Rare Earth Doped Gd2O2S Scintillation Ceramics

doi:10.15541/jim20200544

Abstract

Abstract:

Rare earth ions doped Gd₂O₂S scintillators are new type of oxysulfide scintillators, which have been developed since 1980s. The Gd₂O₂S matrix with cross section of high density and high thermal neutron absorption has high X ray and thermal neutron stopping capacity. The doping of different rare earth ions (Pr³⁺, Tb³⁺, etc.) shows fast decay or high light yield, which plays a very important role in application of scintillation. Composition control of oxysulfide is always a key problem to be solved in the synthesis process. However, the high melting point of Gd₂O₂S material and the serious volatilization of sulfur restrict the preparation of Gd₂O₂S single crystals, with high optical quality and excellent scintillation performance. Ceramic is the main application form of Gd₂O₂S scintillation material. Its pure phase Gd ₂O₂S phosphors with small particle size, narrow particle size distribution and low agglomeration is the key to sintering high quality scintillation ceramics. These ceramics prepared by simply increasing the sintering temperature produce a large number of sulfur vacancies and oxygen vacancies, decreasing the scintillation properties. Therefore, preparation of Gd₂O₂S scintillation ceramics usually need pressure assistance to increase the production cost. In this paper, their scintillation mechanism and research situation are introduced firstly. Then, their fabrication process, solution of defects removal, research status and applications in neutron imaging and medical X-CT fields are overviewed. Finally, we summarized the previous and prospected the future development of Gd₂O₂S scintillation ceramics.

Key words: Gd₂O₂S scintillation ceramics, controllable fabrication, defects control, neutron imaging, medical X-CT, review

CLC Number:

TQ174

LI Jiang, DING Jiyang, HUANG Xinyou. Rare Earth Doped Gd₂O₂S Scintillation Ceramics[J]. Journal of Inorganic Materials, 2021, 36(8): 789-806.

Figures/Tables 24

Fig. 1 Scintillation mechanism of activator doped inorganic scintillators in terms of energy band structure[14]

Fig. 2 History (1940-2017) of first publication of scintillators with light output of >20000 ph/MeV, representing scintillators published in peer-reviewed articles [18] Blue bars: new compounds; Yellow bars: known compounds with new activator or codoped; Red letters: commercial products; Green letters: under development

Table 1 Optical and scintillation properties of selected scintillators

Scintillator	Density/(g·cm^-3)	Z_eff/cm	Decay time/ns	λ_em/nm	Light yield/(×10³, ph/MeV)	Ref.
NaI:Tl	3.67	50.8	230	415	43	[23]
LaI:Ce	5.6	54.2	1-2	452, 502	0.2-0.3	[24]
SrI₂:Eu	4.55	49.85	1200	435	115	[25]
BaBrI:Eu	5.21	51.1	331-714	413	89	[26]
Bi₄Ge₃O₁₂	7.13	75.2	300	505	8.2	[27]
PbWO₄	8.28	75.6	6	420	0.1	[28]
CaWO₄	6.1	63.8	600	430	20	[22]
Gd₂O₂S:Pr,Ce,F	7.34	61.1	4000	510	35	[16]
YAlO₃:Ce	5.5	33.6	30	350	21	[29]
Y₃Al₅O₁₂:Pr	4.56	32.6	23.4	310, 380	9.25	[16]
Gd₂SiO₅:Ce	6.71	59.4	60-600	430	12.5	[16]
Y₂SiO₅:Pr	4.45	35	6.5-33	270, 35	4.58	[30]
Gd₃A_l2Ga₃O₁₂:Ce	6.67	50.6	80-800	520	46	[31]
(Gd,Y)₃(Al,Ga)₅O₁₂:Ce	5.8	45	100-600	560	60	[32]

Fig. 3 Schematic of Gd2O2S structure[41]

Table 2 Basic physical and chemical property of Gd2O2S[41,42]

Property	Feature
Molecular formula	Gd₂O₂S
Relative molecular mass	378
Crystal structure	Hexagonal crystal system
Cell parameters	a=0.38514 nm, c/a=1.73
Melting point	2070 ℃
Density	7.34 g/cm³
Z_eff	61.1
Index of refraction	2.2
Band gap	4.6-4.8 eV
Phonon energy	520 cm^-1
Color	Colorless
Technical aspects	Chemical stability

Fig. 4 FE-SEM images of different powder[52] (a) Commercial Gd2O3 powder; (b) Gd2O3 powder synthesized by coprecipitation; (c) Synthesis by commercial powder; (d) Synthesis by coprecipitation powder

Fig. 5 SEM images of GOS:Tb phosphors synthesized by the flux method[53] (a) Without Na4P2O7 flux; (b) With Na4P2O7 flux

Fig. 6 Structure diagrams of precursor La2(OH) 4SO4·nH2O and calcined products in different atmospheres[63]

Fig. 7 Fluorescence spectra of GOS:Tb powders under different accelerating voltages and electron beam currents[70] (A) Different accelerating voltages; (B) Different beam currents; (C) Variation of luminous intensity with voltage and current; (D) Calculated incident electron depth varied with voltage Colorful figures are available on website

Fig. 8 Total transmittance curves of GOS ceramics (thickness 1.6 mm) prepared by hot pressing[72] 1-GOS:F ceramics; 2-GOS:Pr,Ce ceramics

Fig. 9 FESEM images of the fracture surfaces and EDS analysis[58] (a) Green body; (b) Pre-sintered body; (c) After hot isotatic pressing; (d) EDS analysis of the selected area in (c)

