硅酸盐学报

用于X射线成像的铽离子掺杂硅酸盐微晶玻璃

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李鑫 ¹ , 张健 ¹ , 罗思媛 ¹ , 肖建强 ¹ , 张胜 ¹ , 吴军霄 ¹ , 刘志超 ¹ , 李保珠 ² , 徐旭辉 ¹

硅酸盐学报 | 微晶玻璃专题—研究论文 2024,52(8): 2502-2508

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硅酸盐学报 |微晶玻璃专题—研究论文 2024 , 52 (8) : 2502 -2508

用于X射线成像的铽离子掺杂硅酸盐微晶玻璃

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李鑫¹, 张健¹, 罗思媛¹, 肖建强¹, 张胜¹, 吴军霄¹, 刘志超¹, 李保珠², 徐旭辉¹

作者信息

^1．昆明理工大学材料科学与工程学院，云南省新材料制备与加工重点实验室，昆明 650093

^2．昆明理工大学国土资源工程学院，昆明 650093

通讯作者:

徐旭辉（1986—），男，博士，教授；

李保珠（1973—），男，博士，副教授。

作者简介:

李鑫（1999—），女，硕士研究生。

Terbium Ion Doped Silicate Glass-Ceramics for X-ray Imaging

Xin LI¹, Jian ZHANG¹, Siyuan LUO¹, Jianqiang XIAO¹, Sheng ZHANG¹, Junxiao WU¹, Zhichao LIU¹, Baozhu LI², Xuhui XU¹

Affiliations

^1.Faculty of Materials Science and Engineering, Key Laboratory of Advanced Materials of Yunnan Province, Kunming Universityof Science and Technology, Kunming 650093, China

^2.Faculty of Land Resources Engineering of Kunming University of Science and Technology, Kunming 650093, China

Corresponding Author:

XU Xuhui (1986-), male, Ph.D., Professor. E-mail: xuxuh07@126.com;

LI Baozhu (1973-), male, Ph.D., Associate Professor. libaozhu916@tom.com

LI Xin (1999-), female, Master candidate. E-mail: lx254946@163.com

出版时间: 2024-08-20 doi: 10.14062/j.issn.0454-5648.20230880

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摘要

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X射线成像在工业、医疗和科学研究中得到广泛应用。与直接式X射线探测相比，间接式X射线探测是一种更便宜、更稳定的选择。但如今商用闪烁体大都存在制备成本高、稳定性差等问题，因此寻找制备简单、低成本、高化学稳定性和环境友好的新型闪烁体材料是必要的。通过高温熔融法和热处理工艺，成功地在硅酸盐玻璃基体内原位生长出ZnGa₂O₄纳米晶，通过掺杂Tb³⁺、调整退火温度，使材料既具有高透明度又具有高闪烁性能（光产额优于商业闪烁体BGO）。在X射线下表现出良好的成像性能，实现了16 lp/mm的成像分辨率。同时还表现出长时间的环境稳定性和辐射发光稳定性。这些优异的性能使得ZnGa₂O₄∶Tb³⁺闪烁体玻璃在玻璃闪烁体间接成像领域具有很大的应用潜力。

关键词

微晶玻璃 / X射线成像 / 透明闪烁体 / 铽离子

Abstract

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Introduction

X-ray detectors could be divided into direct and indirect types, the latter has cheaper and more stable properties. As the key component of indirect detection, scintillators could convert high-energy photons into low-energy ultraviolet or visible photons. However, the preparation process of traditional scintillation single crystals is relatively complex and costly, and the hygroscopicity of materials also puts strict requirements on their working environment and packaging technology. Moreover, the Tl and Cd are toxic and not environmentally friendly. Therefore, it is very necessary to find new scintillators with simple preparation, low-cost, chemically stable, and environmentally stable properties. The glass-ceramics combines the excellent optical properties of nanocrystals with the high stability and transparency of inorganic glass. High-quality and large-area glass-ceramics could also be easily obtained. Rare earth ions have special energy level structures and luminescence characteristics. Under optical excitation, they can absorb energy and emit light of specific wavelengths, thereby enhancing their scintillation performance and luminescence characteristics, and are resistibility to radiation damage. When the scintillation glass is irradiated by external excitation light sources, the rare earth ions absorb the energy and transfer to high energy level state, and then release energy through radiation transitions. In this paper, rare earth ions are doped into glass-ceramics to introduce efficient luminescent centers. The luminescence performance of ZnGa₂O₄∶Tb³⁺ glass-ceramics under X-ray irradiation and its indirect imaging ability are studied.

Methods

To prepare ZnGa₂O₄ glass-ceramics composing of 52SiO₂-10Na₂CO₃-22ZnO-16Ga₂O₃-x%Tb₄O₇ (mole fraction), the raw materials were weighed and ground in an agate mortar for 15 min. After uniformly mixing, the powder was transferred to a 30 ml alumina crucible and melted at 1 600 ℃ for 60 min. The sample was poured onto a preheated copper plate at 350 ℃, pressed into shape, and cooling naturally to form the precursor glass. The precursor glass was treated by heating at 600 ℃ for 4 h to release internal stresses. Subsequently, the samples were heat treated at 700, 750, 800, 850, 900 ℃ for 6 h to form glass-ceramics (GC) with different degrees of crystallinity. Finally, these GC samples were polished or ground into powder for further characterization.

