无机材料学报 ›› 2021, Vol. 36 ›› Issue (10): 1118-1124.DOI: 10.15541/jim20210059

• 研究快报 • 上一篇    

热等静压烧结制备细晶粒Ce,Y:SrHfO3闪烁陶瓷

朱丹阳1,2(), 钱康1,3, 陈肖朴1,2, 胡泽望1,2, 刘欣1,2, 李晓英1,2, 潘裕柏3, MIHÓKOVÁ Eva4, NIKL Martin4, 李江1,2()   

  1. 1.中国科学院 上海硅酸盐研究所, 透明光功能无机材料重点实验室, 上海 201899
    2.中国科学院大学 材料科学与光电工程中心, 北京 100049
    3.上海师范大学 物理系, 上海 200234

Fine-grained Ce,Y:SrHfO3 Scintillation Ceramics Fabricated by Hot Isostatic Pressing

ZHU Danyang1,2(), QIAN Kang1,3, CHEN Xiaopu1,2, HU Zewang1,2, LIU Xin1,2, LI Xiaoying1,2, PAN Yubai3, MIHÓKOVÁ Eva4, NIKL Martin4, LI Jiang1,2()   

  1. 1. Key Laboratory of Transparent Opto-functional Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
    2. Center of Materials Science and Optoelectronic Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
    3. Department of Physics, Shanghai Normal University, Shanghai 200234, China, 4. Institute of Physics, Academy of Sciences of the Czech Republic, Prague 16200, Czech Republic
  • Received:2021-02-01 Revised:2021-03-29 Published:2021-10-20 Online:2021-05-10
  • Contact: LI Jiang, professor. E-mail: lijiang@mail.sic.ac.cn
  • Supported by:
    National Key R&D Program of China(2017YFB0310500);National Natural Science Foundation of China(61775226);CAS President’s International Fellowship Initiative(E00YGH21);Operational Programme Research, Development and Education financed by European Structural and Investment Funds and the Czech Ministry of Education, Youth and Sports(SOLID21 CZ.02.1.01/0.0/0.0/16_019/0000760)

摘要:

Ce:SrHfO3陶瓷因具有高密度和高有效原子序数, 对高能射线具有很强的阻止能力。同时, Ce:SrHfO3陶瓷还具有快衰减和高能量分辨率等优异的闪烁性能, 引起了研究人员的广泛关注。由于传统的烧结方法难以实现非立方结构Ce:SrHfO3陶瓷的透明化, 本研究采用真空长时烧结和短时真空预烧结合热等静压烧结(Hot Isostatic Pressing, HIP)方法制备Ce,Y:SrHfO3陶瓷。以金属氧化物和碳酸盐为原料, 1200 ℃下煅烧8 h可以获得平均粒径为152 nm的纯相Ce,Y:SrHfO3粉体。1800 ℃真空烧结20 h获得平均晶粒尺寸为28.6 μm的不透明的Ce,Y:SrHfO3陶瓷, 而两步烧结法可以制备光学透过率良好的Ce,Y:SrHfO3陶瓷。本研究详细分析了陶瓷致密化过程中微结构的演变, 探究了预烧结温度对Ce,Y:SrHfO3陶瓷密度、显微结构和光学透过率的影响。真空预烧(1500 ℃×2 h)结合HIP后处理(1800 ℃×3 h, 200 MPa Ar)所获得的Ce,Y:SrHfO3陶瓷在800 nm处的最高直线透过率为21.6%, 平均晶粒尺寸仅为3.4 μm。在X射线激发下, Ce,Y:SrHfO3陶瓷在400 nm处产生Ce3+ 5d-4f发射峰, 其XEL积分强度比商用锗酸铋(BGO)晶体高3.3倍, Ce,Y:SrHfO3陶瓷在1 μs门宽下的光产额约为3700 ph/MeV。良好的光学和闪烁性能可以拓宽Ce,Y:SrHfO3陶瓷在闪烁探测领域的应用。

关键词: Ce, Y:SrHfO3陶瓷, 热等静压烧结, 微观结构, 晶粒细化, 闪烁性能

Abstract:

Ce:SrHfO3 ceramics possess a strong stopping power to high-energy rays due to their high density and high effective atomic number. However, it is difficult to obtain transparent Ce:SrHfO3 ceramics via traditional sintering method because of its orthogonal structure. In this work, Ce,Y:SrHfO3 ceramics were prepared by long-time vacuum sintering and short-time vacuum pre-sintering combined with hot isostatic pressing (HIP). The Ce,Y:SrHfO3 powders with a pure phase and a mean particle size of 152 nm were prepared by calcining at 1200 ℃ for 8 h using metal oxides and carbonates. The Ce,Y:SrHfO3 ceramics vacuum-sintered at 1800 ℃ for 20 h are opaque with an average grain size of 28.6 μm, while those prepared by the two-step sintering method show good optical transmittance. The evolution of the microstructure in the process of densification was analyzed in detail, and the influence of the pre-sintering temperature on the density, microstructure and optical transparency of Ce,Y:SrHfO3 ceramics was studied. The Ce,Y:SrHfO3 ceramics pre-sintered at 1500 ℃ for 2 h with HIP post-treatment at 1800 ℃ for 3 h have the highest in-line transmittance of 21.6% at 800 nm with a far smaller average grain size of 3.4 μm. Under X-ray excitation, the Ce3+ 5d-4f emission of Ce,Y:SrHfO3 ceramics was observed at 400 nm, and the XEL integral intensity is 3.3 times higher than that of Bi4Ce3O12 (BGO) crystals. The light yield of the Ce,Y:SrHfO3 ceramics is approximately 3700 ph/MeV with the shaping time of 1 μs. Good optical quality and scintillation performance of Ce,Y:SrHfO3 ceramics may expand the application range and potential in the field of scintillation detection.

Key words: Ce, Y:SrHfO3 ceramics, hot isostatic pressing, microstructure, grain refinement, scintillation properties

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