CN114232094A - Uranium-doped bismuth silicate scintillation crystal and preparation method thereof - Google Patents

Uranium-doped bismuth silicate scintillation crystal and preparation method thereof Download PDF

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CN114232094A
CN114232094A CN202111640665.5A CN202111640665A CN114232094A CN 114232094 A CN114232094 A CN 114232094A CN 202111640665 A CN202111640665 A CN 202111640665A CN 114232094 A CN114232094 A CN 114232094A
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crystal
uranium
doped
bismuth silicate
crucible
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徐家跃
田甜
张炎
潘芸芳
李志超
张彦
申慧
马云峰
陈媛芝
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Shanghai Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/34—Silicates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
    • G01T1/2023—Selection of materials

Abstract

The invention belongs to the technical field of crystal growth, and discloses a uranium-doped bismuth silicate scintillation crystal and a preparation method thereof. Is characterized in that: (1) the bismuth silicate scintillation crystal is a scintillation material, and uranium ions are UO2The form is doped, the light output of the crystal can be obviously improved, the doping amount is 0.01-1 mol%, and the molecular formula of the bismuth silicate crystal is Bi4Si3O12(ii) a (2) Selecting high-purity SiO2、Bi2O3Preparing Bi from raw materials according to a stoichiometric ratio by a solid-phase sintering method4Si3O12Polycrystalline material, then Bi is added according to the doping amount4Si3O12Adding UO into polycrystalline material2Mixing all togetherHomogenizing and sintering to obtain uranium doped Bi4Si3O12Polycrystalline materials; (3) selecting bismuth silicate seed crystals, fixing the seed crystals at a seed well at the bottom of a crucible, filling a doped polycrystalline material into the crucible, sealing the crucible, moving the crucible into a ceramic tube, placing the crucible into a zone melting furnace, raising the temperature, preserving the temperature, inoculating the seed crystals, and then descending the seed crystals at a certain speed to grow to obtain the uranium-doped high-light-output bismuth silicate scintillation crystals.

