硅酸盐学报

铕掺杂Gd₂Zr₂O₇透明陶瓷的制备及闪烁性能

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孙志成 ¹ , 冯桂青 ¹ , 王帅华 ¹^,² , 丁雨憧 ³ , 吴少凡 ¹^,²

硅酸盐学报 | 研究论文 2024,52(3): 746-754

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硅酸盐学报 |研究论文 2024 , 52 (3) : 746 -754

铕掺杂Gd₂Zr₂O₇透明陶瓷的制备及闪烁性能

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孙志成¹, 冯桂青¹, 王帅华¹^,², 丁雨憧³, 吴少凡¹^,²

作者信息

^1．中国科学院福建物质结构研究所，福州，350002

^2．闽都创新实验室，福州，350108

^3．中国电子科技集团公司第二十六研究所，重庆 400060

通讯作者:

王帅华（1987—），男，博士，研究员。

作者简介:

孙志成（1998—），男，硕士研究生。

Preparation and Scintillation Properties of Europium-Doped Gd₂Zr₂O₇ Transparent Ceramics

Zhicheng SUN¹, Guiqing FENG¹, Shuaihua WANG¹^,², Yuchong DING³, Shaofan WU¹^,²

Affiliations

^1.Fujian Institute of Materials and Structures, Chinese Academy of Sciences, Fuzhou 350002, China

^2.Fujian Science & Technology Innovation Laboratory for Optoelectronic Information of China, Fuzhou 350108, China

^3.No.26 Research Institute, China Electronics Technology Group Corporation, Chongqing 400060, China

Corresponding Author:

WANG Shuaihua (1987-), male, Ph.D., Professor. E-mail: shwang@fjirsm.ac.cn

SUN Zhicheng (1998-), male, Master candidate. E-mail: sunzhicheng@fjirsm.ac.cn

出版时间: 2024-03-20 doi: 10.14062/j.issn.0454-5648.20230725

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摘要

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与传统闪烁陶瓷相比，基于立方相Gd₂Zr₂O₇具有高密度、高光学透过率和良好的闪烁性能等特征，本工作采用真空烧结法，成功制备出系列Eu³⁺掺杂Gd₂Zr₂O₇透明陶瓷，研究了掺杂离子及掺杂量对其晶体结构、光学透过率、荧光性能及闪烁性能的影响。结果表明，所制备的透明陶瓷样品具有良好的光透过能力；光谱表征发现，20% Eu³⁺掺杂Gd₂Zr₂O₇具有最佳的光致荧光和辐照发光强度，其最强发射峰位于630 nm。X射线成像实验表明，Gd_1.8Eu_0.2Zr₂O₇透明陶瓷的X射线成像分辨率可达11 lp·mm^-1，具备对不同材质物体的成像应用潜力。在医学成像、工业探伤、高能物理等领域具有潜在的应用价值。

关键词

烧绿石 / 缺陷萤石 / 透明陶瓷 / 闪烁性能 / 空间分辨率

Abstract

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Introduction

This paper prepared a series of Eu³⁺ doped Gd₂Zr₂O₇ transparent ceramics by a vacuum sintering method, and charaterized the density and optical transmittance of cubic phase Gd₂Zr₂O₇. The effects of doping ions and their concentration on the crystal structure, optical transmittance, fluorescence performance, and scintillation performance were investigated. The results show that the prepared transparent ceramic samples have a good optical transmittance. The spectral characterization reveals that 20% Eu³⁺ doped Gd₂Zr₂O₇ has optimum fluorescence and irradiated luminescence intensity, and the most intense emission peak is located at 630 nm. The X-ray imaging shows that Gd_1.8Eu_0.2Zr₂O₇ transparent ceramics have an X-ray imaging resolution of up to 11 lp·mm^-1, having a potential for the imaging applications.

Methods

High purity gadolinium oxide, europium oxide and zirconia (purity 4N) as raw materials were mixed according to a stoichiometric ratio (Gd³⁺,Eu³⁺)∶Zr⁴⁺ of 1∶1. The mixed raw materials were ground in anhydrous ethanol and polyethylene glycol (PEG) in a planetary mill with zirconia grinding chamber and ballsat a ball∶material mass ratio of 27∶1 for 72 h. Afterwards, the ground mixture slurry was washed with anhydrous ethanol after drying. Gd_2-_xEu_xZr₂O₇ could be obtained via sintering in a box furnace at 1 400 ℃ according to the reaction: Gd_2-_XEu_XZr₂O₇

(1- X/2)Gd₂O₃ + 2ZrO₂ + X/2Eu₂O₃ → Gd_2-_xEu_xZr₂O₇ (X = 0-0.28)

The ceramic blank was formed via dry pressing and cold isostatic pressing, sintered in a vacuum tungsten furnace at 1 800 ℃ for 10 h, and then annealed in a box furnace in air at 1 250 ℃ for 6 h. Finally, a transparent ceramic with 1 mm thickness was obtained after double-sided polishing.