The phase of the samples was determined by X-ray diffraction analysis, transmission electron microscopy, and scanning electron microscopy. The photoluminescence properties were analyzed by using the excitation spectrum and photoluminescence spectrum of the Hitachi F-7000 fluorescence spectrophotometer with a 150 W Xe lamp as the excitation source. The transmission spectra were determined by using a TU1810 UV/visible spectrophotometer. A miniaturized X-ray tube with Cu-K_α (λ=0.154 05 nm) radiation source was used for X-ray imaging, maintaining a tube voltage and current of 40 kV and 30 mA, respectively, with a Nikon D500 camera for imaging capture. The radiation luminescence spectra of the samples under X-ray irradiation were measured using a fluorescence spectrophotometer (Ocean Optics, QE Pro).

Results and discussion

For the precursor glass treated at the temperature ranging from 700 ℃ to 800 ℃, the samples exhibit a transmittance of over 80% in the wavelength range of 400 nm to 800 nm. However, when the heating temperature exceeds 850 ℃, the transmittance of the samples gradually decreases attributing to the increase of the size of ZnGa₂O₄ nanocrystals precipitated within the glass matrix, resulting in an increase in Rayleigh scattering and the decrease in transparency. Under different doping concentrations of rare earth ion, there is no impurity observed in the XRD diffraction patterns. Additionally, the samples maintain a transmittance of over 80% under different concentrations of Tb³⁺ doping. Based on the intensity of photoluminescence spectra, the optimal Tb³⁺ doping concentration is determined to be 1.5%.

The ZnGa₂O₄∶1.5%Tb³⁺ glass-ceramics exhibits a high absorption coefficient in the range of 0 to 50 keV, with a radiation luminescence yield of 13 000 photons/MeV, which is superior to that of commercial BGO in both absorption coefficient and radiation luminescence yield. Additionally, it exhibits a linear response relationship with X-ray dose rates and demonstrates long-term stability under X-ray irradiation. Indirect X-ray imaging by using this material could clearly visualize the internal structure of printed circuit boards with an imaging resolution of 16 lp/mm. Furthermore, the ZnGa₂O₄∶1.5%Tb³⁺ glass-ceramics could restore its radiation luminescence performance to its initial state via thermal treatment.

Conclusions

ZnGa₂O₄∶1.5%Tb³⁺ glass-ceramics exhibits characteristic emissions of Tb³⁺ under both UV and X-ray irradiation, with a high transmittance of over 80%, which is beneficial for achieving high-resolution X-ray imaging (16 lp/mm). Additionally, under high-energy radiation exposure for a long duration (1 000 h), the RL intensity of ZnGa₂O₄∶1.5%Tb³⁺ glass-ceramics only decreases by 20%, and the radiation damage caused by high-dose X-ray can be restored through simple low-temperature thermal treatment, which reduce the cost of scintillators and meet the long-term lifetime. This study demonstrates that ZnGa₂O₄∶1.5%Tb³⁺ could provide high-quality, efficient, and precise imaging results, and making it promising for applications in medical imaging and non-destructive testing.

Key words

glass-ceramics / X-ray imaging / transparent scintillators / terbium ion

引用本文

李鑫, 张健, 罗思媛, 肖建强, 张胜, 吴军霄, 刘志超, 李保珠, 徐旭辉. 用于X射线成像的铽离子掺杂硅酸盐微晶玻璃. 硅酸盐学报, 2024 , 52 (8) : 2502 -2508 . DOI: 10.14062/j.issn.0454-5648.20230880

Xin LI, Jian ZHANG, Siyuan LUO, Jianqiang XIAO, Sheng ZHANG, Junxiao WU, Zhichao LIU, Baozhu LI, Xuhui XU. Terbium Ion Doped Silicate Glass-Ceramics for X-ray Imaging[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (8) : 2502 -2508 . DOI: 10.14062/j.issn.0454-5648.20230880

基金

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云南省科技厅面上项目(202301AT070149)
云南省科技厅昆明理工大学“双一流”创建联合专项面上项目(202201BE070001-029)
云南省科技重大专项(202202AG050016-4; 202202AG050004)

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2024年第52卷第8期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230880

接收时间：2023-11-17
首发时间：2026-10-22
出版时间：2024-08-20

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出版历史

收稿日期：2023-11-17
修回日期：2023-12-01

基金

云南省科技厅面上项目(202301AT070149)

云南省科技厅昆明理工大学“双一流”创建联合专项面上项目(202201BE070001-029)

云南省科技重大专项(202202AG050016-4; 202202AG050004)

作者信息

^1．昆明理工大学材料科学与工程学院，云南省新材料制备与加工重点实验室，昆明 650093

^2．昆明理工大学国土资源工程学院，昆明 650093

通讯作者:

徐旭辉（1986—），男，博士，教授；

李保珠（1973—），男，博士，副教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20230880

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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