CN110734223B - Lutetium-doped silicate scintillation glass and preparation method thereof - Google Patents
Lutetium-doped silicate scintillation glass and preparation method thereof Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 77
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims abstract description 5
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical group [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000000156 glass melt Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 16
- 238000000137 annealing Methods 0.000 claims description 14
- 229910052593 corundum Inorganic materials 0.000 claims description 14
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 claims 4
- 229910052765 Lutetium Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract description 2
- 238000002059 diagnostic imaging Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000012633 nuclear imaging Methods 0.000 description 2
- 229910003016 Lu2SiO5 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention provides lutetium-doped silicate scintillation glass and a preparation method thereof, and the lutetium group is introduced and the process conditions are controlled, so that the prepared scintillation glass has the advantages of high luminous efficiency, high attenuation speed, high density, strong ray blocking performance and the like, the light yield can reach 27000, and the density can reach 6.5-7.5 g/cm3The glass is obviously higher than the existing scintillating glass, has high mechanical strength, stable chemical property, difficult deliquescence and excellent comprehensive performance, and is suitable for being applied to the fields of petroleum exploration, radiation medical imaging, industrial on-line detection, national security supervision, high-energy physical or nuclear physical experiments and the like; meanwhile, the scheme selects conventional components for precise proportioning, adopts conventional equipment and an improved process method, is simple and easy to prepare, can effectively reduce the cost while ensuring the performance of the glass, can provide the scintillation glass with excellent performance by using limited resources, and is more suitable for expanded production and application.
Description
Technical Field
The invention belongs to the technical field of scintillation materials, and particularly relates to lutetium-doped silicate scintillation glass and a preparation method thereof.
Background
At present, the rapid development and requirement of nuclear imaging technology provides a wide space for the research of novel scintillating materials. The scintillation glass as one of special glass is expected to replace scintillation crystals, and the nuclear imaging technology is promoted to be widely applied in the aspects of image medicine, high-energy physics, safety detection, mineral resource exploration and the like in a spanning way, so that a huge international market is formed, and the scintillation glass becomes one of hot spots and important leading directions of new material research and application.
Among the numerous methods for preparing glass bodies available, the fusion method has been the focus of research because of the following advantages: (1) the process is simple, and different glass shapes can be easily made; (2) the chemical uniformity of the multicomponent system can be improved to the atomic or molecular level; (3) the amount and kind of the doping component are wide, the stoichiometry is accurate and the modification is easy. In recent years, researchers at home and abroad are keenly concerned about preparing microcrystalline scintillation glass by using nano powder through a melting method, and find out a general rule in the preparation process of the microcrystalline scintillation glass to obtain scientific connotation in a process of spanning from nano to micron, which has great theoretical value in materials science. Meanwhile, because the crystal field of the active ions in the polycrystalline glass is different from that of the nano-particles and the single crystals, the basic problems of physical processes such as absorption and emission of the active ions under the condition of existence of crystal boundaries, an energy transfer process and a propagation mechanism of light in the polycrystalline glass and the like are explored, and the method has more important theoretical significance in solving the physical problems in the luminescence process of the scintillating ceramic.
In recent years, many studies on scintillating glass have been focused on LuAG, YAG, Lu2O3Equal material, but for hot Lu2SiO5Ce and Lu2Si2O7The improvement of scintillation crystals such as Ce is rarely reported. The preparation of the scintillation glass needs higher preparation technology and excellent equipment, and faces the same problem of raw materials as many domestic material industries. The purity of raw materials and the particle size of raw material nano powder have higher requirements, and no special enterprise can provide at present at home; meanwhile, the difference between domestic equipment with high sintering temperature and high vacuum degree and foreign equipment is more obvious, and the problems become a bottleneck for restricting the development of the scintillation glass. Therefore, how to provide a scintillation glass with excellent performance by using limited resources and innovative process methods (fine adjustment of components and temperature of heat treatment) is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides lutetium-doped silicate scintillation glass and a preparation method thereof.
The specific technical scheme of the invention is as follows:
in one aspect, the invention provides lutetium-doped silicate scintillatorsThe glass comprises the following components in percentage by mole: SiO2 2 50～60％、H3BO3 12～15％、NaNO3 4～7％、Lu2O3 15～20％、Ce(C2O4)2 1～2％、MgF2 0.5～1％、Al2O3 4～5％、BaCO3 1.5～2％。
Further, the lutetium-doped silicate scintillation glass comprises the following components in percentage by mole: SiO2255.33％、H3BO3 13.84％、NaNO3 5.53％、Lu2O3 16.46％、Ce(C2O4)2 1.43％、MgF2 0.95％、Al2O3 4.61％、BaCO3 1.84％。
The invention also provides a method for preparing the lutetium-doped silicate scintillation glass, which comprises the following steps:
s1: accurately weighing the components and uniformly mixing to obtain a first mixture;
s2: heating the first mixture in a corundum crucible, and melting the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the model in a muffle furnace for annealing, closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: and cutting, grinding and polishing the surface of the scintillation glass primary product to obtain the lutetium-doped silicate scintillation glass.
