CN101654807A - Tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum and preparation method thereof - Google Patents
Tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum and preparation method thereof Download PDFInfo
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- CN101654807A CN101654807A CN200910192493A CN200910192493A CN101654807A CN 101654807 A CN101654807 A CN 101654807A CN 200910192493 A CN200910192493 A CN 200910192493A CN 200910192493 A CN200910192493 A CN 200910192493A CN 101654807 A CN101654807 A CN 101654807A
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- yttrium
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- scintillation crystal
- ytterbium ion
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Abstract
The invention discloses a tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum and a preparation method thereof. The chemical composition formula of the tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum is (YmLu(1-m))3Al5O12:x mol%Yb<3+>, wherein the value range of m is larger than or equal to 0.05, but small than or equal to 0.95, x is the mole percentage composition of activated irons (ytterbium irons) accounting for tombarthite irons in the formula, and the value range ofx is larger than or equal to 0.5, but small than or equal to 50. The garnet scintillation crystal material generates two fast damped fluorescence-emission bands within a wavelength range from 300 to600 nanometers under the excitation of high-energy rays. The preparation method of the tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum adopts a fused mass czochralski method, uses a device, i.e. a medium-frequency induction heating lift-pull type single crystal furnace, and can grow large-sized tombarthite and ytterbium ion activationgarnet scintillation crystal containing lutetium, yttrium and aluminum under high temperature.
Description
Technical field
The present invention relates to a kind of rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum and preparation method thereof.
Background technology
Mix trivalent rare earth ytterbium ion (Yb
3+) scintillation crystal is the class flash luminous material that newly-developed gets up, and might be applied to surveying solar neutrino.Neutrino is a kind of not charged, quality is minimum, penetration power is extremely strong ultimate particle, and it has three types, is respectively electron neutrino, muonic neutrino and τ muon neutrino.The thermonuclear reaction meeting of the sun discharges a large amount of electron neutrinos, but because it is had an effect with any material hardly, therefore is difficult to be found and survey.1997, R.S.Raghavan proposed usefulness
176Yb,
160Gd or
82Se is to solar neutrino v
eCapture effect survey the low energy solar neutrino.Wherein,
160Gd exist 4 energy levels can with solar neutrino v
eHave an effect, and also produce the decay of alpha-particle, and
82The transformation period of Se is very short and threshold value generation γ decay is very low.Therefore, in above three kinds of elements,
176Yb is suitable for being used for surveying solar neutrino v most
e
176Yb and solar neutrino v
eInteraction can describe with following process:
v
e+
176Yb→
176Lu*+e
-(Q＝301keV)
176Lu*→
176Lu+γ(E＝72keV)
The γ particle of an ejected electron and a delay is showing a solar neutrino quilt
176Yb catches.If will detect solar neutrino, the time resolution of the fluorescence that sends that just requires detecting material is in 50 nanoseconds.In the rare earth ytterbium ion activated garnet crystal, Yb
3+The luminous character with fast decay of the charge migration band of ion and Sauerstoffatom, its fluorescence decay life-span is within 30 nanoseconds.
Rare-earth garnet N-type waferN (YAG crystal) has very good physical and mechanical property, is the first-selected substrate material of laser crystals.Wherein, trivalent rare earth neodymium ion (Nd
3+), erbium ion (Er
3+), holmium ion (Ho
3+), ytterbium ion (Yb
3+) wait activated YAG crystal to have application very widely in activation processing and laser medicine field.And, YAG crystalline growth technique maturation, raw materials cost is also low, growth of large size high quality monocrystalline at high temperature easily, therefore, rare earth ytterbium ion activated carbuncle type crystal becomes one of preferred material of scintillation crystal.But this crystal has the little and low density shortcoming of effective atomic number, and the doping content that increases ytterbium ion can improve effective atomic number and density, but concentration quenching effect has limited the further raising of ytterbium ion concentration.Calendar year 2001, people such as N.Guerassimova, Yang Peizhi and P.Antonini have studied Yb respectively
3+Ion-activated yttrium aluminum garnet (YAG:Yb
3+) and YBAG ytterbium aluminum garnet (YbAG) crystalline scintillation properties, think to contain Yb
3+Ionic carbuncle type crystal is a kind of scintillation crystal candidate material of surveying solar neutrino, but still needs its efficient and fall time to optimize.
