CN110004485A - A kind of scintillation crystal and preparation method thereof of rare earth element cerium dopping - Google Patents
A kind of scintillation crystal and preparation method thereof of rare earth element cerium dopping Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The invention discloses a kind of scintillation crystal and preparation method thereof of rare earth element cerium dopping, feature is its chemical structural formula are as follows: MY2X7: Ce, wherein M=K, Cs, Rb；X=Cl, Br, preparation method the following steps are included: (1) by lower purity feedstock MX, CeX3And YX3Raw material is respectively charged into large scale silica crucible, is vacuumized and is heated to 250 DEG C of heat preservations 2 hours；Sealing silica crucible is fitted into crucible decline furnace, and heat up sufficiently melting decline, obtains high-purity MX, CeX3And YX3Raw material；MX:YX in molar ratio again3: CeX3=1:2:0.001 mixing vacuumizes heat-agglomerating and obtains anhydrous MY2X7: Ce polycrystal material；(2) anhydrous MY will be contained2X7: the silica crucible of Ce polycrystal material is put into crucible decline furnace, and heating heating declines again up to solidification completely, then is down to room temperature and obtains scintillation crystal, and advantage is that particle size is big and water suction hygroscopy is low.
Description
Technical field
The present invention relates to a kind of scintillation crystals, scintillation crystal and its preparation more particularly, to a kind of rare earth element cerium dopping
Method.
Background technique
Inorganic scintillation crystal is a kind of novel light functional crystal material, and the blinking characteristic that it has is to absorb X-ray, γ
Ultraviolet light or visible light are inspired after the energy of the high energy particles such as ray.Often combine photomultiplier tube (PMT), silicon photo diode
Detecting element is formed Deng (SPD) etc., the light based on scintillation crystal-light transition effects may be implemented under various technical conditions
High-energy ray precision detection, thus develop it is a variety of by X-ray detection X be imaged based on a series of modern high technologies, be high
The critical material in the fields such as energy physics, nuclear physics, safety random check, the survey of industrial non-destructive triage, nuclear medicine, geological prospecting.
The photoyield of rare earth halide type scintillation crystal is mostly in 30000-80000ph MeV-1Between, energy resolution
Between 3.0%-7.0% (662 keV of@), die-away time is within the scope of 30-50ns, and single rare earth halide and alkali metal rare earth
The not big difference of the scintillation properties of halide all has photoyield high, energy resolution and the good feature of temporal resolution.Closely
During the last ten years, people have put into a large amount of time and efforts to this crystalloid.Saint-Gobain (Saint-Gobain) such as France is public
Department, GE company, RMD company, Lawrence Berkeley National Laboratory, the LawrenceLivermore country in the U.S.
Laboratory, Tennessee university, Wake Forest university, Dutch Delft Polytechnics, Russian BTCP are public
Department, rare earth halide type scintillation crystal grinds in a series of domestic and international research institutions such as Japanese Osaka University, Tokyo University
Hair has carried out emphasis investment.Shanghai Inst. of Silicate, Chinese Academy of Sciences, China, Beijing Glass Inst., Chinese Academy of Sciences's Fujian object in recent years
The units such as matter structural research institute, University Of Ningbo, Hua Kai dragon electronic equipment Co., Ltd have also carried out a large amount of research work.
This kind of compound reported at present mainly has CsCe2Cl7、CsCe2Br7Deng they have fast die-away time, excellent
Elegant energy resolution and higher photoyield.But rare earth halide has the following problems, first is that high-pure anhydrous rare earth halide
The high-volume of raw material, inexpensive technology of preparing cause to maintain height in experiment and growth course due to its strong water imbibition
Anaerobic anhydrous atmosphere, another step keeps growth difficult.It is mainly shown as following two points: one, in the original for synthesizing and handling high-purity
When material, these raw materials of rare earth halide, alkaline-earth halide, during thermal dehydration, rare earth halide is easily hydrolyzed,
Oxygen containing compound is generated, causes the preparation of high-pure anhydrous raw material very difficult, thus cost is prohibitively expensive.Such as LaBr 3:
Only cost of material is up to 2000 dollars every kilogram to Ce, and large batch of cannot provide.And due to, if rare earth halide
After raw material causes purity to reduce because water suction deliquesces, the large scale rate of the multielement rare earth halide scintillation crystal grown is synthesized sharply
It reduces, crystal preparation cost also increases.Two, in the processing of rare earth halide scintillation crystal and in application, the crystalline substance in order to prevent
The water suction of body tide solution, crystal must carry out Non-aqueous processing, this can also be such that preparation cost is greatly promoted.Therefore, water imbibition is prepared
The low crystal of hygroscopy be it is highly important, to promote rare earth scintillating crystals development have great function.
