CN113582548B - Borate scintillation glass embedded with microcrystalline phase and preparation method thereof - Google Patents

Borate scintillation glass embedded with microcrystalline phase and preparation method thereof Download PDF

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CN113582548B
CN113582548B CN202110912686.1A CN202110912686A CN113582548B CN 113582548 B CN113582548 B CN 113582548B CN 202110912686 A CN202110912686 A CN 202110912686A CN 113582548 B CN113582548 B CN 113582548B
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CN113582548A (en
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马云峰
郭超
徐家跃
秦康
吴金成
蒋毅坚
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Shanghai Institute of Technology
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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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

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Abstract

The invention discloses borate scintillation glass embedded with a microcrystalline phase and a preparation method thereof. The matrix of the borate scintillation glass is Li 2 B 4 O 7 The chemical formula of the microcrystalline phase is (Mg) 1‑x Zn x ) 4 (Ta 1‑y Nb y ) 2 O 9 . Grinding and mixing the raw materials, putting the obtained glass mixture into a mould, and tabletting to obtain a blocky glass mixture; then putting the glass into a corundum crucible, putting the corundum crucible into a muffle furnace for heating to obtain glass liquid, and rapidly cooling to obtain a microcrystalline glass sample; and cutting the microcrystalline glass sample to a required size, and grinding and polishing. The scintillation microcrystalline glass material is synthesized by a high-temperature solid-phase method, stably exists in the air, and is safe and simple in process and easy to control. Under the excitation of X-ray, the light yield of the scintillation glass obtained by detection is 948-3606 ph/MeV.

