CN113253332B - GOS-based: tb transparent ceramic scintillation screen high-resolution neutron imaging detector and manufacturing method thereof - Google Patents
GOS-based: tb transparent ceramic scintillation screen high-resolution neutron imaging detector and manufacturing method thereof Download PDFInfo
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 2
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- 229910003451 terbium oxide Inorganic materials 0.000 description 2
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
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- 229910052684 Cerium Inorganic materials 0.000 description 1
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- XAUTYMZTJWXZHZ-IGUOPLJTSA-K bismuth;(e)-1-n'-[2-[[5-[(dimethylamino)methyl]furan-2-yl]methylsulfanyl]ethyl]-1-n-methyl-2-nitroethene-1,1-diamine;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Bi+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-][N+](=O)\C=C(/NC)NCCSCC1=CC=C(CN(C)C)O1 XAUTYMZTJWXZHZ-IGUOPLJTSA-K 0.000 description 1
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- JAOZQVJVXQKQAD-UHFFFAOYSA-K gadolinium(3+);phosphate Chemical compound [Gd+3].[O-]P([O-])([O-])=O JAOZQVJVXQKQAD-UHFFFAOYSA-K 0.000 description 1
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 description 1
- ILCLBMDYDXDUJO-UHFFFAOYSA-K gadolinium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Gd+3] ILCLBMDYDXDUJO-UHFFFAOYSA-K 0.000 description 1
- QLAFITOLRQQGTE-UHFFFAOYSA-H gadolinium(3+);trisulfate Chemical compound [Gd+3].[Gd+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O QLAFITOLRQQGTE-UHFFFAOYSA-H 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
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- 239000001294 propane Substances 0.000 description 1
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- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
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- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- QQCIBICIISNSAY-UHFFFAOYSA-K terbium(3+);phosphate Chemical compound [Tb+3].[O-]P([O-])([O-])=O QQCIBICIISNSAY-UHFFFAOYSA-K 0.000 description 1
- LMEHHJBYKPTNLM-UHFFFAOYSA-H terbium(3+);tricarbonate Chemical compound [Tb+3].[Tb+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O LMEHHJBYKPTNLM-UHFFFAOYSA-H 0.000 description 1
- YJVUGDIORBKPLC-UHFFFAOYSA-N terbium(3+);trinitrate Chemical compound [Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YJVUGDIORBKPLC-UHFFFAOYSA-N 0.000 description 1
- UFPWIQQSPQSOKM-UHFFFAOYSA-H terbium(3+);trisulfate Chemical compound [Tb+3].[Tb+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O UFPWIQQSPQSOKM-UHFFFAOYSA-H 0.000 description 1
- DIRSQPIRPNAECV-UHFFFAOYSA-N terbium;trihydrate Chemical compound O.O.O.[Tb] DIRSQPIRPNAECV-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T3/00—Measuring neutron radiation
- G01T3/06—Measuring neutron radiation with scintillation detectors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
- C04B2235/662—Annealing after sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Abstract
A high-resolution neutron imaging detector based on a GOS-Tb transparent ceramic scintillation screen and a manufacturing method thereof. The high resolution neutron imaging detector includes: the GOS is Tb transparent ceramic scintillating screen and is used for absorbing neutrons and emitting scintillating light; the optical path system is used for collecting the scintillation light on the GOS Tb transparent ceramic scintillation screen and projecting the scintillation light onto the photosensitive element; and a photosensitive element for recording imaging information of neutrons by receiving the scintillation light and performing photoelectric conversion. Because the GOS-Tb transparent ceramic is of a transparent structure and has the thickness of micron level, the light spot size can be effectively reduced, the light output rate can be improved, and the micron-level spatial resolution can be realized.
Description
Technical Field
The invention relates to the field of neutron detectors, in particular to a high-resolution neutron imaging detector based on a GOS (gate oxide sensor) -Tb transparent ceramic scintillation screen and a manufacturing method thereof.
Background
Most of the traditional neutron imaging detectors use 6 LiF/ZnS scintillators. The light yield of such scintillators is highest among all neutron scintillators, which helps to shorten the exposure time of the detector. For high resolution neutron imaging detectors, however, 6 LiF/ZnS scintillators have several drawbacks that are difficult to overcome: firstly, the method comprises the following steps of 6 The LiF/ZnS scintillators are thicker and the thinnest available from UK AST and Switzerland RC Tritec are currently available 6 The LiF/ZnS scintillator thickness is 50 microns and the scintillation screen of this thickness is not spatially resolved on the order of microns. Second is neutronAt the position of 6 The scintillation spot size formed in LiF/ZnS scintillators is greater than 30 microns, which also limits 6 LiF/ZnS scintillators are difficult to achieve spatial resolution on the order of microns. Therefore, a search for a substitute for the above is required 6 A scintillator of LiF/ZnS material.
GOS Tb scintillator has high spatial resolution, can be used as a new generation scintillator substitute material, but has lower light yield and specific ratio 6 The LiF/ZnS: ag scintillator is two orders of magnitude lower. Ultra-thin Gd developed by the swiss national laboratory, pohsh institute (PSI) in 2015 2 O 2 The scintillator is formed by mixing GOS: tb powder with a particle size of about 3 micrometers and an adhesive, and coating and adhering the mixture on an aluminum substrate, and the thickness of the scintillator can be reduced to the micrometer level by adopting the process, so that the spatial resolution can be effectively improved. However, since the PSI is produced by painting the scintillator directly with GOS: tb particles (GOS: tb powder scintillator screen), the microstructure of the scintillator is still a granular structure, and thus the scintillator itself is opaque. When the neutron excited scintillation light propagates outwards, the scintillation light is scattered and absorbed by the particle boundaries, bubbles and defects of the scintillator, so that the light output is reduced, the light spot size is increased (as shown in fig. 1), the disadvantage of low light yield is further aggravated, and the advantages of the GOS-Tb scintillator cannot be fully exerted. Thus, the prior art has yet to be developed.