Summary of the invention
And a kind of absorb water hygroscopy low rare earth element big technical problem to be solved by the invention is to provide particle size
Scintillation crystal of cerium dopping and preparation method thereof.
The technical scheme of the invention to solve the technical problem is: a kind of flashing of rare earth element cerium dopping is brilliant
Body, chemical structural formula are as follows: MY2X7: Ce, wherein M=K, Cs, Rb；X=Cl, Br.
The preparation method of the scintillation crystal of above-mentioned rare earth element cerium dopping, comprising the following steps:
(1) MY2X7: Ce Material synthesis
A. prepared by high pure raw material: by lower purity feedstock MX, CeX3And YX3Raw material is respectively charged into large scale silica crucible, is used
Vacuum pump vacuumizes it, and in vacuum, silica crucible is transferred in tube furnace, and is heated to 250 DEG C of heat preservations 2
Hour；Tube sealing operation is then carried out to it makes that silica crucible is packed into crucible and declines furnace for anhydrous and oxygen-free atmosphere in silica crucible
In, temperature is elevated above 50 DEG C -150 DEG C of material fusing point in silica crucible, heat preservation for 24 hours, is sufficiently melted, then with 6-
The decrease speed of 20mm/day slowly decline until dropping distance reach crystal length in silica crucible, respectively obtain high-purity MX,
CeX3And YX3Raw material；
B. anhydrous MY is prepared2X7: Ce polycrystal material: operating in glove box, anhydrous MX, the CeX that will be prepared3And YX3Raw material massage
You compare MX:YX3: CeX3 =1:2:0.001 ratio weighs, and is fitted into clean ceramic mortar, and grinding 1 hour, after mixing
Being encapsulated in bottom is then to vacuumize in funnelform silica crucible and be heated to 250 DEG C of heat preservations 2 hours, seal silica crucible, put
Enter in tube furnace, be heated above 50 DEG C -150 DEG C of material fusing point in silica crucible, after keeping the temperature 12-72h, with 50-150 DEG C/h's
Speed is slowly dropped to room temperature, obtains anhydrous MY2X7: Ce polycrystal material；
(2) MY2X7: the growth of Ce crystal
Contain anhydrous MY for what step (1) obtained2X7: the silica crucible of Ce polycrystal material is put into vertically arranged crucible decline vertically
Temperature is elevated above in silica crucible after 10-100 DEG C of material fusing point by furnace, after heat preservation for 24 hours, by the bottom temp of silica crucible
Control is being higher than 20-50 DEG C of material fusing point in silica crucible, then is making silica crucible in crucible with the even speed of 0.5-20mm/h
Decline in decline furnace, until being completely solidified into solid, stops decline, then so that crucible is declined furnace with the cooling rate of 10-100 DEG C/h
Room temperature is down to get the scintillation crystal of rare earth element cerium dopping, chemical structural formula are as follows: MY is arrived2X7: Ce, wherein M=K, Cs, Rb；
X=Cl, Br.
Compared with the prior art, the advantages of the present invention are as follows a kind of scintillation crystal of: rare earth element cerium dopping of the present invention and
Preparation method, containing elements such as alkali metal Cs in halide, so that the ratio of rare earth element is significantly reduced, drop
The low cost of crystal raw material.On the other hand, the rare earth ion and hydrone of high charge, small radii are only occurred in due to hydrolyzing
Between, however when be added to the biggish alkaline-earth metal of some ionic radius and rare earth ion carry out it is compound but also MY2X7: Ce halogen
The water-disintegrable reduction of compound makes the water imbibition of this Pseudohalides also because the dissolubility of binary rare-earth halide in water is very low
It reduces.Therefore, by MRE2X7Its materialization (mainly hydrolysis and water imbibition) is studied in the replacement of middle alkali metal, rare earth, halogen
And scintillation properties, it is expected to obtain comprehensive cost performance preferably novel scintillator crystal materials.
