压力辅助烧结BaF2闪烁陶瓷的微结构及性能研究

doi:10.15541/jim20260183

摘要/Abstract

摘要： BaF₂闪烁陶瓷兼具快速的时间响应、高的第一纳秒光产额和短的X射线衰减长度的特点,在超快X射线成像领域具有应用前景。本研究以硝酸钡(Ba(NO₃)₂)及二水合氟化钾(KF·2H₂O)为原料,采用化学共沉淀法合成BaF₂纳米粉体,通过热压烧结结合热等静压烧结(Hot Isostatic Pressing, HIP)后处理制备BaF₂闪烁陶瓷。探究不同温度热压烧结(550~650 ℃)结合HIP后处理对BaF₂闪烁陶瓷微观结构、直线透过率及闪烁性能(X射线激发发光(XEL)、闪烁衰减时间和光产额)的影响规律。结果表明：随着热压温度的升高,陶瓷内的气孔数量先减少后增加。直线透过率、XEL强度、快成分占比和光产额随着热压温度的升高呈现先增加后下降的趋势。经热压烧结(600 ℃×2 h, 50 MPa)结合HIP(600 ℃×3 h, 100 MPa Ar)制备的陶瓷的直线透过率为60.4%@800 nm(1 mm厚),快发光XEL强度最高且慢分量抑制明显,快分量占比12.2%,光产额4675 ph/MeV@3 μs,低于575 ℃热压烧结样品的5524 ph/MeV@3 μs(2 mm厚)。缺陷表征测试结果表明,575~650 ℃热压烧结的样品内部存在三种特征陷阱能级：0.80、1.16和1.20 eV,可能分别对应一种本征的电子缺陷、晶格氧(OF')和钡空位(VBa'')。而550 ℃热压烧结样品存在一个3.11 eV深陷阱能级,可能因陶瓷致密化程度较低,内部存在大量悬挂键而产生,进而导致其无法测到光电峰。575~650 ℃制备的样品随温度升高,缺陷含量有所增加,因此热释光强度逐渐上升,而光产额则呈现出下降趋势。

关键词: BaF₂陶瓷, 化学共沉淀法, 热压烧结, 微结构, 闪烁性能

Abstract: BaF₂ scintillation ceramics offer fast response, high light yield within the first nanosecond, and short X-ray attenuation length, making them promising for ultrafast X-ray imaging. In this study, BaF₂ nanopowder was synthesized via the chemical co-precipitation method using barium nitrate and potassium fluoride dihydrate. The ceramics were prepared using hot pressing (HP) followed by hot isostatic pressing (HIP) treatment. The effects of HP temperatures (550-650 ℃) combined with HIP treatment on microstructure, transmittance, and scintillation properties (XEL, scintillation decay time, and light yield) were investigated. Results indicate that with increasing HP temperature, the number of pores first decreases and then increases. In-line transmittance, XEL intensity, fast scintillation proportion, and light yield all show a trend of first increasing and then decreasing with increasing HP temperature. The optimal ceramics were obtained by HP (600 ℃×2 h, 50 MPa) combined with HIP (600 ℃×3 h, 100 MPa Ar), achieving an in-line transmittance of 60.4% at 800 nm (1 mm in thickness), the highest fast XEL intensity with significant slow component suppression, fast component of 12.2%, and a light yield of 4675 ph/MeV@3 μs, lower than the 575 ℃ HP sample (2 mm in thickness) (5524 ph/MeV@3 μs). Defect characterization revealed three trap levels inside the 575-650 ℃ hot pressed samples: 0.80 eV, 1.16 eV, and 1.20 eV, which may correspond to an intrinsic electronic defect, a lattice oxygen (OF'), and a barium vacancy (VBa''), respectively. The 550 ℃ sample has the deep trap energy level of 3.11 eV, which may be due to the lower densification of the ceramic, resulting in a large number of dangling bonds that form deep traps, making the photoelectron peak undetectable. For the samples prepared at 575-650 ℃, with increasing temperature, defect concentration increases, so the thermal stimulated luminescence intensity gradually rises, while the light yield decreases.

Key words: BaF₂ ceramics, chemical coprecipitation method, hot-pressing sintering, microstructure, scintillation properties

中图分类号:

TQ174

刘恒, 胡辰, 侯京山, 叶君豪, 黄东, 李廷松, 房永征, 李江. 压力辅助烧结BaF₂闪烁陶瓷的微结构及性能研究[J]. 无机材料学报, DOI: 10.15541/jim20260183.

LIU Heng, HU Chen, HOU Jingshan, YE Junhao, HUANG Dong, LI Tingsong, FANG Yongzheng, LI Jiang. Microstructure and Properties of BaF₂ Scintillation Ceramics Fabricated by Pressure-assisted Sintering[J]. Journal of Inorganic Materials, DOI: 10.15541/jim20260183.

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压力辅助烧结BaF₂闪烁陶瓷的微结构及性能研究

Microstructure and Properties of BaF₂ Scintillation Ceramics Fabricated by Pressure-assisted Sintering

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