Disclosure of Invention
The invention aims to provide a high-resolution neutron imaging detector based on a GOS (gate oxide, source and sensor) Tb transparent ceramic scintillation screen and a manufacturing method thereof, and because the main structure in the GOS Tb transparent ceramic scintillation screen, namely the GOS Tb transparent ceramic is a transparent structure and has the thickness of micron level, and an optical imaging system is redesigned, the high-resolution neutron imaging detector can effectively reduce the light spot size and improve the light yield, thereby realizing micron-level spatial resolution. In this application, a high resolution neutron imaging detector refers to a micron-scale spatially resolved neutron imaging detector.
It should be noted that, although the technology of manufacturing the scintillation screen by adopting GOS: tb transparent ceramics is available in the field of medical imaging at present, the technology is applied to X-CT equipment for example. However, the difference between the method and the device is that firstly, the method and the device are different from the application field, and the GOS-Tb transparent ceramic scintillating screen is mainly applied to the field of micron-level high-resolution neutron imaging detection; secondly, the doped ions are different, in the application, the doped ions in the GOS transparent ceramic raw material are Tb, and the main doped ions in the GOS transparent ceramic raw material in the medical imaging field are Pr and Ce; thirdly, the size grades of the two are different, the size of the prepared GOS-Tb transparent ceramic is in a micron level, especially smaller than 30 mu m, and the GOS-Pr or GOS-Ce transparent ceramic applied in the medical imaging field is in a millimeter level, so that the material cannot be processed to the micron level due to the problem of self rigidity.
According to a first aspect, the present application provides a high resolution neutron imaging detector based on a GOS: tb transparent ceramic scintillating screen. As shown in fig. 2 or 5, the high-resolution neutron imaging detector (hereinafter referred to as a detector) mainly includes three core parts: scintillators (also known as scintillation screens, neutron scintillators), optical systems, and photosensitive elements. The scintillator is sensitive to the neutron, nuclear reaction can occur after the neutron hits the scintillator, and the scintillator emits scintillation light after absorbing the neutron; the optical path system collects the scintillation light and focuses and projects the scintillation light onto a chip of the photosensitive element; the scintillation light is converted into an electric signal by the photoelectric conversion action of the photosensitive element, and image information of neutrons is formed. The main factors affecting the spatial resolution of the detector include: scintillator thickness, the size of scintillation spot (spot formed on the scintillator after neutron incidence), imaging quality and optical magnification in the optical path system, and pixel size of the photosensitive element, etc. Therefore, to increase the spatial resolution of the detector, the present application makes the following improvements.
The spatial resolution of a high resolution neutron imaging detector is closely related to the size of the scintillation spot and the scintillator thickness, as shown in fig. 3, and in general, the detector intrinsic resolution is on the order of magnitude of the scintillation spot size and the scintillator thickness. The smaller the size of the scintillation spot, the thinner the scintillation screen thickness, and the higher the intrinsic resolution of the detector. Therefore, reducing the thickness of the scintillation screen and using a scintillation screen with smaller scintillation spots helps to improve spatial resolution.
The improvement points of the application are as follows: a GOS: tb transparent ceramic scintillator screen with a thickness in the order of micrometers was used as a scintillator. The GOS-Tb transparent ceramic scintillating screen has the advantages that the compact is high and the structure is transparent, so that the problems of large light spot size and low light output efficiency (low light yield) formed by the GOS-Tb powder scintillating screen in the prior art can be effectively solved; secondly, the thickness is set to be in a micron level (the conventional technology cannot directly prepare GOS: tb transparent ceramic into a micron level, and the micron level is usually in a millimeter level), the light loss is low, the light transmittance is high, the spatial resolution of the detector can be effectively improved, and the detector is particularly suitable for being applied to high-resolution neutron imaging detectors.
The GOS-Tb transparent ceramic scintillating screen is formed by sintering GOS-Tb powder. Because of the mechanical properties of GOS: tb transparent ceramics, it is not easy to directly process into dimensions down to the order of micrometers in thickness. The prior art discloses that GOS may be used: the Tb powder and the binder are mixed without sintering to form the scintillator, but the scintillator manufactured by the process has low transparency, so that the size of a scintillation light spot formed on an optical path system becomes large, the light output efficiency of scintillation light in the propagation process is influenced, and the detection efficiency of neutrons is further influenced.
In the present application, the GOS: tb transparent ceramic is formed by terbium ion (Tb 3+ ) The doped GOS-Tb powder (namely terbium-doped gadolinium oxysulfide powder) is prepared. The terbium ion doping may be added to Gadolinium Oxysulfide (GOS) in the form of terbium compounds, which may be prepared from gadolinium compounds as well as sulfur compounds.