Detailed description of the invention
Fig. 1 is CsY in embodiment 12Cl7: the XRD spectrum of Ce powder；
Fig. 2 is CsY in embodiment 12Cl7: the excitation of X-rays emission spectrum of Ce crystal；
Fig. 3 is CsY in crucible in embodiment 12Cl7: Ce crystal picture；
Fig. 4 is RbY in embodiment 22Cl7: the XRD spectrum of Ce powder；
Fig. 5 is RbY in embodiment 22Cl77: the excitation of X-rays emission spectrum of Ce crystal；
Fig. 6 is RbY in crucible in embodiment 22Cl7: Ce crystal picture；
Fig. 7 is CsY2Cl7: Ce crystal is placed in the metamorphosis in air, and a is before changing, and b is after changing；
Fig. 8 is the water absorption versus time curve figure of a variety of crystal under certain condition.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1
A kind of rare earth halide mixing scintillation crystal, chemical structural formula CsY2Cl7: Ce, above-mentioned rare earth halide mixing are dodged
Bright crystal is prepared using Bridgman-Stockbarger method, and specific step is as follows for preparation method:
1、CsY2Cl7: Ce Material synthesis
1.1 raw materials preparation: by lower purity feedstock CsCl, CeCl3And YCl3Raw material is respectively charged into large scale silica crucible；
1.2 vacuumize and heat: being vacuumized using vacuum pump to it, crucible is transferred to tube furnace by vacuum
It is interior, and be heated to 250 DEG C and keep the temperature 2 hours, to remove the absorption water and the crystallization water that contain in raw material；
1.3 seal and clean: then carrying out tube sealing operation to it, it is ensured that are anhydrous and oxygen-free atmosphere in crucible, are packed into crucible decline
Temperature is elevated above 50 DEG C -150 DEG C of material fusing point in silica crucible by furnace, and heat preservation for 24 hours, is sufficiently melted；Again with 6-
The decrease speed of 20mm/day slowly declines until dropping distance reaches crystal length in silica crucible, and spontaneous impurities removal obtains high-purity
CsCl、CeCl3、YCl3Raw material.It is operated in glove box, gives up impurity, take out transparent part as experimental raw；
1.4 prepare anhydrous CsY2Cl7: Ce polycrystal material: operating in glove box, anhydrous CsCl, the CeCl that will be prepared3、YCl3
Raw material CsCl:YCl in molar ratio3: CeCl3 =1:2:0.001 ratio weighs, and is fitted into clean ceramic mortar, and it is small to grind 1
When, make uniformly to mix；
The roasting of 1.5 heating in vacuum: being encapsulated in bottom is then to vacuumize 250 DEG C of heat preservations 2 of heating in funnelform silica crucible
Hour, silica crucible is sealed, is put into tube furnace, 50 DEG C -150 DEG C of material fusing point in silica crucible are heated above, keeps the temperature 12-
After 72h, room temperature (process is pre-sintering process) is slowly dropped to using the speed of 50-150 DEG C/h, obtains anhydrous MY2X7: Ce polycrystalline
Material.
By CsCl, YCl3And CeCl3By 730 DEG C of temperature melt process obtain polycrystal powder XRD spectrum as shown in Figure 1,
The XRD diffraction maximum of polycrystal powder and pure CsY2Cl7Standard PDF card is completely the same, and not extra miscellaneous peak shows by CsCl,
YCl3And CeCl3The raw material of synthesis in solid state is pure CsY2Cl7Polycrystal material.XRD data are imported into Jade, are counted by fitting
It calculates and determines that its cell parameter is a=13.354, b=6.967, c=7.922 are orthorhombic structure, and have reported
Crystal phase structure match.Water removal analysis, using cassette coulometry to the CsY of synthesis2Cl7Water content in polycrystal material into
Row detection, the detection of oxygen content is carried out using the impulse melting reduction method based on infrared absorption, it was therefore concluded that water content is lower than
10ppm。
2、CsY2Cl7: the growth of Ce crystal
2.1 crystal materials: anhydrous MY will be contained2X7: the sealing silica crucible of Ce polycrystal material is put into the crucible placed vertically vertically
Decline in furnace, temperature is elevated above 10-100 DEG C of material fusing point in silica crucible, heat preservation for 24 hours, carries out fully melt；
2.2 crystal growths: the bottom temp control of silica crucible is then being higher than in silica crucible 20-50 on material fusing point
DEG C, then decline silica crucible in crucible decline furnace with the even speed of 0.5-20mm/h, until being completely solidified into solid, stop
Only decline, then drops to crucible with the cooling rate of 10-100 DEG C/h and be down to room temperature.