Rare earth lutetium element is close to the ytterbium element in the periodic table of elements, belong to lanthanon together, and atomic radius is quite approaching, and the lutetium atom has big ordination number and do not have luminous energy level.Ruthenium ion with in the part rare earth lutetium ion replacement yttrium aluminum garnet host crystal can not change the crystalline configuration, and can enlarge markedly the crystal effective atomic number, improves crystalline density, increases the uptake factor of crystal to energetic ray.
Summary of the invention
The objective of the invention is to overcome the existing little and low density problem of rare earth ytterbium ion activated yttrium aluminium garnet crystal effective atomic number, the rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum that a kind of effective atomic number is big, density is high material is provided.
Another object of the present invention provides the preparation method of above-mentioned rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum.
Rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum material of the present invention has following chemical constitution expression: (Y
mLu
1-m)
3Al
5O
12: x mol%Yb
3+, wherein: the span of m: 0.05≤m≤0.95; X is the shared chemical formula middle-weight rare earths of active ions (ytterbium ion) ionic molar content, and its span is: 0.5≤x≤50.This crystalline material has higher uptake factor to energetic ray, excites down at energetic ray, produces the fluorescent emission band of two fast decay in the 300-600 nanometer wavelength range.The invention still further relates to the preparation method of this crystalline material, this preparation method is growing large-size ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum at high temperature.
Rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum material of the present invention prepares by the high-temperature fusant vertical pulling method according to the following steps: take by weighing reaction raw materials by atom number ratio in the chemical formula, raw material is a high purity rare earth oxides and alumina powder jointed.Through after the pre-burning, thorough mixing, binder, raw material is put into the iridium crucible of Medium Frequency Induction Heating Furnace, in high-purity argon gas or high pure nitrogen, be heated to the powder raw material fusion.Obtaining the rare earth ytterbium ion through process pulling growths such as seeding, shouldering, isometrical, ending, coolings again activates and contains lutetium, yttrium and aluminum garnet monocrystalline.
Compare with existing ytterbium ion activated yttrium aluminium garnet scintillation crystal, ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum of the present invention has the advantage that effective atomic number is big, density is high.Excite down at energetic ray, scintillation crystal of the present invention produces two fast fluorescent emission bands in the 300-600 nanometer wavelength range, and peak value belongs to Yb respectively respectively in 330 nanometers and 485 nanometers
3+← O
2-Charge migration takes the trivalent ytterbium ion to
2F
5/2With
2F
7/2The transition emission peak of energy level is suitable for being used for doing the detecting material of energetic ray.
Description of drawings
Fig. 1 is the fluorescence emission spectrogram of scintillation crystal of the present invention under x-ray excited.
Embodiment
Embodiment 1
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 10.0945g, lutecium oxide (Lu
2O
3) 336.2102g, ytterbium oxide (Yb
2O
3) 1.7617g, aluminum oxide (Al
2O
3) 151.9318g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 2
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 65.6621g, lutecium oxide (Lu
2O
3) 231.4252g, ytterbium oxide (Yb
2O
3) 38.1975g, aluminum oxide (Al
2O
3) 164.7134g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 3
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 176.9626g, lutecium oxide (Lu
2O
3) 44.5502g, ytterbium oxide (Yb
2O
3) 88.2378g, aluminum oxide (Al
2O
3) 190.2475g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 4
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 265.2763g, lutecium oxide (Lu
2O
3) 22.1439g, ytterbium oxide (Yb
2O
3) 2.4366g, aluminum oxide (Al
2O
3) 210.1407g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 5
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 65.8589g, lutecium oxide (Lu
2O
3) 77.3730g, ytterbium oxide (Yb
2O
3) 191.5599g, aluminum oxide (Al
2O
3) 165.2071g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 6
Take by weighing the high-purity yttrium oxide (Y after the pre-burning
2O
3) 90.7118g, lutecium oxide (Lu
2O
3) 119.8922g, ytterbium oxide (Yb
2O
3) 118.7316g, aluminum oxide (Al
2O
3) 170.6629g, after mixing with mixer, with the raw material compacting, be put in the iridium crucible in the Medium frequency induction single crystal growing furnace, in high-purity argon gas atmosphere, be heated to raw materials melt, pass through processes such as seeding, shouldering, isometrical, ending, cooling again, growth obtains scintillation crystal.