Further, in step S2, the melting conditions are as follows:
the heating temperature is 1700 ℃, and the time is 180 min.
Further, in step S3, the annealing conditions are as follows:
the temperature is preserved for 4 hours at 700-800 ℃, and then the temperature is reduced to 300-400 ℃ at the speed of 50 ℃/h.
The invention also provides application of the lutetium-doped silicate scintillation glass in X-ray detection.
Hair brushThe beneficial effects are as follows: the invention provides lutetium-doped silicate scintillation glass and a preparation method thereof, and the lutetium group is introduced and the process conditions are controlled, so that the prepared scintillation glass has the advantages of high luminous efficiency, high attenuation speed, high density, strong ray blocking performance and the like, the light yield can reach 27000, and the density can reach 6.5-7.5 g/cm3The glass is obviously higher than the existing scintillating glass, has high mechanical strength, stable chemical property, difficult deliquescence and excellent comprehensive performance, and is suitable for being applied to the fields of petroleum exploration, radiation medical imaging, industrial on-line detection, national security supervision, high-energy physical or nuclear physical experiments and the like; meanwhile, the scheme selects conventional components for precise proportioning, adopts conventional equipment and an improved process method, is simple and easy to prepare, can effectively reduce the cost while ensuring the performance of the glass, can provide the scintillation glass with excellent performance by using limited resources, and is more suitable for expanded production and application.
Drawings
FIG. 1 is an X-ray diffraction pattern of a scintillating glass provided herein, when heat treated at 900 ℃;
FIG. 2 is an X-ray diffraction pattern of a scintillating glass provided herein, when heat treated at 1000 ℃;
FIG. 3 is an absorption spectrum of scintillation glass subjected to heat treatment at 1000 ℃ under excitation of violet light;
FIG. 4 is a graph showing the emission spectrum of a scintillating glass subjected to a heat treatment at 1000 ℃ under excitation of violet light.
Detailed Description
Unless otherwise indicated, implied from the context, or customary in the art, the testing and characterization methods used are synchronized to the filing date of the present application. Where applicable, the contents of any patent, patent application, or publication referred to in this application are hereby incorporated by reference in their entirety, and the equivalent family of patents is also incorporated by reference, especially with respect to the definitions of those documents disclosed in the art with respect to synthetic techniques, products, and process designs, etc. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
The present invention will be described in further detail with reference to the following examples and drawings.
Example 1
A lutetium-doped silicate scintillation glass comprises the following components in percentage by mole: SiO2 2 50％、H3BO315％、NaNO3 7％、Lu2O3 20％、Ce(C2O4)2 2％、MgF2 0.5％、Al2O3 5％、BaCO31.5 percent. The scintillation glass is prepared by the following method:
s1: accurately weighing the components according to the proportion and uniformly mixing to obtain a first mixture;
s2: placing the first mixture in a corundum crucible, and heating at 1700 ℃ for 180min to melt the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the uniform glass melt in a muffle furnace for annealing, firstly placing the uniform glass melt at 700 ℃ for heat preservation for 4h, and then cooling to 300 ℃ at the speed of 50 ℃/h; closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: and cutting, grinding and polishing the surface of the scintillation glass primary product to obtain the lutetium-doped silicate scintillation glass.
Example 2
A lutetium-doped silicate scintillation glass comprises the following components in percentage by mole: SiO22 60％、H3BO312％、NaNO3 4％、Lu2O3 15％、Ce(C2O4)2 1％、MgF2 1％、Al2O3 4％、BaCO32 percent. The scintillation glass is prepared by the following method:
s1: accurately weighing the components according to the proportion and uniformly mixing to obtain a first mixture;
s2: placing the first mixture in a corundum crucible, and heating at 1700 ℃ for 180min to melt the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the uniform glass melt in a muffle furnace for annealing, firstly placing the uniform glass melt at 800 ℃ for heat preservation for 4 hours, and then cooling to 400 ℃ at the speed of 50 ℃/h; closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: and cutting, grinding and polishing the surface of the scintillation glass primary product to obtain the lutetium-doped silicate scintillation glass.
Example 3
A lutetium-doped silicate scintillation glass comprises the following components in percentage by mole: SiO22 55.33％、H3BO313.84％、NaNO3 5.53％、Lu2O3 16.46％、Ce(C2O4)2 1.43％、MgF2 0.95％、Al2O3 4.61％、BaCO31.84 percent. The scintillation glass is prepared by the following method:
s1: accurately weighing the components according to the proportion and uniformly mixing to obtain a first mixture;
s2: placing the first mixture in a corundum crucible, and heating at 1700 ℃ for 180min to melt the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the uniform glass melt in a muffle furnace for annealing, firstly placing the uniform glass melt at 700 ℃ for heat preservation for 4h, and then cooling to 300 ℃ at the speed of 50 ℃/h; closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: and cutting, grinding and polishing the surface of the scintillation glass primary product to obtain the lutetium-doped silicate scintillation glass.