2.3 obtain crystal: finally, operating in glove box, taking out the CsY prepared in silica crucible2Cl7: the sudden strain of a muscle of Ce
Bright crystal.
The scintillation properties of 2.4 CsY2Cl7:Ce are tested and analysis
Excitation of X-rays emission spectrum is tested using excitation of X-rays emission spectrometer is voluntarily built, is sharp with tungsten target X-ray tube
Light emitting source, photomultiplier tube carry out detector transmitting light.Fig. 2 is the excitation of X-rays emission spectrum of CsY2Cl7:Ce crystal, entire light
It is in symmetrical structure than wider luminous zone that spectrum has one in the wave-length coverage of 300-600nm, and the position of peak value is 400nm left
It is right.It is almost consistent with the photoluminescence emission wavelength under ultraviolet lamp excitation, it can match well with light emitting diode.
2.5 CsY2Cl7: the growth characteristics of Ce crystal
The polycrystal material that above-mentioned high temperature process heat obtains is gone out into CsY by Bridgman-Stockbarge method for growing2Cl7: Ce monocrystalline.Fig. 3 is crystalline substance
Body takes out the picture of silica crucible from decline furnace, and the upper end of the crucible crystal is fog-like opaque, due in single crystal growth process
Impurities removal process and growth course in technique influence, intermediate shouldering part can be seen that transparent do not crack is about 20
The transparent single crystal of mm.The portion of monocrystalline is taken out from crucible, polishes to obtain 12 mm of φ × 10mm circle by cutting and grinding
The monocrystalline of the transparent no cracking of cylinder.Illustrate, the crystal structure and growth technique of the crystal can be easier to grow transparent big
Monocrystalline, more preferably as scintillation crystal performance.
Embodiment 2
A kind of rare earth halide mixing scintillation crystal, constitutional chemistry formula are RbY2Cl7: Ce, above-mentioned rare earth halide mixing are dodged
Bright crystal is prepared using Bridgman-Stockbarger method, and specific step is as follows for preparation method:
1. RbY2Cl7: Ce Material synthesis
1.1 raw materials preparation: by lower purity feedstock RbCl, CeCl3、YCl3Raw material is respectively charged into large scale silica crucible.
1.2 vacuumize and heat: being vacuumized using vacuum pump to it, crucible is transferred to tubular type by vacuum
It in furnace, and is heated to 250 DEG C and keeps the temperature 2 hours, to remove the absorption water and the crystallization water that contain in raw material；
1.3 seal and clean: then carrying out tube sealing operation to it, it is ensured that are anhydrous and oxygen-free atmosphere in crucible, are packed into crucible decline
Temperature is elevated above 50 DEG C -150 DEG C of material fusing point in silica crucible by furnace, and heat preservation for 24 hours, is sufficiently melted, then with 6-
The decrease speed of 20mm/day slowly declines until dropping distance reaches crystal length in silica crucible, and spontaneous impurities removal obtains high-purity
RbCl、CeCl3、YCl3Raw material operates in glove box, gives up impurity, takes out transparent part as experimental raw；
1.4 prepare anhydrous RbY2Cl7: Ce polycrystal material: operating in glove box, anhydrous RbCl, the CeCl that will be prepared3、YCl3
Raw material RbCl:YCl in molar ratio3: CeCl3=1:2:0.001 ratio weighs, and is fitted into clean ceramic mortar, and it is small to grind 1
When, make uniformly to mix；
The roasting of 1.5 heating in vacuum: being encapsulated in bottom is then to vacuumize 250 DEG C of heat preservations 2 of heating in funnelform silica crucible
Hour, silica crucible is sealed, is put into tube furnace, 50 DEG C -150 DEG C of material fusing point in silica crucible are heated above, keeps the temperature 12-
After 72h, room temperature is slowly dropped to the speed of 50-150 DEG C/h, obtains anhydrous RbY2Cl7: Ce polycrystal material；
By RbCl, YCl3And CeCl3The XRD spectrum of polycrystal powder is obtained as shown in figure 4, more by 760 DEG C of temperature melt process
The XRD diffraction maximum of crystalline flour body and pure RbY2Cl7: completely the same, the not extra miscellaneous peak of Ce standard PDF card, show by
RbCl, YCl3And CeCl3The raw material of synthesis in solid state is pure RbY2Cl7: Ce polycrystal material.Water removal analysis, using cassette coulometry pair
The RbY of synthesis2Cl7: the water content in Ce polycrystal material is detected, and is carried out using the impulse melting reduction method based on infrared absorption
The detection of oxygen content, it was therefore concluded that water content is lower than 10ppm.