Embodiment 7
Along direction perpendicular to crystal growth, it is the single-chip of 1.0mm that embodiment 1 gained crystal-cut is become thickness, after the polishing both surfaces, under x-ray excited, mensuration obtains the fluorescence emission spectrogram of rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum, and as shown in Figure 1, crystal produces two fast fluorescent emission bands in the 300-600 nanometer wavelength range, peak value is suitable for being used for doing the detecting material of energetic ray respectively in 330 nanometers and 485 nanometers.
Claims (3)
1, a kind of rare earth ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum material, its chemical constitution expression is: (Y
mLu
1-m)
3Al
5O
12: xmol%Yb
3+, wherein:
The span of m: 0.05≤m≤0.95; X is the shared chemical formula middle-weight rare earths of a ytterbium ion ionic molar content, and its span is: 0.5≤x≤50.
2, the described rare earth ytterbium ion of claim 1 activation garnet scintillation crystal containing lutetium, yttrium and aluminum preparation methods, it is characterized in that at first raw material by the accurate weighing of chemical constitution formula, thorough mixing is even, carry out putting into Medium Frequency Induction Heating Furnace behind the binder, adopt high-temperature fusant Grown by CZ Method monocrystal material.
3, by the described rare earth ytterbium ion of claim 2 activation garnet scintillation crystal containing lutetium, yttrium and aluminum preparation methods, it is characterized in that described raw material is rare earth oxide and aluminum oxide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899710A (en) * | 2010-08-10 | 2010-12-01 | 中山大学 | Trivalent rare earth cerium and ytterbium ion codoped yttrium aluminum garnet laser crystal and manufacturing method thereof |
| CN103059860A (en) * | 2012-09-17 | 2013-04-24 | 温州大学 | Manganese-doped yttrium aluminium garnet monocrystal material and application for same |
| CN103397385A (en) * | 2013-08-19 | 2013-11-20 | 山东大学 | Ytterbium, lutecium, gadolinium and gallium doped garnet laser crystal, preparation method and applications thereof |
| CN103614776A (en) * | 2013-10-25 | 2014-03-05 | 中国科学院合肥物质科学研究院 | Laser crystal with wavelength near 2.9 micron and preparation method thereof |
| WO2019157126A1 (en) * | 2018-02-07 | 2019-08-15 | University Of Tennessee Research Foundation | Garnet scintillator co-doped with monovalent ion |
| RU2795600C2 (en) * | 2018-02-07 | 2023-05-05 | Юниверсити Оф Теннесси Рисерч Фаундэйшн | Garnet scintillator solegated with a monovalent ion |
-
2009
- 2009-09-18 CN CN200910192493A patent/CN101654807A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899710A (en) * | 2010-08-10 | 2010-12-01 | 中山大学 | Trivalent rare earth cerium and ytterbium ion codoped yttrium aluminum garnet laser crystal and manufacturing method thereof |
| CN103059860A (en) * | 2012-09-17 | 2013-04-24 | 温州大学 | Manganese-doped yttrium aluminium garnet monocrystal material and application for same |
| CN103059860B (en) * | 2012-09-17 | 2015-01-07 | 温州大学 | Manganese-doped yttrium aluminium garnet monocrystal material and application for same |
| CN103397385A (en) * | 2013-08-19 | 2013-11-20 | 山东大学 | Ytterbium, lutecium, gadolinium and gallium doped garnet laser crystal, preparation method and applications thereof |
| CN103614776A (en) * | 2013-10-25 | 2014-03-05 | 中国科学院合肥物质科学研究院 | Laser crystal with wavelength near 2.9 micron and preparation method thereof |
| CN103614776B (en) * | 2013-10-25 | 2015-11-18 | 中国科学院合肥物质科学研究院 | Wavelength laser crystal and preparation method thereof near a kind of 2.9 microns |
| WO2019157126A1 (en) * | 2018-02-07 | 2019-08-15 | University Of Tennessee Research Foundation | Garnet scintillator co-doped with monovalent ion |
| US11230667B2 (en) | 2018-02-07 | 2022-01-25 | University Of Tennessee Research Foundation | Garnet scintillator co-doped with monovalent ion |
| RU2795600C2 (en) * | 2018-02-07 | 2023-05-05 | Юниверсити Оф Теннесси Рисерч Фаундэйшн | Garnet scintillator solegated with a monovalent ion |
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Open date: 20100224 |