Description

Uranium-doped bismuth silicate scintillation crystal and preparation method thereof
Technical Field
The invention belongs to the technical field of crystal growth, and particularly discloses a uranium-doped bismuth silicate scintillation crystal and a preparation method thereof.
Background
The scintillation crystal is a functional material crystal capable of absorbing high-energy particles or rays and emitting scintillation light, is generally used for detecting X rays, gamma rays and high-energy particles, and has wide application in the fields of high-energy physics, medical imaging, safety inspection, geological exploration and the like. At present, inorganic scintillation crystals are various in variety, and mainly comprise sodium iodide (NaI: Tl), cesium iodide (CsI: Tl) and bismuth germanate (Bi)4Ge3O12) Lutetium silicate (Lu)2SiO5Ce), lead tungstate (PbWO)4) And the like. The Bismuth Germanate (BGO) crystal has low melting point and excellent scintillation property, is a scintillation crystal material with excellent comprehensive performance, and is widely applied to the fields of large-scale electromagnetic energy devices, X-ray tomography (XCT), Positron Emission Tomography (PET) and the like. However, BGO crystals have a long decay time and a low radiation hardness, especially GeO2The raw materials are expensive, and the wider application of BGO crystals is limited by the problems, so people look to the Bismuth Silicate (BSO) crystals.
BSO scintillation crystal is Bi2O3-SiO2Near one in a pseudobinary systemThe melting compound and the BGO crystal belong to a cubic crystal system, have similar melting points and slightly lower density, and have basic conditions for being used as scintillation crystals. Studies have shown that the decay time of BSO crystals (100ns) is short, being only 1/3 for BGO; the radiation damage resistance is better than BGO; its raw material (SiO)2) The cost is low, so that the BSO crystal is expected to replace BGO crystal in certain application fields. Besides, the BSO scintillation crystal has both Cherenkov and scintillation properties, and has been deeply researched and applied in dual readout energy meters, and the properties of the BSO scintillation crystal are superior to those of BGO and PbWO4And others. However, BSO crystals also have certain problems, particularly with low light output, only 20% of BGO. In order to improve the light output of the BSO crystal, a rare earth element doping test is carried out, and the fact that the light output of the BSO crystal can be improved by 1.5 times by trace Dy doped BSO crystal is found. For transition metal doping, it was found that Ta doping can increase the light output of BSO crystals, with an optimum doping level of 1 mol%. To date, no report has been made on the improvement of the light output of BSO crystals by actinides. UO2Ceramics are important nuclear fuel materials, UO2The crystal is a semiconductor and a topological insulator, and has potential application in the fields of photovoltaics, thermoelectricity and the like. The invention provides a through UO2A new method for improving the light output of the BSO crystal by doping and a technical approach for growing the doped BSO crystal by a region melting method are provided.
The BSO crystal growth method includes a Czochralski method, a Bridgman-Stockbarge method and the like. In Bi2O3-SiO2In the pseudo-binary phase diagram, due to Bi2O3And SiO2The density and the melting point of the crystal are greatly different, the phase system is complex, and the composition segregation is easy to generate in the crystal growth process, so that the crystal defect and even the growth failure are caused. Although the Czochralski method can grow BSO crystals, the crystal size is not large and the quality is not high; the Bridgman method is the primary growth method for BSO crystals. But the component separation is serious in the later growth stage of the descent method, which not only wastes raw materials, but also is not beneficial to the improvement of the crystal quality.
Disclosure of Invention
The invention aims to provide a method for improving the scintillation property and the crystal growth of a bismuth silicate crystal, which aims to solve the problems of low light output, difficult control of crystal growth and the like of the crystal.
In order to achieve the purpose, the technical scheme of the invention is as follows: uranium-doped bismuth silicate scintillation crystal doped with U4+，U4+With UO2The doping amount is 0.01-1 mol%, and the molecular formula of the bismuth silicate crystal is Bi4Si3O12。
Further, UO2The doping amount was 0.5 mol%. The light output reaches the maximum value at the doping amount
Further, a preparation method of the uranium-doped bismuth silicate scintillation crystal comprises the following steps:
(1) selecting high-purity SiO2、Bi2O3Raw materials are proportioned according to the stoichiometric ratio and sintered for 6 to 15 hours at the temperature of 750 to 850 ℃ by adopting a solid-phase sintering method to obtain Bi4Si3O12Polycrystalline materials; according to the doping amount to Bi4Si3O12Adding UO into polycrystalline material2Grinding and mixing uniformly, and sintering at the temperature of 850 ℃ for 5-10 h to obtain uranium-doped Bi4Si3O12Polycrystalline materials;
(2) selecting bismuth silicate seed crystal, fixing the seed crystal at the seed well part at the bottom of the crucible, and filling the synthesized doped polycrystalline material with Bi fixed therein4Si3O12Sealing the crucible of the seed crystal, and moving the crucible into a position with a proper height in the ceramic tube;
(3) heating the crystal furnace to 1050-1200 ℃ within 12-20 h, and preserving heat for 4-12 h; gradually lifting the ceramic tube, melting the polycrystalline material in a certain area at the upper part of the seed crystal to form a stable melting area, then inoculating, and preserving heat for 1-3 h;