The specific steps for preparing the GOS-Tb transparent ceramic by adopting the GOS-Tb powder are as follows:
1. synthesizing a precursor GOS and Tb powder: according to the mole ratio of sulfate ion and gadolinium ion being 0.5-1.75, terbium ion doping amount being 0.001at.% to 10at.% of total gadolinium ion, putting gadolinium compound and terbium compound into water solution, adding sulfuric acid, sulfate or other sulfides for mixing, heating or adding precipitant (such as ammonia water, ammonium carbonate) to collect precipitate, and washing precipitate with alcohol and acid to obtain precursor. Reducing the calcined GOS Tb powder precursor by adopting a reducing agent, wherein the reduction temperature is 600-1100 ℃, and the reduction time is 1-15 h; the reducing agent includes any one of hydrogen, methane and propane. Gadolinium compounds include gadolinium oxide, gadolinium hydroxide, gadolinium halides, gadolinium nitrate, gadolinium sulfate, gadolinium phosphate and gadolinium carbonate; terbium compounds and sulfur-containing materials react to form gadolinium oxysulfide, and the terbium compounds are added to provide terbium ion doping to the gadolinium oxysulfide, wherein the terbium compounds include at least one of terbium oxide, terbium hydroxide, terbium halide, terbium nitrate, terbium sulfate, terbium phosphate, and terbium carbonate.
Alternatively, GOS may also be synthesized by: for example, terbium oxide and gadolinium oxide are mixed and ball-milled according to the proportion that the terbium ion doping amount accounts for 0.001at.% to 10at.% of the total gadolinium ion, then the elemental sulfur and the fluxing agent are added according to the proportion of 1:0.3:0.3 to 1:0.6:0.6, the elemental sulfur and the fluxing agent sodium carbonate are mixed and ball-milled uniformly, the obtained product is calcined in a muffle furnace at the temperature of 400 ℃ to 1300 ℃ for 1 h to 5h, and the GOS:Tb powder is obtained after the calcined product is subjected to acid washing, water washing and alcohol washing.
2. Sintering: sintering the reduced GOS/Tb powder by any one method or combination method of pressureless sintering, hot-pressing sintering or hot isostatic pressing sintering, wherein the sintering temperature is 1200-1700 ℃, the sintering time is 0.5-20 h, and the GOS/Tb transparent ceramic is prepared preliminarily;
3. annealing: annealing the sintered GOS-Tb transparent ceramic; after annealing treatment, S vacancies and O vacancies generated by sintering the GOS-Tb transparent ceramic can be supplemented. Specifically, the annealing atmosphere comprises at least one of air, argon, hydrogen or sulfur-containing gas, and in addition, the annealing temperature and the annealing time have an important influence on the properties of the GOS-Tb transparent ceramic, and in order to make the prepared GOS-Tb transparent ceramic have a uniform crystal structure, the annealing temperature is preferably 900-1200 ℃ and the annealing time is preferably 1-50 h.
By the preparation method, the GOS-Tb transparent ceramic with high transmittance can be prepared. If it is to be used in a high resolution neutron imaging detector, it is also polished to a thickness as low as a micrometer.
The scintillator has an important influence on the performance of the detector, and based on the same, the application also provides a novel GOS-Tb transparent ceramic scintillation screen which consists of a substrate, a reflecting layer film and a GOS-Tb transparent ceramic, wherein the GOS-Tb transparent ceramic particularly refers to the ceramic structure prepared by the method. The ductility of the substrate and the reflecting layer film is strong, the thickness of the substrate and the reflecting layer film can be less than or equal to 1mm, and the GOS-Tb transparent ceramic can be thinned to ensure that the thickness of the GOS-Tb transparent ceramic is as low as micrometer (preferably less than 30 mu m). And the whole GOS-Tb transparent ceramic is transparent, so that light can pass through the scintillator to the greatest extent.
The GOS-Tb transparent ceramic is prepared by sintering and annealing the GOS-Tb powder. The biggest difference with the GOS-Tb powder scintillation screen is that a binder is not required to be added, and the microstructure is transparent crystal rather than non-transparent particle structure. After the sintered ceramic is formed, the Tb becomes compact and transparent, when the sintered transparent scintillating ceramic is used as a neutron scintillating screen, scintillating light excited by neutrons can directly transmit out through the scintillator, the light spot size can be further reduced, and the light output yield can be improved.
FIG. 4 is a graph of GOS: tb transparent ceramic scintillating screen thickness versus neutron absorption efficiency in an embodiment of the application. As shown in FIG. 4, the GOS-Tb transparent ceramic scintillating screen still has high absorption efficiency when the thickness is thinner, and the GOS-Tb transparent ceramic scintillating screen has high absorption efficiency when the thickness is 10 mu m nat GOS Tb (natural Gd scintillator) has an absorption efficiency of 68% or so 157 GOS Tb (isotope) 157 Gd-enriched scintillator) absorption efficiency of about 99%; at a thickness of 2 μm nat GOS Tb absorption efficiency is reduced to about 20 percent, while 157 GOS and Tb still have the absorption efficiency of more than 70%, and the absorption efficiency advantage is obvious when the thickness is ultra-thin. Therefore, it is preferable to employ 157 GOS: tb to prepare the GOS: tb transparent ceramic scintillating screen.
The GOS-Tb transparent ceramic is adopted as the material of the GOS-Tb transparent ceramic scintillation screen, and the difficulty is that the GOS-Tb transparent ceramic is difficult to directly process to the micrometer level. The high-resolution neutron imaging detector with high resolution in micron level requires that the thickness of GOS-Tb transparent ceramic in the scintillator is in micron level, if the GOS-Tb transparent ceramic is directly thinned, on one hand, the high requirements on the thinning process and the mechanical properties of the ceramic are realized; on the other hand, the mechanical strength of the processed GOS-Tb transparent ceramic is insufficient, and the subsequent operation is not facilitated. The design of the substrate provides practical and theoretical possibility for preparing the ultrathin GOS-Tb transparent ceramic scintillating screen.
