Fabrication and Microstructure of Gd2O2S:Tb Scintillation Ceramics from Water-bath Synthesized Nano-powders: Influence of H2SO4/Gd2O3 Molar Ratio

doi:10.15541/jim20220542

Abstract

Abstract:

The Gd₂O₂S: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 Gd₂O₃ secondary phase in Gd₂O₂S ceramics impedes the scintillation property. In this work, The Gd₂O₂S:Tb precursors were synthesized in water-bath with H₂SO₄ and Gd₂O₃ as starting materials. Molar ratio of H₂SO₄ to Gd₂O₃ 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 2Gd₂O₃·Gd₂(SO₄)₃·xH₂O (n<2.00) to Gd₂O₃·2Gd₂(SO₄)₃·xH₂O (2.25≤n≤2.75), and to Gd₂(SO₄)₃·8H₂O (n=3.00). After being calcined and reduced, all the powders form pure Gd₂O₂S phase. Morphology of the Gd₂O₂S: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 Gd₂O₂S: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 Gd₂O₃ secondary phase from the Gd₂O₂S:Tb ceramics. This work provides a way for eliminating the secondary phase in Gd₂O₂S:Tb scintillation ceramics.

Key words: water-bath method, molar ratio of H₂SO₄ to Gd₂O₃, Gd₂O₂S:Tb nanopowder, scintillation ceramics

CLC Number:

TQ174

WU Junlin, DING Jiyang, HUANG Xinyou, ZHU Danyang, HUANG Dong, DAI Zhengfa, YANG Wenqin, JIANG Xingfen, ZHOU Jianrong, SUN Zhijia, LI Jiang. Fabrication and Microstructure of Gd₂O₂S:Tb Scintillation Ceramics from Water-bath Synthesized Nano-powders: Influence of H₂SO₄/Gd₂O₃ Molar Ratio[J]. Journal of Inorganic Materials, 2023, 38(4): 452-460.

Figures/Tables 9

Fig. 1 XRD patterns of the products prepared with different n of H2SO4 and Gd2O3 in hot water bath at 90 ℃ for 2 h

Fig. 2 XRD patterns of the products calcined in air at 600 ℃ for 3 h from the precursors prepared with different n

Fig. 3 XRD patterns of the products calcined in air and reduced in H2 at 750 ℃ for 2 h from the precursors prepared with different n

Fig. 4 FESEM morphologies of Gd2O2S: Tb powders with different n (a) n=1.00; (b) n=1.25; (c) n=1.50; (d) n=1.75; (e) n=2.00; (f) n=2.25; (g) n=2.50; (h) n=2.75; (i) n=3.00

Fig. 5 XEL spectra and normalized integral intensity curves in the range of 350-700 nm of Gd2O2S:Tb powders with different n (a) XEL spectra; (b) Normalized integral intensity curves; Colorful figures are available on website

Fig. 6 Relative densities of Gd2O2S:Tb ceramics vacuum pre-sintered at 1300 ℃ for 3 h and HIP post-treatment at 1450 ℃ for 3 h fabricated from the powders with different n

Fig. 7 FESEM micrograph and EDS patterns (white area) of the Gd2O2S:Tb ceramics vacuum pre-sintered at 1300 ℃ for 3 h and HIP post-treatment at 1450 ℃ for 3 h fabricated from the powders prepared with n=1.00

Fig. 8 FESEM morphologies of Gd2O2S:Tb ceramics fabricated from the powders prepared with different n (a) n=1.00; (b) n=1.25; (c) n=1.50; (d) n=1.75; (e) n=2.00; (f) n=2.25; (g) n=2.50; (h) n=2.75; (i) n=3.00

Fig. 9 XEL spectra and normalized integral intensity curves in the range of 350-700 nm of Gd2O2S:Tb ceramics fabricated from the powders with different n (a) XEL spectra; (b) Normalized integral intensity curves; Colorful figures are available on website

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Fabrication and Microstructure of Gd₂O₂S:Tb Scintillation Ceramics from Water-bath Synthesized Nano-powders: Influence of H₂SO₄/Gd₂O₃ Molar Ratio

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