CN-121974566-A - Transparent glass ceramic and preparation method and application thereof

Abstract

The invention discloses transparent microcrystalline glass and a preparation method and application thereof. Relates to the field of luminescent materials. The method for preparing the transparent glass ceramics comprises the following steps of S1 grinding Li 2 O、SiO 2 、Al 2 O 3 , mgO and Eu 2 O 3 to obtain mixed powder, S2 melting the mixed powder in a reducing atmosphere at 1600-1610 ℃ and then rapidly cooling to obtain precursor amorphous glass, and S3 carrying out heat treatment on the precursor amorphous glass in the reducing atmosphere at the heat treatment temperature of more than 860 ℃ and less than 1200 ℃ to obtain the transparent glass ceramics. The microcrystalline glass prepared by the method has high luminous efficiency, excellent thermal stability, high transparency and good X-ray imaging performance.

Inventors

• HU TAO
• HUANG JIAQI
• WANG GUANGXIA
• GAO YAN

Assignees

• 五邑大学

Dates

Publication Date

20260505

Application Date

20251223

Claims (10)

1. 1. The method for preparing the transparent glass ceramics is characterized by comprising the following steps: S1, grinding Li 2 O、SiO 2 、Al 2 O 3 , mgO and Eu 2 O 3 to obtain mixed powder; s2, melting the mixed powder in a reducing atmosphere at 1600-1610 ℃, and then rapidly cooling to obtain precursor amorphous glass; And S3, carrying out heat treatment on the precursor amorphous glass in a reducing atmosphere, wherein the heat treatment temperature is more than 860 ℃ and less than 1200 ℃ to obtain the transparent microcrystalline glass.
2. 2. The method according to claim 1, wherein the time for the melting treatment in the step S2 is 2 to 4 hours.
3. 3. The method according to claim 1, wherein the reducing atmosphere in steps S2 and S3 consists of H 2 and/or carbon powder.
4. 4. The method according to claim 1, wherein the heat treatment temperature in the step S3 is 920-1050 ℃.
5. 5. The method according to claim 1, wherein the heat treatment time in the step S3 is 30min to 2h.
6. 6. A transparent glass ceramic prepared by the method according to any one of claims 1 to 5, wherein the crystal phase of the glass ceramic is Mg 0.6 Al 1.2 Si 1.8 O 6 :Eu 2+ , and the matrix component comprises Li 2 O、SiO 2 、Al 2 O 3 、MgO、Eu 2 O 3 .
7. 7. The transparent glass ceramic according to claim 6, wherein the matrix component comprises the following components in mole percent SiO 2 50%-55%,Al 2 O 3 25%-30%,MgO 8%-12%,Li 2 O 8-12%、Eu 2 O 3 0.02%-1.00%.
8. 8. The transparent glass ceramic according to claim 7, wherein the matrix component comprises the following components in mole percent SiO 2 53.84-55.00%,Al 2 O 3 25.00-26.92%,MgO 8.00-9.62%,Li 2 O 8.00-9.62%,Eu 2 O 3 0.02-1.00%.
9. 9. The transparent glass-ceramic according to claim 6, wherein the size of the crystallites of the transparent glass-ceramic is 1-100nm.
10. 10. Use of a transparent glass ceramic according to claim 6 for X-ray imaging, information storage or solid state lighting.

Description

Transparent glass ceramic and preparation method and application thereof Technical Field The invention relates to the technical field of luminescent materials, in particular to transparent glass ceramics and a preparation method and application thereof. Background The transparent glass ceramics are novel solid optical functional materials with important application value, and are unique in that the mechanical strength and the thermal stability of a glass matrix are organically combined with the excellent optical characteristics of a fluorescent material, so that the transparent glass ceramics exhibit excellent comprehensive performance. With the rapid development of modern technology, the material has increasingly wide application prospects in various fields such as illumination, display technology, X-ray imaging, medical equipment and the like, and the transparent microcrystalline glass material with high performance is deeply researched and developed, so that the material has a vital significance for promoting the technical upgrading and innovation of related industries. In the current technical background, the luminescent materials commonly used in the market mainly comprise three categories of fluorescent powder, glass and ceramic. The fluorescent powder is widely applied to various light-emitting devices by virtue of higher luminous efficiency and relatively simple preparation process, the glass material is an indispensable basic material in the optical field by virtue of good transparency and thermal stability, and the fluorescent ceramic is used as a composite functional material, so that the fluorescent powder has the high quantum efficiency of the fluorescent powder and the high thermal conductivity and the physicochemical stability of a glass matrix, and is attractive in scenes with higher performance requirements. In addition, in the critical application field of X-ray imaging, as a core component for converting high-energy X-rays into low-energy visible light, the demand of the scintillator material is continuously growing along with the development of the fields of safety detection, medical imaging, radioactivity detection and the like, and currently, the commercial scintillator material comprises single crystal scintillators and the like, and the material is prominent in terms of scintillation performance and long-term stability and is a mainstream choice in the current market. However, the above-mentioned prior art materials have defects that are difficult to overcome, and limit further application and development. The fluorescent powder is easy to generate light attenuation phenomenon in the long-time use process, so that the luminous intensity is gradually reduced, and the use effect is seriously affected, and more importantly, the fluorescent powder usually needs to be fixed and protected by depending on organic resin in the LED device packaging process, and long-time light irradiation can accelerate the ageing and yellowing of the organic resin, even cause ablation problems, and further cause serious consequences such as color development drift, lighting device failure and the like. Although the glass material has the advantages of transparency and thermal stability, the amorphous structure in the glass material can inhibit the luminescence center, so that the luminescence effect of the glass material is obviously different from that of fluorescent powder. The fluorescent ceramic has the advantages of various materials, but the preparation process faces a plurality of technical bottlenecks, on one hand, most ceramic greenware has extremely high requirements on the purity of raw materials and is prepared by high-pressure molding of irregularly-shaped powder, a large number of pores are easily generated in the mode, so that the transparency of the ceramic is greatly reduced, and on the other hand, the existing methods for preparing the transparent ceramic, such as a cold isostatic pressing method, a grouting method, a hot isostatic pressing method, a laser beam suspension melting method, a plasma spark sintering method and the like, all require extreme preparation environments with ultrahigh pressure or ultrahigh temperature, so that the production cost is high, the technological process is extremely complex, and the large-scale production is difficult to realize. In the field of X-ray imaging, the technical drawbacks of scintillator materials are likewise significant. The single crystal scintillator has the problems of long time consumption of the synthesis step and poor device processability, which greatly limits the flexibility and efficiency of the single crystal scintillator in practical application, while the glass scintillator is used as a potential substitute material, the scintillation luminous intensity and the X-ray imaging resolution of the single crystal scintillator are still relatively low, and compared with the commercial single crystal scintillator, a significant difference