The substrate functions to provide support for the GOS: tb transparent ceramic. Since the GOS-Tb transparent ceramic is fixed on a substrate with certain rigidity, the GOS-Tb transparent ceramic is not deformed due to insufficient supporting force when the GOS-Tb ceramic is thinned. The choice of the base material needs to meet certain rigidity conditions, i.e. still has certain rigidity when the thickness is less than or equal to 1mm, so that after GOS: tb transparent ceramic packaging, the base material still has supportability and processability (difficult deformation). Preferably, the substrate is made of materials selected from aluminum oxide, silicon nitride, silicon carbide, zirconium dioxide, aluminum nitride, magnesia-alumina spinel and yttrium aluminum garnet, and other materials with better mechanical properties.
Preferably, the substrate is GOS-Tb transparent ceramic to provide a supporting function, after a layer of metal is plated on the substrate as a reflecting layer film, the GOS-Tb transparent ceramic is combined on the reflecting layer film, and then the GOS-Tb transparent ceramic is thinned, so that the thickness of the GOS-Tb transparent ceramic can be thinned to be less than 30 mu m. The thinning treatment refers to reducing the thickness of the GOS-Tb transparent ceramic to be in the micron level by thinning, etching or sputtering processes and the like. Thinning refers to directly polishing the GOS Tb transparent ceramic above the substrate to thin the thickness of the GOS Tb transparent ceramic to achieve ideal micron-level thickness; etching means etching thinning by means of solution reaction, photo-volatilization, gas phase corrosion, plasma corrosion and the like; sputtering means that particles (ions or neutral atoms and molecules) with certain energy bombard the surface of the GOS-Tb transparent ceramic, so that atoms or molecules near the surface of the GOS-Tb transparent ceramic obtain enough energy to finally escape, and the thinning process is completed. The above-mentioned several thinning processes are all conventional technical means, and are not described in detail here.
The reflective layer film has the function of improving the utilization rate of the scintillation light. The surface of the light-sensitive element has the characteristic of high reflectivity, can reflect scintillation light to the lens as much as possible, and then enters the light-sensitive element such as a CCD camera, a sCMOS camera or a TpxCam camera, and the like, so that the photon collection efficiency of the light-sensitive element is improved, and the spatial resolution of neutron imaging is improved. The material of the reflective layer film is preferably a metal material, more preferably gold, silver, aluminum or lead, and the like, and the reflective layer film is manufactured into a film layer with a thickness of about several millimeters by utilizing the characteristics of strong reflective capability and good ductility of the metal, so as to improve the reflective efficiency.
In view of the foregoing improvements, the present application also adaptively improves upon optically amplified imaging systems in detectors to meet high resolution requirements. The optical magnification imaging system comprises an optical path system and a photosensitive element, wherein the optical path system comprises a reflecting mirror and an optical imaging lens (short for lens), and the photosensitive element is a scientific CCD camera, an sCMOS camera or a TpxCam camera. Typically, the lens is assembled on the photosensitive element, i.e. the lens is assembled at the front end of a CCD camera, an sCMOS camera or a TpxCam camera. The specific structure of each component is explained below.
To achieve spatial resolution on the order of micrometers, an optical imaging lens in an optical path system must meet the following requirements: the diffraction limit of the lens is less than 1 micron, the optical magnification of 3 to 6 times is achieved, the aberration is less than 0.1 percent, and the achromatic design is realized. The optical lens on the market cannot meet the requirement of spatial resolution in the micron order, so the application is redesigned for the optical path system and the optical element of the detector.
In this application, the optical path system includes a mirror and a lens (also called an imaging lens, including a convex lens, having a magnifying function), and the optical magnification is performed by the lens to achieve a higher spatial resolution. In an optical path system, a single lens is generally used to amplify the scintillation light. As shown in fig. 2 or fig. 6, the reflecting mirror forms an included angle with the GOS-Tb transparent ceramic scintillation screen and the lens respectively, and forms an included angle of 45 degrees with the two normally respectively, and the reflecting mirror can deflect the optical path of the scintillation light by 90 degrees, so that the scintillation light transmitted by the GOS-Tb transparent ceramic scintillation screen can vertically enter the lens after being reflected by the reflecting mirror, and then be amplified by the lens and projected onto the photosensitive element. The lens can be purchased from the market and assembled according to actual requirements. Preferably, the reflectivity of the mirror is greater than 90%.
Of course, when the magnification of a single lens is insufficient, the superposition magnification of double lenses can be adopted, so that the magnification of a higher magnification can be realized. For example, a lens with a focal length of 50mm is used as an objective lens, and after the lens is placed on a scintillator, a photosensitive element (such as a PI SOPHIA 2048B scientific research grade CCD camera or an Andor Neo 5.5sCMOS camera) is connected with the lens with a focal length of 200mm, and an imaging light path built by the method can reach 4-5 times of optical magnification, so that the requirement of high resolution of a micron level can be met.
In a preferred embodiment, a filter (also called an optical filter or a filter) may be added between the lens and the photosensitive element to reduce the effect of chromatic aberration. Because the light emitted by the GOS Tb scintillator is blue-green light and the wavelength range is from 400nm to 560nm, a filter which can only transmit the scintillation light in the wavelength range can be selected, the influence of chromatic aberration is reduced, and the spatial resolution is further improved. Of course, in other embodiments, if the light-shielding performance of the detector is strong, no filter need be added separately.