Results and discussion

A ceramic powder prepared by ball grinding was sintered in a vacuum tungsten wire furnace to prepare transparent ceramics with a high light transmission rate. The XRD results show that when 20% Eu³⁺ is added to Gd₂Zr₂O₇, the crystal structure of Gd_1.8Eu_0.2Zr₂O₇ appears some superlattice diffraction peaks (331) of pyrochlore. The crystal structure changes from defective fluorite to pyrochlore. The optical transmittance spectra indicate that the optical transmittance decreases from 76% to 65% (@1 500 nm) when the doping content of Eu³⁺ increases from 0 to 28%. There exist 6 distinct excitation peaks between 230 nm and 500 nm. A wide excitation peak at 267 nm is attributed to the charge transfer band of O^2-—Eu³⁺. In addition, five excitation peaks at 362, 382, 393, 414 nm and 465 nm correspond to 4f-4f energy level transitions ⁷F₀→⁵D₄, ⁵G_J, ⁵L₆, 5D₃ and ⁵D₂ in Eu³⁺, respectively. Among six excitation peaks, a wide excitation peak at 267 nm has the most intense intensity. All the excitation peak intensities increase when Eu³⁺ concentration increases from 4% to 20%. When Eu³⁺ doping amount is 20%, the maximum excitation peak intensity appears. The further characterization of the scintillation properties of ceramic samples indicates that the X-ray irradiation intensity is a maximum value when the doping amount is 20%. At 630 nm, the radiation luminescence intensity value is 1.1×10⁴, and the material has an X-ray absorption capacity equivalent to that of BGO crystals, and also has a good anti-radiation damage ability. Finally, X-ray imaging tests on Gd_1.8Eu_0.2Zr₂O₇ ceramic samples of different materials show that the Gd_1.8Eu_0.2Zr₂O₇ ceramic sample can clearly distinguish metal and plastic materials, and has a limit spatial resolution of 11 1p·mm^-1, indicating that the modified material is a potential X-ray detection material.

Conclusions

A series of Eu³⁺ doped transparent ceramics were prepared by a vacuum sintering method. The crystal structure of Gd_2-_xEu_xZr₂O₇ was gradually changed from defective fluorite to pyrochlore via adjusting the doping amount of Eu³⁺. At 630 nm, the Gd_2-_xEu_xZr₂O₇ transparent ceramic sample showed the optimum fluorescence emission and X-ray irradiation intensity, and the material had a limit spatial resolution of 11 1p·mm^-1, which could clearly distinguish metal and plastic materials, confirming an application potential of the A₂B₂O₇ series of scintillating transparent ceramics X-ray imaging.

Key words

pyrochlore / defective fluorite / transparent ceramics / scintillation properties / spatial resolution

引用本文

孙志成, 冯桂青, 王帅华, 丁雨憧, 吴少凡. 铕掺杂Gd₂Zr₂O₇透明陶瓷的制备及闪烁性能. 硅酸盐学报, 2024 , 52 (3) : 746 -754 . DOI: 10.14062/j.issn.0454-5648.20230725

Zhicheng SUN, Guiqing FENG, Shuaihua WANG, Yuchong DING, Shaofan WU. Preparation and Scintillation Properties of Europium-Doped Gd₂Zr₂O₇ Transparent Ceramics[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (3) : 746 -754 . DOI: 10.14062/j.issn.0454-5648.20230725

基金

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国家自然基金面上项目(22075284)
福建省自然科学基金杰出青年项目(2023J06051)
中国科学院青年促进会(2019304)
中国科学院仪器研制项目(YJKYYQ20210039)

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2024年第52卷第3期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230725

接收时间：2023-09-18
首发时间：2026-10-22
出版时间：2024-03-20

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出版历史

收稿日期：2023-09-18
修回日期：2023-10-30

基金

国家自然基金面上项目(22075284)

福建省自然科学基金杰出青年项目(2023J06051)

中国科学院青年促进会(2019304)

中国科学院仪器研制项目(YJKYYQ20210039)

作者信息

^1．中国科学院福建物质结构研究所，福州，350002

^2．闽都创新实验室，福州，350108

^3．中国电子科技集团公司第二十六研究所，重庆 400060

通讯作者:

王帅华（1987—），男，博士，研究员。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20230725

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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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