Description

Borate scintillation glass embedded with microcrystalline phase and preparation method thereof
Technical Field
The invention relates to an inlay (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 A microcrystalline phase borate scintillating glass and a preparation method thereof belong to the technical field of scintillator luminescent materials.
Background
The scintillator is an energy conversion luminescent material with a scintillation luminescent property, can emit light in an ultraviolet or visible region under the irradiation of various ionizing radiations, high-energy particles and the like, and is combined with various photomultiplier tubes, charge-coupled devices and photodiodes to realize the detection, discrimination and quantitative analysis of various ionizing radiations and high-energy particles. The scintillator is widely applied to high-energy physical experiments, nuclear medicine imaging, industrial nondestructive inspection, safety inspection, environmental monitoring and exploration, astronomical observation and the like. Scintillator discovery from the earliest CdWO 4 Tl and Bi for commercial applications 4 Ge 3 O 12 The variety of (BGO) scintillation single crystals is continuously expanded and enriched, and the (BGO) scintillation single crystals mainly comprise single crystals, transparent ceramics, glass, macromolecules, quantum dots, gases, various composite materials and the like. Flicker (flicker)Common requirements of the body mainly include high productivity, fast attenuation, excellent ray cutting capability, stable physicochemical property, irradiation resistance and high energy resolution.
The glass scintillator is an important scintillation material, and has obvious advantages in the aspects of high doping, large-size preparation and optical fiber besides having the common characteristic of the scintillator. Glass, as a metastable material, can be subjected to a heat treatment to obtain a nano-scale microcrystalline phase in the glass, since the size of the crystal particles is smaller than the wavelength of visible light, and light scattering caused by the crystal particles can be avoided. The scintillation property can be effectively improved by combining the glass and the microcrystal. The glass scintillator material is used as an important supplement for other scintillator materials such as crystals, organic plastics, liquid and the like, has continuously adjustable component design, a simpler large-size preparation process, an excellent cutting and hot bending process and a mature optical fiber drawing process, and has certain advantages in aspects of large-volume detectors, optical fiber imaging, position resolution, micro-area dose detection and the like. In general, glass has many potentials to be mined as a scintillator, and related researches are still in an exploration stage at present, and how to exert the advantages of the glass to enable the glass to form complementation with other scintillators is the key point of the development of the glass scintillator.
Traditional oxide systems such as silicates and aluminates have good chemical properties, but have low refractive index and large phonon energy. And the physical and chemical stability of the glass can be obviously improved by doping components capable of effectively reducing phonon energy and other stabilizing agents in a borate system. The luminescent centers generally have larger absorption and emission cross sections in borate glass, which is beneficial to fluorescence emission and energy transfer. Meanwhile, the borate system glass has the characteristics of high near infrared and visible light region (400-1400 nm) transmittance, excellent optical performance, stable physicochemical property, lower melting temperature and the like. At present, no report that a glass scintillator obtained by doping compound with borate glass is applied to the field of radiation detection exists.
Patent ZL201810018733.6 discloses an intrinsic luminous scintillation crystal magnesium tantalate, a preparation method and application thereof, wherein the chemical formula of the intrinsic luminous scintillation crystal magnesium tantalate is Mg 4 Ta 2 O 9 Is a hexagonCrystal system having an ilmenite structure, with a light yield of 16000ph/MeV for scintillation luminescence, and CdWO 4 The crystal is equivalent, about 30% of the light yield of the CsI (Tl) crystal, the decay time is 5 mus, and the CdWO crystal is superior to the CdWO crystal 4 Crystals, but longer than CsI (Tl) crystals. The energy resolution is 6.2 percent and is higher than that of CdWO 4 Crystal, comparable to CsI (Tl). The crystal is environment-friendly, has no problem that toxic elements pollute the environment from production, processing, application and recovery, and has potential application prospect in the aspect of a ray imaging probe.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a series of scintillating microcrystalline glasses with high fluorescence emission efficiency are provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
borate scintillation glass embedded with microcrystalline phase, and matrix of the borate scintillation glass is Li 2 B 4 O 7 The chemical formula of the microcrystalline phase is (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 And the microcrystalline phase is uniformly distributed in the scintillation microcrystalline glass. This material is denoted as Li 2 B 4 O 7 -(Mg 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 。
Preferably, in the formula of the microcrystalline phase, x =0 to 0.5, y =0 to 0.5.
Preferably, the mass percentage of the microcrystalline phase in the scintillation glass is 1-20%.
The invention also provides a preparation method of the borate scintillating glass embedded with the microcrystalline phase, which comprises the following steps:
step 1): weighing raw materials according to a proportion, and then placing the raw materials in a mortar for fully grinding and mixing to obtain a uniform glass mixture;
step 2): placing the glass mixture in a die, and tabletting by using a hydraulic tablet press to obtain a blocky glass mixture;
step 3): putting the massive glass mixture into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 1000-1100 ℃, and preserving heat for 4-12 hours to obtain glass liquid;
step 4): rapidly cooling the glass liquid to obtain a microcrystalline glass sample;
step 5): and cutting the microcrystalline glass sample to a required size, grinding the microcrystalline glass sample by using metallographic abrasive paper, and polishing the microcrystalline glass sample by using a polishing agent.
Preferably, the borate scintillating glass embedded with the microcrystalline phase has the light yield of 948-3606 ph/MeV. Wherein Li 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield was highest and was 45.1% of the BGO crystals.
The invention also provides application of the borate scintillation glass embedded with the microcrystalline phase in a scintillator material.
The scintillation microcrystalline glass has high fluorescence emission efficiency, and the measured Li with the highest luminous efficiency 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The fluorescence emission efficiency under X-ray excitation of (b) corresponds to 45% of that of the BGO crystal. Meanwhile, the scintillation glass-ceramic provided by the invention has good structural uniformity, can be cast into various shapes, is easy to realize large-scale and large-size industrial production, can be used in the fields of nuclear reactors, particle physics, radiation safety, cosmic ray detection and the like, and has wide application prospects and great practical significance.
Under X-ray excitation, obtained (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The light yield of the sample is 21218-70150 ph/MeV. Comparative Mg 4 Ta 2 O 9 The light yield is greatly improved. Therefore, the invention utilizes the preparation of Li at lower temperature 2 B 4 O 7 -(Mg 1- x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The scintillation microcrystalline glass material has higher light output under the excitation of high-energy rays.
Drawings
FIG. 1 is an X-ray diffraction pattern of a scintillating microcrystalline glass prepared in each of the examples;
FIGS. 2 and 3 are the transmittance spectra of the scintillating microcrystalline glass prepared in each example;
FIG. 4 shows Li 2 B 4 O 7 -1wt％Mg 4 Ta 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 5 is Li 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 Ta 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 6 is Li 2 B 4 O 7 -1wt％Mg 4 (Ta 0.5 Nb 0.5 ) 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 7 shows Li 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 8 is Li 2 B 4 O 7 -5wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 9 is Li 2 B 4 O 7 -10wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 10 shows Li 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 An emission spectrogram of the scintillation microcrystalline glass measured under the excitation of X rays;