2 . RbY2Cl7: the growth of Ce crystal
2.1 crystal materials: the silica crucible of sealing being packed into and is put into the decline furnace placed vertically vertically, and setting temperature rises to molten
10-100 DEG C on point, heat preservation for 24 hours, carries out fully melt.
2.2 crystal growths: then the bottom temp of silica crucible is controlled 20-50 DEG C on fusing point, then with 0.5-20mm/
The even speed of h declines silica crucible in crucible decline furnace, until being completely solidified into solid.Stop decline, then with 10-
The cooling rate of 100 DEG C/h makes crucible decline furnace be down to room temperature.
2.3 obtain crystal: finally, operating in glove box, taking out the RbY prepared in silica crucible2Cl7: the sudden strain of a muscle of Ce
Bright crystal.
2.4 RbY2Cl7: the scintillation properties test and analysis of Ce
Excitation of X-rays emission spectrum is tested using excitation of X-rays emission spectrometer is voluntarily built, is sharp with tungsten target X-ray tube
Light emitting source, photomultiplier tube carry out detector transmitting light.Fig. 5 is RbY2Cl7: the excitation of X-rays emission spectrum of Ce crystal, entire light
It is in symmetrical structure than wider luminous zone that spectrum has one in the wave-length coverage of 300-600nm, and the position of peak value is 410nm left
It is right.It is almost consistent with the photoluminescence emission wavelength under ultraviolet lamp excitation, it can match well with light emitting diode.
2.5 RbY2Cl7: the growth characteristics of Ce crystal
The polycrystal material that above-mentioned high temperature process heat obtains is gone out into RbY by Bridgman-Stockbarge method for growing2Cl7: Ce monocrystalline.Fig. 6 is crystalline substance
Body takes out the picture of silica crucible from decline furnace, and the upper end of the crucible crystal is fog-like opaque, due in single crystal growth process
Impurities removal process and growth course in technique influence, intermediate shouldering part can be seen that transparent do not crack is about 15
The transparent single crystal of mm.The portion of monocrystalline is taken out from crucible, polishes to obtain 10 mm of φ × 10mm cylinder by cutting and grinding
The monocrystalline of the transparent no cracking of body.Illustrate, the crystal structure and growth technique of the crystal can be easier to grow transparent big list
Crystalline substance, more preferably as scintillation crystal performance.
Comparative test
CsY2Cl7: Ce and RbY2Cl7: it is the water imbibition of Ce crystal, water-disintegrable
Crystal is put can occur moisture absorption phenomenon in air, and Fig. 7 is CsY at room temperature2Cl7: the moisture absorption process of Ce crystal, indoor humidity
Index is 50%, and temperature is 25 DEG C, and by crystal, from glove box, taking-up is as shown in (a) in Fig. 7, transparent state, with the time
Passage, there is white mist to crystal in devitrification, surface gradually, and crystal such as (b) in Fig. 7 is shown after 5 h, and surface is translucent,
Shape changes.