(4) and (3) descending and moving the ceramic tube at the speed of 0.2-0.6 mm/h, carrying out crystal growth, cooling to room temperature, and then stripping the crucible to obtain the uranium-doped bismuth silicate scintillation crystal with high light output.
Further, the optimal orientation of the BSO seed is <001 >; the cross section of the seed crystal is round, rectangular, square or required.
Further, the platinum crucible in the step (2) has the thickness of 0.1-0.3mm, is columnar, is provided with a seed well at the bottom for placing seed crystals, and is sealed by a cover.
Further, a crucible used in crystal growth is a platinum crucible, the wall thickness of the crucible is 0.10-0.2 mm, and the crucible is cylindrical, rectangular, square or wedge-shaped.
Furthermore, a plurality of equivalent stations are arranged in the crystal furnace body, and more than two crystals can grow simultaneously.
The technical scheme of the invention has the working principle and the beneficial effects that:
the invention is intended to pass through UO2Doping increases the light output of the BSO crystal. It is believed that the use of rare earth doping can improve the luminous efficiency of the crystal. However, in BGO and BSO crystals, doping does not find improvement in the light output of the crystal, and conversely doping rare earth ions more readily introduces new luminescence centers. We have found that the light output of BSO crystal can be increased to 1.5 times by the trace doping of individual rare earth elements. We therefore associate what effect actinide doping will have on BSO crystal light output? We predict UO by first-principles calculations and extensive experimentation2The doping can obviously improve the light output of the crystal, but the light-emitting center is still Bi ions, so the decay time is unchanged. The zone melting growth process provided by the invention can inhibit component separation and is beneficial to the uniformity of dopants in the crystal, and the process is a practical BSO crystal growth method.
The invention provides a zone melting growth process for inhibiting component separation by controlling a melting interval. Controlling the proper melt zone height according to the melt characteristics, on one hand, inhibits the volatilization and separation of components, and on the other hand, helps the uniformity of dopants in the crystal, and is a practical BSO crystal growth method.
Drawings
FIG. 1 shows uranium-doped BSO crystals of different concentrations grown by the method of the present invention;
FIG. 2 is 0.05 mol% UO2Doped BSO single crystal X-ray diffraction spectrum.
Detailed Description
The following is further detailed by way of specific embodiments:
a uranium-doped bismuth silicate scintillation crystal is characterized in that the bismuth silicate crystal is doped with U4+，U4+With UO2The doping amount is 0.01-1 mol%, and the molecular formula of the bismuth silicate crystal is Bi4Si3O12. In this example, UO2The doping amount is preferably 0.5 mol%.
FIG. 1 shows uranium-doped BSO crystals of different concentrations grown by the method of the present invention;
FIG. 2 is 0.05 mol% UO2Doped BSO single crystal X-ray diffraction spectrum.
Example 1
A uranium-doped bismuth silicate scintillation crystal and a preparation method thereof comprise the following steps:
4N purity SiO2、Bi2O3Raw materials are weighed and proportioned according to the stoichiometric ratio, ground and uniformly mixed, and sintered for 8 hours at 820 ℃ to obtain Bi4Si3O12Polycrystalline materials; 0.1 mol% of UO was added2Grinding and mixing uniformly, putting into a columnar Pt crucible with seed crystals, melting, inoculating and growing at 1150 ℃ in a zone-melting furnace, wherein the height of a melting zone is 70mm, the growth rate is 0.5mm/h, cooling to room temperature after the growth is finished, and then stripping off the crucible to obtain the cylindrical uranium-doped bismuth silicate crystal with high light output.
Example 2
A preparation method of a uranium-doped bismuth silicate scintillation crystal comprises the following steps:
4N purity SiO2、Bi2O3The raw materials are weighed and proportioned according to the stoichiometric ratio, ground and mixed uniformly, and sintered for 12 hours at 800 ℃ to obtain Bi4Si3O12Polycrystalline materials; 1 mol% of UO was added2Grinding and mixing uniformly, putting the mixture into a columnar Pt crucible with seed crystals, wherein the thickness of the crucible is 0.2mm, placing the crucible into a ceramic tube, moving the crucible into a zone furnace at a proper height, setting the temperature at 1150 ℃, controlling the melting zone at 40mm, raising the temperature, melting materials, inoculating and growing at the growth rate of 0.2mm/h, cooling to room temperature after the growth is finished, and then stripping the crucible to obtain the uranium-doped bismuth silicate crystal with high light output.
Example 3
A preparation method of a uranium-doped bismuth silicate scintillation crystal comprises the following steps:
4N purity SiO2、Bi2O3The raw materials are weighed and proportioned according to the stoichiometric ratio, ground and uniformly mixed, and sintered for 10 hours at 815 ℃ to obtain Bi4Si3O12Polycrystalline materials; 0.5 mol% of UO was added2Grinding and mixing uniformly, putting the mixture into a square Pt crucible with seed crystals, wherein the thickness of the crucible is 0.2mm, melting, inoculating and growing at 1150 ℃ in a zone-melting furnace, the height of a melting zone is 60mm, the growth rate is 0.3mm/h, cooling to room temperature after the growth is finished, and then stripping the crucible to obtain the uranium-doped square bismuth silicate crystal with high light output.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.