FIG. 11 shows Li 2 B 4 O 7 -20wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The emission spectrum of the scintillation glass ceramics is measured under the excitation of X rays.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Li 2 B 4 O 7 -1wt％Mg 4 Ta 2 O 9 (LBO-1wt% MTO) production and testing of scintillating microcrystalline glass: accurately weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、Ta 2 O 5 Fully grinding the glass raw material in an agate mortar for 60 minutes, pouring the ground raw material into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1000 ℃ for heat preservation for 4 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain the target scintillation glass ceramics, and processing the obtained scintillation glass ceramics into the scintillation glass ceramics after cutting, surface grinding and polishing.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -1wt％Mg 4 Ta 2 O 9 Shown in the graph. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-1wt% and MTO in FIG. 2, the sample transmittance was found to be good. As shown in fig. 4, li 2 B 4 O 7 -1wt％Mg 4 Ta 2 O 9 The 30keV X-ray excitation emission spectrum shows that the emission wavelength is 398nm, the luminous intensity is 11.8 percent of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -1wt％Mg 4 Ta 2 O 9 The light yield of (a) is 948ph/MeV.
Example 2
Li 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 Ta 2 O 9 (LBO-1wt% MZTO) production and testing of scintillating microcrystalline glasses: accurately weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 Fully grinding the glass raw material in an agate mortar for 60 minutes, pouring the ground raw material into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1000 ℃ for heat preservation for 4 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain the target scintillation glass ceramics, and processing the obtained scintillation glass ceramics into the scintillation glass ceramics after cutting, surface grinding and polishing.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 Ta 2 O 9 Shown in the graph. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-1wt% and MZTO in FIG. 2, the sample transmittance was found to be good. Li as shown in FIG. 5 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 Ta 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 403nm, the luminous intensity is 14.7 percent of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -1wt％
(Mg 0.5 Zn 0.5 ) 4 Ta 2 O 9 The light yield of (a) was 1179ph/MeV.
Example 3
Li 2 B 4 O 7 -1wt％Mg 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-1wt% MTNO) preparation and testing of scintillating microcrystalline glass: accurately weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、Ta 2 O 5 、Nb 2 O 5 Fully grinding the glass raw material in an agate mortar for 60 minutes, pouring the ground raw material into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1000 ℃ for heat preservation for 4 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain the target scintillation glass ceramics, and processing the obtained scintillation glass ceramics into the scintillation glass ceramics after cutting, surface grinding and polishing.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -1wt％Mg 4 (Ta 0.5 Nb 0.5 ) 2 O 9 Shown in the graph. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-1wt% and MTNO in FIG. 2, the sample transmittance was found to be good. As shown in FIG. 6, li 2 B 4 O 7 -1wt％Mg 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 399nm, the luminous intensity is 12.5 percent of the BGO crystal, and Li is obtained by detection 2 B 4 O 7 -1wt％
Mg 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield of (2) was 998ph/MeV.
Example 4
Li 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-1wt% MZTNO) production and testing of scintillating microcrystalline glass: precisely weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 、Nb 2 O 5 Fully grinding glass raw materials in an agate mortar for 60 minutes, pouring the ground raw materials into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1050 ℃ for heat preservation for 8 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain target scintillation glass ceramics, and processing the obtained scintillation glass ceramics after cutting, surface grinding and polishing to obtain the scintillation glass ceramics.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 As shown. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-1wt% and MZTNO in FIG. 2, the sample transmittance was found to be good. As shown in FIG. 7, li 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 413nm, the luminous intensity is 18.1 percent of that of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -1wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield of (a) is 1445ph/MeV.
Example 5
Li 2 B 4 O 7 -5wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-5wt%MZTNO) preparation and testing of the scintillating microcrystalline glass: accurately weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 、Nb 2 O 5 Fully grinding glass raw materials in an agate mortar for 60 minutes, pouring the ground raw materials into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1050 ℃ for heat preservation for 8 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain target scintillation glass ceramics, and processing the obtained scintillation glass ceramics after cutting, surface grinding and polishing to obtain the scintillation glass ceramics.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -5wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 As shown. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-5wt% and MZTNO in FIG. 3, the sample transmittance was found to be good. As shown in fig. 8, li 2 B 4 O 7 -5wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 426nm, the luminous intensity is 20.8 percent of the BGO crystal, and Li is obtained by detection 2 B 4 O 7 -5wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 Light yield of1665ph/MeV.
Example 6
Li 2 B 4 O 7 -10wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-10wt% MZTNO) preparation and testing of scintillating microcrystalline glass: accurately weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 、Nb 2 O 5 Fully grinding glass raw materials in an agate mortar for 60 minutes, pouring the ground raw materials into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1050 ℃ for heat preservation for 8 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain target scintillation glass ceramics, and processing the obtained scintillation glass ceramics after cutting, surface grinding and polishing to obtain the scintillation glass ceramics.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -10wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 As shown. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-10wt% as indicated by MZTNO in FIG. 3, the sample transmittance was found to be good. As shown in fig. 9, li 2 B 4 O 7 -10wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 420nm, the luminous intensity is 38.4 percent of that of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -10wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield of (a) is 3075ph/MeV.
Example 7
Li 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-15wt% MZTNO) preparation and testing of scintillating microcrystalline glass: accurately weighing and calculating glass by using analytical balanceGlass raw material Li 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 、Nb 2 O 5 Fully grinding the glass raw material in an agate mortar for 60 minutes, pouring the ground raw material into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1100 ℃ for heat preservation for 12 hours to obtain uniform glass liquid, then rapidly cooling the glass liquid to obtain the target scintillation glass ceramics, and processing the obtained scintillation glass ceramics into the scintillation glass ceramics after cutting, surface grinding and polishing.
The X-ray diffraction peak of the product is shown as Li in figure 1 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 As shown. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-15wt% MZTNO in FIG. 3, the sample transmittance was found to be good. As shown in fig. 10, li 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrogram shows that the emission wavelength is 426nm, the luminous intensity is 45.1 percent of that of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -15wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield of (a) is 3606ph/MeV.
Example 8
Li 2 B 4 O 7 -20wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 (LBO-20wt% MZTNO) production and testing of scintillating microcrystalline glass: precisely weighing the calculated glass raw material Li by using an analytical balance 2 B 4 O 7 、MgO、ZnO、Ta 2 O 5 、Nb 2 O 5 Fully grinding the glass raw material in an agate mortar for 60 minutes, pouring the ground raw material into a corundum crucible, putting the corundum crucible into a high-temperature muffle furnace at 1100 ℃ for heat preservation for 12 hours to obtain uniform glass liquid, and then rapidly cooling the glass liquid to obtain the glass liquidMarking the scintillation microcrystalline glass, and processing the obtained scintillation microcrystalline glass primary product into the scintillation microcrystalline glass after cutting, surface grinding and polishing.
The X-ray diffraction peak of the product is as Li in figure 1 2 B 4 O 7 -20wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 As shown. As can be seen from the graph, all diffraction peaks correspond to the standard diffraction peak (PDF # 08-0717). As shown by LBO-20wt% MZTNO in FIG. 3, the sample transmittance was found to be good. As shown in fig. 11, li 2 B 4 O 7 -20wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The 30k eV X-ray excitation emission spectrum shows that the emission wavelength is 431nm, the luminous intensity is 28.7 percent of that of BGO crystal, and Li is obtained by detection 2 B 4 O 7 -20wt％(Mg 0.5 Zn 0.5 ) 4 (Ta 0.5 Nb 0.5 ) 2 O 9 The light yield of (2) is 2297ph/MeV.