In one embodiment, to enhance light shielding and reduce the effect of other light on detector accuracy, the components may be placed in a dark room where shielding is good. Specifically, including first darkroom, second darkroom to and connect in the photophobic telescopic tube of first darkroom and second darkroom, can adjust the relative position of second darkroom and first darkroom through photophobic telescopic tube. The first darkroom and the second darkroom are both internally provided with the boron aluminum alloy plates for absorbing stray neutrons, so that the influence on imaging can be effectively reduced. More specifically, the GOS is that the Tb transparent ceramic flicker screen and the reflecting mirror are positioned in the first darkroom, the lens is positioned in the light-shielding telescopic sleeve, the photosensitive element is positioned in the second darkroom, and the lens is close to one side of the second darkroom and is arranged at the front end of the photosensitive element.
In addition to the performance of imaging lenses, the accuracy of manufacturing and mounting of the scintillator, mirrors, and photosensitive chips (components in the photosensitive element) also affects the resolution of the detector, the nature of the optical path system being to reflect the scintillation light onto the photosensitive element. If the scintillator, the reflector or the photosensitive element has too large error in the installation process, a certain included angle exists between each plane, so that an included angle exists between an image formed by the scintillator and the photosensitive element, and the images cannot be completely overlapped, thereby causing uneven focusing. Calculations indicate that the angular error of the individual planes cannot exceed 0.1mrad in order to ensure focus uniformity. Because the mechanical installation cannot reach such high precision, a special fine adjustment mechanism needs to be designed to adjust the included angle between the planes to the range of design requirements. The depth of field of high resolution optical lenses is typically narrow and very fine focus adjustments are required to include the flicker screen exactly within the depth of field of the lens. Preliminary estimates indicate that in order to ensure focus accuracy, the movement step of the lens during focus is to achieve micrometer accuracy, which requires a very precise motion control module for the focus mechanism. In one embodiment, the second darkroom is arranged on the high-precision moving platform, the high-precision moving platform can realize micro-scale fine tuning movement, a command is sent to the controller through a program to realize fine tuning of the high-precision moving platform, specifically, the movable block on the high-precision moving platform is controlled to move relatively, and the second darkroom on the movable block is driven to move, so that the second darkroom can perform fine tuning movement, and accurate focusing of a lens is realized.
In one embodiment, the device further comprises a cooling device for cooling the photosensitive element in the second dark room. The refrigerating device can be a product which is purchased in the market and has a cooling effect. Preferably, the refrigerating device is connected to one side of the second darkroom and is also mounted on the high-precision moving platform.
In one embodiment, the first darkroom and the high-precision moving platform are arranged on the bottom plate, the second darkroom is positioned on the high-precision moving platform, and the second darkroom can be finely adjusted relative to the first darkroom under the driving of the high-precision moving platform. Specifically, a movable block is arranged on the high-precision moving platform and used for installing the second darkroom, and the second darkroom can be driven to move relative to the first darkroom through the movable block, so that fine adjustment is realized.
According to a second aspect, the present application also provides a method for manufacturing a high resolution neutron imaging detector according to the first aspect, comprising the preparation of a GOS: tb transparent ceramic scintillation screen and the assembly of the detector structure. The preparation steps of the GOS and Tb transparent ceramic scintillation screen are as follows: and plating the reflecting layer film on the substrate by adopting a film plating technology, bonding and fixing the GOS-Tb transparent ceramic on the reflecting layer film by using a small amount of bonding agents, and thinning the GOS-Tb transparent ceramic to ensure that the thickness of the GOS-Tb transparent ceramic is less than 30 mu m, thus obtaining the GOS-Tb transparent ceramic scintillation screen. The GOS-Tb transparent ceramic scintillating screen prepared by the step has high transparency and high light yield, and the formed scintillating light spots are small.
The specific structure of the high-resolution neutron imaging detector is shown in figure 5, which is assembled by adopting the prepared GOS-Tb transparent ceramic scintillation screen, a light path system (comprising a reflecting mirror and a lens) and a photosensitive element (such as a CCD camera, a sCMOS camera or a TpxCam camera).
According to the high-resolution neutron imaging detector and the manufacturing method thereof, the ultrathin GOS-Tb transparent ceramic scintillator is adopted, the light yield and the transmittance of the transparent ceramic scintillator are improved through different doping and process optimization, meanwhile, a high-precision optical path system with high optical magnification is designed, and the light collection efficiency and the optical imaging precision of the optical path system are improved, so that the micron-level high-resolution detection effect is realized, and the neutron detector has higher spatial resolution capability and better light output.