In order to further consider CsY2Cl7: Ce and RbY2Cl7: the water imbibition of Ce crystal uses LaBr3Crystal is done pair with it
Than.Fig. 8 is the moisture absorption comparison diagram of each crystal, increases coefficient using gravimetric method test moisture, quantitatively can probe into crystal
Water imbibition.Curve CsY in figure2Cl7: Ce, RbY2Cl7: Ce, LaBr3: Ce crystal is under the conditions of room temperature, humidity 50% in 5 hours
Water suction variation, LaBr3:Ce crystal easily make moist, and water imbibition is CsY2Cl7: 5.3 times of Ce crystal, RbY2Cl7: Ce crystal
Water imbibition is CsY2Cl7: 1.4 times of Ce crystal, CsY2Cl7: Ce crystal is least sensitive to water, it is possible to reduce encapsulates in detector
The cost of technology has preferably practicability.
In recent years, although Cs2LiYCl6The quality and size of crystal are greatly improved, but due to the water suction of its height
Property and hygroscopy, make the test to the crystal and using there is very big difficulty, cause now also almost without researcher to this
The transmission and absorption spectrum of crystal are tested, and cell parameter also lacks measured data.However CsY2Cl7: this crystalloid of Ce, I
All it has been carried out through absorption spectrum test, also calculated the data such as his relatively accurate cell parameter, also further
It demonstrates, the scintillation crystal of such rare earth element cerium dopping reduces the cost of encapsulation technology in detector, has more practical valence
Value.
Above description is not limitation of the present invention, and the present invention is also not limited to the example above.The art it is common
Within the essential scope of the present invention, the variations, modifications, additions or substitutions made also should belong to protection of the invention to technical staff
Range.
Claims (2)
1. a kind of scintillation crystal of rare earth element cerium dopping, it is characterised in that its chemical structural formula are as follows: MY2X7: Ce, wherein M=K,
Cs, Rb；X=Cl, Br.
2. a kind of preparation method of the scintillation crystal of rare earth element cerium dopping described in claim 1, it is characterised in that including with
Lower step:
(1) MY2X7: Ce Material synthesis
A. prepared by high pure raw material: by lower purity feedstock MX, CeX3And YX3Raw material is respectively charged into large scale silica crucible, using true
Sky pump vacuumizes it, and in vacuum, silica crucible is transferred in tube furnace, and it is small to be heated to 250 DEG C of heat preservations 2
When；Tube sealing operation is then carried out to it makes that silica crucible is fitted into crucible decline furnace for anhydrous and oxygen-free atmosphere in silica crucible,
Temperature is elevated above 50 DEG C -150 DEG C of material fusing point in silica crucible, heat preservation for 24 hours, is sufficiently melted, then with 6-20mm/
The decrease speed of day slowly decline until dropping distance reach crystal length in silica crucible, respectively obtain high-purity MX, CeX3With
YX3Raw material；
B. anhydrous MY is prepared2X7: Ce polycrystal material: operating in glove box, anhydrous MX, the CeX that will be prepared3And YX3Raw material massage
You compare MX:YX3: CeX3 The ratio of=1:2:0.001 weighs, and is fitted into clean ceramic mortar, and grinds 1 hour, is uniformly mixed
Post package is then to vacuumize in funnelform silica crucible and be heated to 250 DEG C of heat preservations 2 hours, seal silica crucible in bottom,
It is put into tube furnace, is heated above 50 DEG C -150 DEG C of material fusing point in silica crucible, after keeping the temperature 12-72h, with 50-150 DEG C/h
Speed be slowly dropped to room temperature, obtain anhydrous MY2X7: Ce polycrystal material；
(2) MY2X7: the growth of Ce crystal
Contain anhydrous MY for what step (1) obtained2X7: the silica crucible of Ce polycrystal material is put into vertically arranged crucible decline vertically
Temperature is elevated above in silica crucible after 10-100 DEG C of material fusing point by furnace, after heat preservation for 24 hours, by the bottom temp of silica crucible
Control is being higher than in silica crucible after 20-50 DEG C of material fusing point, then is making silica crucible in earthenware with the even speed of 0.5-20mm/h
Decline in crucible decline furnace, until being completely solidified into solid, stops decline, then decline crucible with the cooling rate of 10-100 DEG C/h
Furnace is down to room temperature to get the scintillation crystal of rare earth element cerium dopping, chemical structural formula are as follows: MY is arrived2X7: Ce, wherein M=K, Cs,
Rb；X=Cl, Br.
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| CN113337888A (en) * | 2021-05-20 | 2021-09-03 | 中国科学院上海光学精密机械研究所 | Preparation method of cerium antimonide single crystal |
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