阅读说明：本技术 一种掺杂镥基硅酸盐闪烁玻璃及其制备方法 (lutetium-doped silicate scintillation glass and preparation method thereof ) 是由 尹士玉 王昊 郭红阳 于 2019-11-21 设计创作，主要内容包括：本发明提供了一种掺杂镥基硅酸盐闪烁玻璃及其制备方法,通过引入镥基并控制工艺条件,使制得的该闪烁玻璃具有产光效率高、衰减速度快、密度大、阻拦射线性能强等优点,光产额可高达27000,密度能达到6.5～7.5g/cm<Sup>3</Sup>,均显著高于现有的闪烁玻璃,且机械强度高、化学性质稳定、不易潮解,综合性能优异,适合应用于石油勘探、放射医学成像、工业在线检测、国家安全监察、高能物理或核物理实验等领域中；同时,上述方案选用常规成分进行精确配比,并采用常规设备和改进的工艺方法,制备方法简单易行,可在保证玻璃性能的同时有效降低成本,从而能够利用有限的资源来提供性能优良的闪烁玻璃,更加适合扩大生产和应用。(The invention provides lutetium-doped silicate scintillation glass and a preparation method thereof, wherein lutetium groups are introduced and 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/cm 3 The 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 petroleum exploration, radiation medical imaging, industrial on-line detection, national security supervision and high-energy physical or nuclear physical experimentsEtc. in the field; 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.)

1, lutetium-doped silicate scintillation glass, which is characterized by comprising the following components in percentage by mol of SiO₂50～60％、H₃BO₃12～15％、NaNO₃4～7％、Lu₂O₃15～20％、Ce(C₂O₄)₂1～2％、MgF₂0.5～1％、Al₂O₃4～5％、BaCO₃1.5～2％。

2. The lutetium-doped silicate scintillation glass of claim 1, comprising the following components in mole percent: SiO2₂55.33％、H₃BO₃13.84％、NaNO₃5.53％、Lu₂O₃16.46％、Ce(C₂O₄)₂1.43％、MgF₂0.95％、Al₂O₃4.61％、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, methods of making the lutetium-doped silicate scintillation glass of any of claims 1-4 and , comprising the steps of:

s1, accurately weighing the components and uniformly mixing to obtain a th mixture;

s2, placing the th mixture in a corundum crucible for heating and melting into 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.

6. The method of claim 5, wherein in step S2, the melting conditions are as follows:

the heating temperature is 1700 ℃, and the time is 180 min.

7. The method of claim 5, wherein 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.

8. Use of the lutetium-doped silicate scintillating glass of any of claims 1-4 in X-ray detection.

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 the requirement of the nuclear imaging technology provide wide space for the research of novel scintillating materials, kinds of scintillating glass as special glass are expected to replace scintillating crystals, and the nuclear imaging technology is promoted to be applied more in the aspects of imaging 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 nuclear imaging technology becomes a hotspot and an important frontier of the research and the application of new materials.

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 Lu for heat ₂SiO₅Ce and Lu₂Si₂O₇The preparation of the scintillation glass needs higher preparation technology and excellent equipment, and faces the same problems of raw materials as the domestic numerous material industries, namely, the raw materials have higher requirements on the purity of the raw materials, the particle size of the raw material nano powder and the like, and no special exists at present in ChinaMeanwhile, the difference between domestic equipment with high sintering temperature and high vacuum degree and foreign equipment is more obvious, and the problems become bottlenecks for restricting the development of the scintillating glass, so how to provide the scintillating glass with excellent performance by using limited resources and innovative process methods (temperature for fine adjustment of components and heat treatment) becomes a technical problem to be solved by the technical personnel in the field.

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:

the aspect of the invention provides lutetium-doped silicate scintillating glass which comprises the following components in percentage by mole ₂50～60％、H₃BO₃12～15％、NaNO₃4～7％、Lu₂O₃15～20％、Ce(C₂O₄)₂1～2％、MgF₂0.5～1％、Al₂O₃4～5％、BaCO₃1.5～2％。

, the lutetium-doped silicate scintillation glass comprises the following components in percentage by mol₂55.33％、H₃BO₃13.84％、NaNO₃5.53％、Lu₂O₃16.46％、Ce(C₂O₄)₂1.43％、MgF₂0.95％、Al₂O₃4.61％、BaCO₃1.84％。

In another aspect, the invention provides a method for preparing the lutetium-doped silicate scintillation glass, comprising the following steps:

s1, accurately weighing the components and uniformly mixing to obtain a th mixture;

s2, placing the th mixture in a corundum crucible for heating and melting into 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.

, in step S2, the melting conditions are as follows:

the heating temperature is 1700 ℃, and the time is 180 min.

, 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.

The lutetium-doped silicate scintillation glass and the preparation method thereof have the beneficial effects that 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

Where applicable, the contents of any patent, patent application, or publication referred to in this application are hereby incorporated by reference in their entirety for all purposes, and the equivalents thereof are also incorporated by reference for all purposes, especially as to the definitions of synthetic techniques, products, and process designs, etc. in this application, if the definitions of specific terms disclosed in the prior art and provided in this application are not , the definitions of terms provided in this application shall control.

The invention is further illustrated in detail in connection with the following examples and the figures.