Drawings
Fig. 1 is a comparative diagram: the influence of the powder scintillator (left) and the transparent ceramic scintillator (right) on the scintillation light;
FIG. 2 is a block diagram of a high resolution neutron imaging detector according to an embodiment of the present application;
FIG. 3 is a plot of the spot-thickness relationship for a GOS: tb transparent ceramic scintillating screen as described in the examples herein; the abscissa represents thickness, and the ordinate represents scintillation spot size; as can be seen, the scintillation spot size has approximately twice the thickness, and a scintillator thickness below 5 μm can reach a spot of about 10 μm;
FIG. 4 is a graph of GOS: tb transparent ceramic scintillating screen thickness versus neutron absorption efficiency in an embodiment of the application; the abscissa represents thickness, and the ordinate represents neutron absorption efficiency; as shown in the figure, the absorption efficiency is still high even when the thickness is small, and the absorption efficiency is 10 μm nat GOS Tb (natural Gd scintillator) has an absorption efficiency of 68% or so 157 GOS Tb (isotope) 157 Gd-enriched scintillator) absorption efficiency of about 99%; at a thickness of 2 μm nat GOS Tb absorption efficiency is reduced to about 20 percent, while 157 GOS and Tb still have the absorption efficiency of more than 70%, and the absorption efficiency advantage is obvious when the thickness is ultra-thin. Therefore, it is preferable to employ 157 GOS is Tb to prepare a GOS-Tb transparent ceramic scintillating screen;
FIG. 5 is a schematic diagram of a high resolution neutron imaging detector in an embodiment of the application; the device comprises a first darkroom 100, a second darkroom 200, a light-shielding telescopic sleeve 300, a refrigerating device 400, a high-precision moving platform 500, a bottom plate 600, a GOS: tb transparent ceramic scintillating screen 110, a reflecting mirror 120 and a photosensitive element 210, wherein the first darkroom is provided with a first light-shielding layer;
fig. 6 is a graph of the results of a test performed on a sample (motor) using the high resolution neutron imaging detector of an embodiment of the present application, from which the internal structure of the sample can be clearly seen.
Detailed Description
The invention will be described in further detail below with reference to the drawings by means of specific embodiments. Wherein like elements in different embodiments are numbered alike in association. In the following embodiments, numerous specific details are set forth in order to provide a better understanding of the present application. However, one skilled in the art will readily recognize that some of the features may be omitted, or replaced by other elements, materials, or methods in different situations. In some instances, some operations associated with the present application have not been shown or described in the specification to avoid obscuring the core portions of the present application, and may not be necessary for a person skilled in the art to describe in detail the relevant operations based on the description herein and the general knowledge of one skilled in the art.
Furthermore, the described features, operations, or characteristics of the description may be combined in any suitable manner in various embodiments. Also, various steps or acts in the method descriptions may be interchanged or modified in a manner apparent to those of ordinary skill in the art. Thus, the various orders in the description and drawings are for clarity of description of only certain embodiments, and are not meant to be required orders unless otherwise indicated.
The numbering of the components itself, e.g. "first", "second", etc., is used herein merely to distinguish between the described objects and does not have any sequential or technical meaning. The terms "coupled" and "connected," as used herein, are intended to encompass both direct and indirect coupling (coupling), unless otherwise indicated.
Example 1
GOS, preparation of Tb transparent ceramic:
GOS, tb transparent ceramic:
a quartz beaker was filled with 400mL of deionized water, and then 0.67mL of Tb (NO) having a concentration of 1.4922mol/L was pipetted 3 ) 3 Adding the solution into the quartz beaker, and stirring for 15min to obtain Tb 3+ Thoroughly dispersed in deionized water. 36.0686g of Gd were then weighed with an electronic balance 2 O 3 Slowly pouring commercial powder into the quartz beaker to obtain a mixed suspension, transferring the suspension into a water bath kettle with the water bath temperature of 5 ℃, and stirring for 30min. Then 20.4333g of a 96% strength by mass concentrated sulfuric acid solution was weighed by an electronic balance, poured into another quartz beaker, and the volume was set to 100mL so that the concentrated sulfuric acid was sufficiently diluted to prepare a 2mol/L dilute sulfuric acid solution. Then dilute sulfuric acid is dripped into the suspension at the dripping speed of 16mL/min, after the reaction is carried out for 40min, the water bath kettle is heated to 90 ℃, and the temperature is kept for 2h (the control of the initial temperature of the water bath is controlled, so that the sintering activity of GOS ceramic powder can be improved, and the sintering temperature of scintillating ceramic is reduced). Pouring the supernatant after the reaction is finished, washing the precipitated product with water, and then putting the precipitated product into a baking oven for drying, namelyA precursor can be obtained. The precursor is screened by a 200-mesh screen, calcined in a muffle furnace at 600 ℃ for 3 hours, and then flowed in a tube furnace to obtain H 2 Calcining at 750 ℃ for 2.5h in the atmosphere to obtain GOS ceramic powder. The GOS ceramic powder was press-formed at a pressure of 30MPa and then cold isostatic pressed at a pressure of 250 MPa. Sintering the formed biscuit for 3 hours at 1350 ℃ in a vacuum tungsten filament furnace, then sintering for 3 hours at 1450 ℃ and 176MPa in a hot isostatic pressing furnace, and finally polishing the two sides of the sintered GOS-Tb scintillating ceramic to be 1mm thick to prepare the GOS-Tb transparent ceramic for later use.
Example two
GOS, manufacturing Tb transparent ceramic scintillation screen:
an aluminum film was deposited on silicon nitride having a thickness of about 30 μm by a sputtering film plating technique, and the thickness of the aluminum film was controlled to be 1 to 5 μm. A layer of polyurethane is lightly coated on the aluminum film or coated on four corners of the aluminum film in a dot matrix mode, so that the influence on the performance of the GOS-Tb transparent ceramic scintillating screen is reduced. And (3) polishing the two sides of the GOS-Tb transparent ceramic prepared in the first embodiment to about 200 mu m in thickness, placing the GOS-Tb transparent ceramic on an aluminum film, fixing the GOS-Tb transparent ceramic on the aluminum film through polyurethane, and airing to prepare the GOS-Tb transparent ceramic scintillation screen.
