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Gd_(2)O_(2)S:Tb闪烁陶瓷的制备与结构:水浴合成中H_(2)SO_(4)/Gd_(2)O_(3)摩尔比的影响

Fabrication and Microstructure of Gd_(2)O_(2)S:Tb Scintillation Ceramics from Water-bath Synthesized Nano-powders:Influence of H_(2)SO_(4)/Gd_(2)O_(3)Molar Ratio
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摘要 Gd_(2)O_(2)S:Tb闪烁陶瓷以其明亮的绿色发光、高能量转换效率和高中子俘获截面而广泛应用于中子成像和工业无损检测等领域,但Gd_(2)O_(2)S:Tb陶瓷中存在的Gd_(2)O_(3)第二相影响其闪烁性能。本工作以H_(2)SO_(4)和Gd_(2)O_(3)为原料,采用水浴法合成Gd_(2)O_(2)S:Tb前驱体,研究了H_(2)SO_(4)与Gd_(2)O_(3)的摩尔比(n)对前驱体和Gd_(2)O_(2)S:Tb粉体性能的影响。前驱体的化学组成随n增大而变化:2Gd_(2)O_(3)·Gd_(2)(SO_(4))_(3)·xH_(2)O(n<2.00)、Gd_(2)O_(3)·2Gd_(2)(SO_(4))_(3)·xH_(2)O(2.25≤n≤2.75)和Gd_(2)(SO_(4))_(3)·8H_(2)O(n=3.00),经过空气煅烧和氢气还原后,所有的粉体均形成Gd_(2)O_(2)S相。Gd_(2)O_(2)S:Tb粉体的形貌与前驱体的相组成密切相关,随着n增大,Gd_(2)O_(2)S:Tb粉体的XEL强度增加呈现出两个阶段,对应前驱体的相转变阶段。采用真空预烧结合热等静压烧结制备了Gd_(2)O_(2)S:Tb陶瓷,相较于n为2.00、2.25、2.50,其他n制备的Gd_(2)O_(2)S:Tb陶瓷都达到了较高的相对密度和XEL强度,不同n制备的陶瓷中都存在Gd_(2)O_(3)第二相,n增大有利于减少陶瓷内部的第二相,为进一步消除Gd_(2)O_(2)S:Tb陶瓷中的第二相提供了思路。 The Gd_(2)O_(2)S:Tb scintillation ceramics is extensively used for neutron radiography and industrial non-destructive testing due to its bright green emission,high intrinsic conversion efficiency and high thermal neutron capture cross-section.However,the existence of Gd_(2)O_(3)secondary phase in Gd_(2)O_(2)S ceramics impedes the scintillation property.In this work,The Gd_(2)O_(2)S:Tb precursors were synthesized in water-bath with H_(2)SO_(4)and Gd_(2)O_(3)as starting materials.Molar ratio of H_(2)SO_(4)to Gd_(2)O_(3)defined as n was adjusted to synthesize the precursors.,which influence on the properties of the precursors and powders was studied.Chemical composition of the precursors changes with the increase of n,from 2Gd_(2)O_(3)·Gd_(2)(SO_(4))_(3)·xH_(2)O(n<2.00)to Gd_(2)O_(3)·2Gd_(2)(SO_(4))_(3)·xH_(2)O(2.25≤n≤2.75),and to Gd_(2)(SO_(4))_(3)·8H_(2)O(n=3.00).After being calcined and reduced,all the powders form pure Gd_(2)O_(2)S phase.Morphology of the Gd_(2)O_(2)S:Tb powders is closely related to the phase composition of the precursor.Increasement of the XEL intensity shows two stages with n increase,corresponding to the phase transition of the precursor,respectively.The Gd_(2)O_(2)S:Tb scintillation ceramics were therefore fabricated by vacuum pre-sintering and HIP post-treatment.The ceramics were fabricated from the powders prepared with different n,achieving high relative density and XEL intensity,except the ceramics fabricated from the powders prepared with the n=2.00,2.25,2.50.The increase of n is beneficial to the removal of the Gd_(2)O_(3)secondary phase from the Gd_(2)O_(2)S:Tb ceramics.This work provides a way for eliminating the secondary phase in Gd_(2)O_(2)S:Tb scintillation ceramics.
作者 吴俊林 丁继扬 黄新友 朱丹阳 黄东 代正发 杨文钦 蒋兴奋 周健荣 孙志嘉 李江 WU Junlin;DING Jiyang;HUANG Xinyou;ZHU Danyang;HUANG Dong;DAI Zhengfa;YANG Wenqin;JIANG Xingfen;ZHOU Jianrong;SUN Zhijia;LI Jiang(Key Laboratory of Transparent Opto-functional Inorganic Materials,Shanghai Institute of Ceramics,Chinese Academy of Sciences,Shanghai 201899,China;Center of Materials Science and Optoelectronics Engineering,University of Chinese Academy of Sciences,Beijing 100049,China;School of Material Science and Engineering,Jiangsu University,Zhenjiang 212013,China;Spallation Neutron Source Science Center,Dongguan 523803,China;State Key Laboratory of Particle Detection and Electronics,Institute of High Energy Physics,Chinese Academy of Sciences,Beijing 100049,China)
出处 《无机材料学报》 SCIE EI CAS CSCD 北大核心 2023年第4期452-460,共9页 Journal of Inorganic Materials
基金 National Natural Science Foundation of China(12175254,U1832119) National Key R&D Program of China(2021YFE0104800) International Partnership Program of Chinese Academy of Sciences(121631KYSB20200039) International Cooperation Project of Shanghai Science and Technology Commission(20520750200) National Centre for Research and Development(WPC2/1/SCAPOL/2021)。
关键词 水浴法 H_(2)SO_(4)与Gd_(2)O_(3)摩尔比 Gd_(2)O_(2)S:Tb纳米粉体 闪烁陶瓷 water-bath method molar ratio of H_(2)SO_(4)to Gd_(2)O_(3) Gd_(2)O_(2)S:Tb nanopowder scintillation ceramics
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