山东大学 Prepn process and use of calcium and lithium dopped Ta-Ga garnet crystal
CN100447308C (en) * 2007-04-30 2008-12-31 山东大学 Calcium dopped Ta-Ga garnet crystal prepn process and use
CN100540755C (en) * 2007-05-10 2009-09-16 中国科学院安徽光学精密机械研究所 Efficient radioprotective Yb 3+Sensitization Er 3+Contain scandium garnet laser crystals and preparation method thereof
CN101409424B (en) * 2007-10-12 2010-09-29 中国科学院安徽光学精密机械研究所 Nd, er: GSGG and preparation method of Nd, er: GSGG anti-radiation laser crystal sensitized by Nd3+ion
CN105283526A (en) * 2013-10-23 2016-01-27 株式会社光波 Single crystal phosphor, phosphor-containing member and light emitting device
CN105658764A (en) * 2013-10-23 2016-06-08 株式会社光波 Single-crystal phosphor and light-emitting device
JP2018191006A (en) * 2013-10-23 2018-11-29 株式会社光波 Light-emitting device

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Publication number Priority date Publication date Assignee Title
CN100447309C (en) * 2007-04-30 2008-12-31 山东大学 Prepn process and use of calcium and lithium dopped Ta-Ga garnet crystal
CN100447308C (en) * 2007-04-30 2008-12-31 山东大学 Calcium dopped Ta-Ga garnet crystal prepn process and use
CN100540755C (en) * 2007-05-10 2009-09-16 中国科学院安徽光学精密机械研究所 Efficient radioprotective Yb 3+Sensitization Er 3+Contain scandium garnet laser crystals and preparation method thereof
CN101409424B (en) * 2007-10-12 2010-09-29 中国科学院安徽光学精密机械研究所 Nd, er: GSGG and preparation method of Nd, er: GSGG anti-radiation laser crystal sensitized by Nd3+ion
CN105283526A (en) * 2013-10-23 2016-01-27 株式会社光波 Single crystal phosphor, phosphor-containing member and light emitting device
CN105658764A (en) * 2013-10-23 2016-06-08 株式会社光波 Single-crystal phosphor and light-emitting device
US20160240748A1 (en) * 2013-10-23 2016-08-18 Koha Co., Ltd. Single-crystal phosphor and light-emitting device
CN108538991A (en) * 2013-10-23 2018-09-14 株式会社光波 The cie color of light-emitting device（X, y）Method of adjustment
JP2018191006A (en) * 2013-10-23 2018-11-29 株式会社光波 Light-emitting device
CN110838540A (en) * 2013-10-23 2020-02-25 株式会社光波 Light emitting device
CN110835534A (en) * 2013-10-23 2020-02-25 株式会社光波 Phosphor-containing member and light-emitting device

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