Example III
High resolution neutron imaging detector assembly:
and assembling the GOS-Tb transparent ceramic scintillation screen manufactured in the second embodiment into the high-resolution neutron imaging detector. As shown in fig. 6, the detector comprises a first darkroom 100, a second darkroom 200, a light-proof telescopic sleeve 300, a refrigerating device 400, a high-precision moving platform 500, a bottom plate 600, a GOS: tb transparent ceramic scintillating screen 110, a reflecting mirror 120 and a photosensitive element 210. Wherein the lens is located in the light-tight telescopic sleeve 300, not shown. The first darkroom 100 is fixed on the base 600, the second darkroom 200 is positioned on the high precision moving platform 500, and the high precision moving platform 500 is movably disposed on the base 600. GOS Tb transparent ceramic flicker screen 110 and mirror 120 are positioned in first darkroom 100, photosensitive element 210 is positioned in second darkroom 200, and first darkroom 100 and second darkroom 200 are connected by light-proof telescopic sleeve 300. The high-resolution neutron imaging detector has higher spatial resolution and better light output.
The GOS-Tb transparent ceramic scintillation screen 110 is fixed at the inner side of an incident window of the first darkroom 100, and the angle of a reflecting mirror 120 (the reflecting efficiency is more than 90%) in the first darkroom 100 is adjusted to enable a light path to deflect 90 degrees, so that a lens and a photosensitive element 210 (particularly a scientific research grade camera) are ensured to be far away from neutron straight-through beam current, radiation damage is reduced, and scintillation light can be reflected into the lens and the photosensitive element.
The lens in the light-shielding telescopic sleeve 300 can amplify the imaging on the GOS-Tb transparent ceramic scintillating screen 110 so as to improve the spatial resolution. The first darkroom 100, the light-shielding telescopic sleeve 300 and the second darkroom 200 together form a light-shielding system, so that the interference of ambient light can be effectively avoided. The first darkroom 100 and the second darkroom 200 are composed of aluminum plates, and the aluminum plates are lined with boron aluminum alloy plates, so that stray neutrons can be effectively absorbed, and the imaging quality is improved.
The photosensitive element 210 is a CCD camera, which is a scientific imaging CCD camera, and the cooling temperature of the chip can reach-80 ℃. To improve the heat dissipation environment of the photosensitive element 210, a refrigerating device 400 is added outside the second darkroom. The CCD camera has extremely low dark current noise, so that imaging has a high signal-to-noise ratio level. Focusing during CCD camera imaging can be achieved through accurate fine tuning movement of the high-precision moving platform 500. Specifically, the high-precision moving platform 500 is provided with a movable block, and the second darkroom 200 is fixed on the movable block, so that the fine adjustment of the position of the second darkroom 200 is realized through the control of the movable block. The structure is arranged on the mounting bottom plate 600, so that the whole detector is integrated, and the detector can be mounted on different experimental platforms according to the needs.
The sample (motor) was tested using the assembled high resolution neutron imaging detector described above, with the test results shown in fig. 6. The structure of the rotor and the connecting part inside the motor can be clearly seen from the figure, and the good resolution effect is shown.
The foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (9)
1. A high-resolution neutron imaging detector based on a GOS:Tb transparent ceramic scintillation screen is characterized by comprising the following components:
the GOS is Tb transparent ceramic scintillating screen and is used for absorbing neutrons and emitting scintillating light; the thickness of the GOS and the Tb transparent ceramic in the GOS and Tb transparent ceramic scintillation screen is in a micron level;
the optical path system is used for collecting scintillation light emitted by the GOS Tb transparent ceramic scintillation screen and projecting the scintillation light onto the photosensitive element;
the photosensitive element is used for receiving the scintillation light projected by the light path system, performing photoelectric conversion and recording imaging information of neutrons;
the preparation method of the high-resolution neutron imaging detector comprises the following steps:
GOS, preparation of Tb transparent ceramic scintillation screen: plating a reflecting layer film on a substrate by adopting a film plating technology, bonding and fixing the GOS-Tb transparent ceramic on the reflecting layer film, and thinning the GOS-Tb transparent ceramic to make the thickness of the GOS-Tb transparent ceramic smaller than 30 mu m to obtain the GOS-Tb transparent ceramic scintillation screen; the substrate is made of at least one of aluminum oxide, silicon nitride, silicon carbide, zirconium dioxide, aluminum nitride, magnesia-alumina spinel and yttrium aluminum garnet;
the prepared GOS is adopted, and a Tb transparent ceramic scintillation screen, a light path system and a photosensitive element are assembled to form the high-resolution neutron imaging detector; wherein the optical path system comprises a reflector and a lens; the photosensitive element is a CCD camera, an sCMOS camera or a TpxCam camera.
2. The high-resolution neutron imaging detector based on the GOS-Tb transparent ceramic scintillation screen of claim 1, wherein the GOS-Tb transparent ceramic scintillation screen is formed by sequentially assembling a substrate, a reflecting layer film and GOS-Tb transparent ceramic; wherein the thickness of the GOS-Tb transparent ceramic is less than 30 mu m.
3. The high-resolution neutron imaging detector based on a GOS: tb transparent ceramic scintillating screen as claimed in claim 2,
the substrate is made of at least one of aluminum oxide, silicon nitride, silicon carbide, zirconium dioxide, aluminum nitride, magnesia-alumina spinel and yttrium aluminum garnet; the material of the reflecting layer film comprises at least one of aluminum, silver, lead and gold; the GOS-Tb transparent ceramic is prepared from GOS-Tb powder through sintering and annealing treatment.