Example 4
A lutetium-doped silicate scintillation glass comprises the following components in percentage by mole: SiO22 55.33％、H3BO313.84％、NaNO3 5.53％、Lu2O3 16.46％、Ce(C2O4)2 1.43％、MgF2 0.95％、Al2O3 4.61％、BaCO31.84 percent. The scintillation glass is prepared by the following method:
s1: accurately weighing the components according to the proportion and uniformly mixing to obtain a first mixture;
s2: placing the first mixture in a corundum crucible, and heating at 1700 ℃ for 180min to melt the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the uniform glass melt in a muffle furnace for annealing, firstly placing the uniform glass melt at 800 ℃ for heat preservation for 4 hours, and then cooling to 400 ℃ at the speed of 50 ℃/h; closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: and cutting, grinding and polishing the surface of the scintillation glass primary product to obtain the lutetium-doped silicate scintillation glass.
Test examples X-ray excitation test
When the scintillation glass prepared in experimental example 4 was subjected to heat treatment at 900 ℃ and 1000 ℃, respectively, it was found from the X-ray diffraction patterns (fig. 1 and 2) that a high intensity peak was generated at 26 ° upon heat treatment at 1000 ℃, indicating that nanocrystalline particles having a scintillation effect were generated at this point upon heat treatment; the peak is not generated when the heat treatment is carried out at 900 ℃, which shows that the heat treatment effect at 1000 ℃ is obviously better than 900 ℃.
The scintillation glass after the heat treatment at 1000 ℃ is irradiated with purple light, and the absorption spectrum (figure 3) and the emission spectrum (figure 4) show that the scintillation glass can effectively absorb the purple light and release red light, and the light yield can reach 27000Photon/MeV through calculation, which is obviously higher than that of the existing scintillation glass.
In addition, through measurement, the density of the scintillation glass prepared by the method provided by the application can reach 6.5-7.5 g/cm3And is also obviously higher than the prior scintillation glass. Therefore, the scintillation glass provided by the application has the advantages of high density, high luminous intensity and excellent comprehensive performance, and is suitable for wide application.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A lutetium-doped silicate scintillation glass is characterized by comprising the following components in percentage by mol: SiO22 50～60％、H3BO3 12～15％、NaNO3 4～7％、Lu2O3 15～20％、Ce(C2O4)2 1～2％、MgF2 0.5～1％、Al2O34～5％、BaCO3 1.5～2％；
The method for doping lutetium-based silicate scintillation glass comprises the following steps:
s1: accurately weighing the components and uniformly mixing to obtain a first mixture;
s2: heating the first mixture in a corundum crucible, and melting the mixture into a uniform glass melt;
s3: pouring and molding the uniform glass melt in a model, placing the model in a muffle furnace for annealing, closing the muffle furnace after the annealing is finished, and automatically cooling to room temperature to obtain a scintillation glass primary product;
s4: cutting, grinding and polishing the surface of the scintillation glass initial product to obtain the lutetium-doped silicate scintillation glass;
in step S2, the melting conditions are as follows:
the heating temperature is 1700 ℃, and the time is 180 min. .
2. The lutetium-doped silicate scintillation glass of claim 1, comprising the following components in mole percent: SiO22 55.33％、H3BO3 13.84％、NaNO3 5.53％、Lu2O3 16.46％、Ce(C2O4)2 1.43％、MgF20.95％、Al2O3 4.61％、BaCO31.84％。
3. The lutetium-doped silicate scintillation glass of claim 1, comprising the following components in mole percent: 250% of SiO, 315% of H3BO, 37% of NaNO, 320% of Lu2O, 22% of Ce (C2O4), 20.5% of MgF20, 35% of Al2O and 31.5% of BaCO31.
4. The lutetium-doped silicate scintillation glass of claim 1, comprising the following components in mole percent: SiO 260%, H3BO 312%, NaNO 34%, Lu2O 315%, Ce (C2O4) 21%, MgF 21%, Al2O 34% and BaCO 32%.
5. A method of making the lutetium-doped silicate scintillation glass of any one of claims 1-4, comprising the steps of:
in step S3, the annealing conditions are as follows:
the temperature is preserved for 4 hours at 700-800 ℃, and then the temperature is reduced to 300-400 ℃ at the speed of 50 ℃/h.
6. Use of the lutetium-doped silicate scintillation glass of any one of claims 1 to 4 in X-ray detection.
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