Claims (3)

1. A method for preparing borate scintillating glass embedded with a microcrystalline phase, which is characterized by comprising the following steps:
step 1): weighing raw materials according to a proportion, and then placing the raw materials in a mortar for fully grinding and mixing to obtain a uniform glass mixture;
step 2): placing the glass mixture in a die, and tabletting by using a hydraulic tablet press to obtain a blocky glass mixture;
step 3): putting the blocky glass mixture into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 1000 to 1100 ℃, and preserving heat for 4 to 12 hours to obtain glass liquid;
step 4): rapidly cooling the glass liquid to obtain a microcrystalline glass sample;
and step 5): cutting a microcrystalline glass sample to a required size, grinding the microcrystalline glass sample by using metallographic abrasive paper, and polishing the microcrystalline glass sample by using a polishing agent;
the matrix of the borate scintillation glass is Li 2 B 4 O 7 The chemical formula of the microcrystalline phase is (Mg) x1- Zn x ) 4 (Ta y1- Nb y ) 2 O 9 And the microcrystalline phase is uniformly distributed in the scintillation microcrystalline glass; in the chemical formula of the microcrystalline phase,x = 0~0.5，y = 0~0.5。
2. the method for preparing borate scintillation glass embedded with a microcrystalline phase according to claim 1, wherein the mass percentage of the microcrystalline phase in the scintillation glass is 1 to 20%.
3. The method for producing a borate scintillation glass embedded with a microcrystalline phase according to claim 1, wherein the light yield of the borate scintillation glass embedded with a microcrystalline phase is 948 to 3606ph/MeV.
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