4. The GOS-based Tb transparent ceramic scintillating screen high resolution neutron imaging detector of claim 3, wherein the optical path system comprises a reflector and a lens; the reflecting surface of the reflecting mirror forms an included angle with the GOS:Tb transparent ceramic scintillation screen and the lens respectively, and scintillation light emitted by the GOS:Tb transparent ceramic scintillation screen is reflected into the lens through the reflecting mirror; the lens is used for amplifying the scintillation light reflected by the reflecting mirror and projecting the scintillation light onto the photosensitive element.
5. The high-resolution neutron imaging detector based on the GOS-Tb transparent ceramic scintillation screen, as set forth in claim 4, is characterized in that a filter is arranged between the lens and the photosensitive element, and the filter can transmit scintillation light with a wavelength range of 400-560 nm.
6. The GOS-Tb transparent ceramic scintillating screen-based high-resolution neutron imaging detector of claim 5, wherein the photosensitive element is a CCD camera, an sCMOS camera or a TpxCam camera.
7. The high-resolution neutron imaging detector based on the GOS Tb transparent ceramic scintillating screen according to any one of claims 4 to 6, further comprising a first darkroom, a second darkroom and a light-shielding telescopic sleeve connected with the first darkroom and the second darkroom, wherein the relative position of the second darkroom and the first darkroom is adjusted through the light-shielding telescopic sleeve; the GOS is characterized in that a Tb transparent ceramic flicker screen and the reflecting mirror are positioned in the first dark room, the lens is positioned in the light-shielding telescopic sleeve, and the photosensitive element is positioned in the second dark room; wherein, the first darkroom and the second darkroom are internally provided with boron aluminum alloy plates for absorbing stray neutrons.
8. The GOS-Tb transparent ceramic scintillating screen-based high-resolution neutron imaging detector of claim 7, further comprising a refrigerating device connected to the second darkroom for refrigerating the photosensitive elements in the second darkroom.
9. The GOS-based Tb scintillator panel high resolution neutron imaging detector of claim 8, further comprising a high precision moving platform and a base plate; the second darkroom and the refrigerating device are movably arranged on the high-precision moving platform, the high-precision moving platform is arranged on the bottom plate, and the first darkroom is fixedly arranged on the bottom plate.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514100A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Twinkling transparent ceramics system with garnet structure and preparation method thereof |
| CN102239425A (en) * | 2008-12-23 | 2011-11-09 | 圣戈本陶瓷及塑料股份有限公司 | Scintillation separator |
| CN102279409A (en) * | 2011-06-28 | 2011-12-14 | 中国原子能科学研究院 | Neutron Beam Position Detector |
| CN102890284A (en) * | 2012-10-10 | 2013-01-23 | 中国科学院高能物理研究所 | Nuclear detection device |
| CN105158791A (en) * | 2015-06-29 | 2015-12-16 | 上海大学 | Integrated-type neutron detector based on ZnO film, and preparation method for integrated-type neutron detector |
| CN105324684A (en) * | 2013-06-13 | 2016-02-10 | 皇家飞利浦有限公司 | Detector for radiotherapy treatment guidance and verification |
| CN106154302A (en) * | 2015-03-24 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | A kind of ray detection flat panel detector scintillator panel and preparation method thereof |
| CN112068187A (en) * | 2020-09-03 | 2020-12-11 | 中国科学院高能物理研究所 | High-sensitivity thermal neutron detector |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9750958B2 (en) * | 2012-02-23 | 2017-09-05 | Steven M. Ebstein | Dosimetric scintillating screen detector for charged particle radiotherapy quality assurance |
| JP6762949B2 (en) * | 2015-09-18 | 2020-09-30 | 株式会社東芝 | Scintillator array for neutron detection and neutron detection method |
-
2021
- 2021-04-02 CN CN202110363620.1A patent/CN113253332B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102239425A (en) * | 2008-12-23 | 2011-11-09 | 圣戈本陶瓷及塑料股份有限公司 | Scintillation separator |
| CN101514100A (en) * | 2009-03-10 | 2009-08-26 | 中国科学院上海硅酸盐研究所 | Twinkling transparent ceramics system with garnet structure and preparation method thereof |
| CN102279409A (en) * | 2011-06-28 | 2011-12-14 | 中国原子能科学研究院 | Neutron Beam Position Detector |
| CN102890284A (en) * | 2012-10-10 | 2013-01-23 | 中国科学院高能物理研究所 | Nuclear detection device |
| CN105324684A (en) * | 2013-06-13 | 2016-02-10 | 皇家飞利浦有限公司 | Detector for radiotherapy treatment guidance and verification |
| CN106154302A (en) * | 2015-03-24 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | A kind of ray detection flat panel detector scintillator panel and preparation method thereof |
| CN105158791A (en) * | 2015-06-29 | 2015-12-16 | 上海大学 | Integrated-type neutron detector based on ZnO film, and preparation method for integrated-type neutron detector |
| CN112068187A (en) * | 2020-09-03 | 2020-12-11 | 中国科学院高能物理研究所 | High-sensitivity thermal neutron detector |
Non-Patent Citations (3)
| Title |
|---|
| A highly adaptive detector system for high resolution neutron imaging;N. Kardjilov;《Nuclear Instruments and Methods in Physics Research A》;95-99 * |
| Fabrication and properties of Gd2O2S：Tb scintillation ceramics for the high-resolution neutron imaging;Hongming Pan;《Optical Materials》;正文第1-3部分 * |
| 用于位置灵敏型中子探测器的~(6)LiF/ZnS(Ag)闪烁体性能研究;唐军杰;王拓;张强;孙志嘉;吴冲;;发光学报;20130115(01);78-81 * |
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