Fig. 10 Microstructures of GOS ceramics prepared by pressureless sintering under different conditions[78] (a) 1380 ℃×6 h, 1.0 K/min; (b) 1300 ℃×3 h, 2.8 K/min

Fig. 11 Pulse height spectra (a) of GOS:Pr, Ce, F ceramics with different thicknesses prepared by pressureless sintering and commercial GOS ceramics, and afterglow curve (b) of GOS:Pr,Ce,F ceramics by pressureless sintering and commercial ceramics[79] (a) Sample thickness is 0.5 mm, 1.0 mm, and 1.5 mm, respectively; (b) Commercial ceramic thickness is 0.5 mm Colorful figures are available on website

Fig. 12 Influence of annealing temperature on the afterglow performance of GOS: Pr ceramics[75]

Table 3 Scintillation property of GOS ceramics doped with different rare earth ions

Scintillators	λ_em/nm	Decay time/μs	Afterglow/(%, after 3 ms/100 ms)	Light yield/(ph·MeV^-1)	Ref.
Gd₂O₂S:Pr,Ce,F	510	4	<0.1/<0.01	35000	[29,85]
Gd₂O₂S:Tb	545	1×10³	-	60000	[29]
Gd₂O₂S:Eu	625	1×10³	0.14%@3 ms	60000	[73,85-86]
Gd₂O₂S:Eu,Tb,Ce,Ca	600	-	0.18%@30 ms	62000	[87]

Fig. 13 Schematic diagram of neutron imaging[95]

Table 4 Property of commonly used neutron imaging scintillation screen nuclides

Isotope	Reaction	Cross-section of thermal neutron adsorption/m²	Natural abundance/%	Ref.
⁶Li	³H, ⁴He	9.1×10^-26	7.5	[96-97]
¹⁰B	α, γ, ⁷Li	3.83×10^-25	19.9	[97]
¹¹³Cd	γ, e^-	2.1×10^-24	12.2	[98]
¹⁵⁵Gd	γ, e^-	6.09×10^-24	14.7	[96-97]
¹⁵⁷Gd	γ, e^-	2.55×10^-23	15.7	[96-97]

Table 5 Inorganic scintillators used in neutron imaging and their properties

Scintillator	Density/ (g·cm^-3)	λ_em/nm	Light yield		α/β ratio	τ/ns		Ref.
Scintillator	Density/ (g·cm^-3)	λ_em/nm	Neutron/(×10³, ph·neu.^-1)	γ/(×10³, ph·MeV^-1)	α/β ratio	Neutron	γ	Ref.
⁶Li-glass:Ce	2.5	395	6	4	0.3	70	70	[99]
⁶LiI:Eu	4.1	470	50	12	0.87	1.4×10³	1.4×10³	[6,100]
⁶LiF/ZnS:Ag	2.6	450	160	75	0.44	8×10⁴	100	[99,101]
LiYSiO₄:Ce	3.8	410	10	10	-	-	3.8×10⁴	[102]
⁶Li₆Gd(¹¹BO₃)₃:Ce	3.5	385, 415	40	25	0.32	-	200,800	[103]
Cs₂⁶LiYCl₆:Ce	3.3	380	70	22	0.66	100,10³	100,10³	[6,99]

Fig. 14 Principle diagram of X-CT imaging system[29]

Table 6 Inorganic scintillators for medical imaging and their properties

Scintillator	Density/(g·cm^-3)	Thickness to stop 99%*/mm	λ_em/nm	Light yield/ (ph·MeV^-1)	Decay time/μs	Afterglow/(% after 3 ms/100 ms)	Ref.
CsI:Tl	4.51	6.8	550	66000	1.22	>2/0.3	[16]
Bi₄Ge₃O₁₂	7.13	-	480	9000	0.30	0.005%@3 ms	[29]
CdWO₄	7.9	2.4	495	20000	5.00	<0.1/0.02	[16,29]
(Y,Gd)₂O₃:Eu,Pr	5.9	6.1	610	42000	1000	4.9/<0.01	[114]
Gd₂O₂S:Pr,Ce,F	7.3	2.9	510	35000	4	<0.1/<0.01	[29,85,115]
Gd₃(Ga,Al)₂O₁₂:Ce	6.2	-	540	58000	0.09-0.17	<0.01%@20 ms	[40]

Fig. 15 Gemstone scintillator material and detector module for Discovery CT750 HD[114]

Fig. 16 Photo of GOS:Pr,Ce,F scintillation ceramics prepared in Toshiba[116]

Fig. 17 Afterglow (a) and X-ray absorption efficiency (b) curves of German Siemens GOS (UFC ) scintillation ceramics[117] Colorful figures are available on website

Table 7 Performance of GOS:Pr,Ce(F) scintillation ceramics prepared in the major companies abroad and at home

Manufacturer	λ_em/nm	Light yield/(ph·MeV^-1)	Decay time/μs	Afterglow	Ref.
Siemens (Germany)	512	50000	3	0.01%@2.5-4 ms	[29,117]
Philips (Netherlands)	514	40000	3	0.02%@3 ms	[118]
Toshiba (Japan)	512	36000	3	0.08%@10 ms	[116]
Hitachi (Japan)	512	42000	3	0.001%@300 ms	[119]
Iray (China)	510	27000	3	0.1%@3 ms	[120]

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Rare Earth Doped Gd₂O₂S Scintillation Ceramics

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