Claims (6)

1. A uranium-doped bismuth silicate scintillation crystal is characterized in that the bismuth silicate crystal is doped with U4+，U4+With UO2The doping amount is 0.01-1 mol%, and the molecular formula of the bismuth silicate crystal is Bi4Si3O12。
2. A uranium doped bismuth silicate scintillation crystal according to claim 1, characterized in that UO2The doping amount was 0.5 mol%.
3. A method of preparing a uranium doped bismuth silicate scintillation crystal according to any one of claims 1-2, characterized by comprising the steps of:
1) selecting high-purity SiO2、Bi2O3The raw materials are proportioned according to the stoichiometric ratio, a solid-phase sintering method is adopted,sintering at 750-850 ℃ for 6-15 hours to obtain Bi4Si3O12Polycrystalline materials; according to the doping amount to Bi4Si3O12Adding UO into polycrystalline material2Grinding and mixing uniformly, and sintering at the temperature of 850 ℃ for 5-10 h to obtain uranium-doped Bi4Si3O12Polycrystalline materials;
2) selecting bismuth silicate seed crystal, fixing the seed crystal at the seed well part at the bottom of the crucible, and filling the synthesized doped polycrystalline material with Bi fixed therein4Si3O12Sealing the crucible of the seed crystal, and moving the crucible into a position with a proper height in the ceramic tube;
3) heating the crystal furnace to 1050-1200 ℃ within 12-20 h, and preserving heat for 4-12 h; gradually lifting the ceramic tube, inoculating after the polycrystalline material in a certain area at the upper part of the seed crystal is melted, and preserving the temperature for 1-3 h;
4) and (3) descending and moving the ceramic tube or the heating body at the speed of 0.2-0.6 mm/h to perform crystal growth, so as to obtain the uranium-doped bismuth silicate scintillation crystal with high light output.
4. A method for preparing a uranium doped bismuth silicate scintillation crystal according to claim 3, wherein the optimal orientation of the BSO seed crystal is <001 >; the cross section of the seed crystal is round, rectangular, square or required.
5. A uranium-doped bismuth silicate scintillation crystal according to claim 3, wherein the crucible used for crystal growth is a platinum crucible, the crucible wall thickness is 0.10-0.2 mm, and the crucible is cylindrical, rectangular, square or wedge-shaped.
6. The method for preparing a uranium-doped bismuth silicate scintillation crystal according to claim 3, wherein the method comprises the following steps: a plurality of equivalent stations are arranged in the crystal furnace body, and more than two crystals can grow simultaneously.
CN202111640665.5A 2021-12-29 2021-12-29 Uranium-doped bismuth silicate scintillation crystal and preparation method thereof Pending CN114232094A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1540818A (en) * 2003-10-28 2004-10-27 中国科学院上海光学精密机械研究所 Self modulated laser crystal and preparation method
CN103643293A (en) * 2013-12-25 2014-03-19 中国科学院上海硅酸盐研究所 Bismuth silicate scintillation crystal as well as preparation method and application thereof
CN104562205A (en) * 2015-01-28 2015-04-29 中国科学院上海硅酸盐研究所 Anion-cation co-doped bismuth silicate scintillation crystal and preparation method thereof
CN106948006A (en) * 2017-02-28 2017-07-14 上海应用技术大学 A kind of High Light Output Bismuth silicate scintillation crystal and preparation method thereof
CN107163938A (en) * 2017-05-24 2017-09-15 上海应用技术大学 A kind of Ho doping bismuth silicate green emitting phosphor and preparation method thereof
CN107268086A (en) * 2016-04-06 2017-10-20 中国科学院上海硅酸盐研究所 A kind of method for improving Bismuth silicate scintillation crystal near ultraviolet band transmitance
CN108384532A (en) * 2018-03-28 2018-08-10 苏州大学 Application containing uranium compound as scintillator
CN113403685A (en) * 2021-06-11 2021-09-17 上海应用技术大学 Single-doped uranium lithium niobate crystal and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1540818A (en) * 2003-10-28 2004-10-27 中国科学院上海光学精密机械研究所 Self modulated laser crystal and preparation method
CN103643293A (en) * 2013-12-25 2014-03-19 中国科学院上海硅酸盐研究所 Bismuth silicate scintillation crystal as well as preparation method and application thereof
CN104562205A (en) * 2015-01-28 2015-04-29 中国科学院上海硅酸盐研究所 Anion-cation co-doped bismuth silicate scintillation crystal and preparation method thereof
CN107268086A (en) * 2016-04-06 2017-10-20 中国科学院上海硅酸盐研究所 A kind of method for improving Bismuth silicate scintillation crystal near ultraviolet band transmitance
CN106948006A (en) * 2017-02-28 2017-07-14 上海应用技术大学 A kind of High Light Output Bismuth silicate scintillation crystal and preparation method thereof
CN107163938A (en) * 2017-05-24 2017-09-15 上海应用技术大学 A kind of Ho doping bismuth silicate green emitting phosphor and preparation method thereof
CN108384532A (en) * 2018-03-28 2018-08-10 苏州大学 Application containing uranium compound as scintillator
CN113403685A (en) * 2021-06-11 2021-09-17 上海应用技术大学 Single-doped uranium lithium niobate crystal and preparation method thereof

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