CN113773838B - Application of europium-doped gadolinium silicate crystal and preparation method thereof - Google Patents
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Abstract
The invention discloses an application of europium-doped gadolinium silicate crystal and a preparation method thereof, wherein the europium-doped gadolinium silicate crystal is used as a thermoluminescent crystal, and the chemical expression of the europium-doped gadolinium silicate crystal is Gd 2‑x SiO 5 : xEu, wherein x is 0.03-0.07; the crystal has low-temperature and high-temperature heat release peaks; the low-temperature heat release peak is at 143 deg.C, the wavelength is 585nm, the trap depth is 1.16eV, and the frequency factor is 2.76 × 10 9 s ‑ (ii) a The high-temperature heat release peak is at 352 deg.C, the emission wavelength is 978nm, the trap depth is 1.61eV, and the frequency factor is 3.84 × 10 12 s ‑1 . The europium-doped gadolinium silicate thermoluminescent crystal is prepared by adopting an optical floating zone method, and comprises four steps of powder preparation, material rod preparation, crystal growth and annealing treatment, wherein the pulling speed can reach 15mm/h and the growth direction is [212]]. The europium-doped gadolinium silicate thermoluminescent crystal has good thermoluminescent performance and good radiation dose thermoluminescent linear response to gamma rays; the device can be used for the passage of cultural relics and the detection of radiation dose; the preparation process is simple and fast.
Description
Technical Field
The invention belongs to the technical field of novel crystal materials, and particularly relates to an application of a europium-doped gadolinium silicate crystal and a preparation method thereof.
Background
Gadolinium silicate crystal (Gd) 2 SiO 5 GSO) belongs to rare earth silicate, and is an optical crystal and base with excellent performanceA material. The GSO crystal can be directly used as a novel large-scale hadron collider detector (LHCF) and has an integral brightness of 5nb -1 Lower measurement LHCF in the zero degree region
The resolution of electromagnetic shower energy of high-energy particles generated in p-p collision is 3%, and the resolution of 100GeV electron energy is 123 μm; rebuilding pi 0 The peak mass resolution is 3.7%, and the operating fluctuations under high radiation conditions are less than 1% [ Ueno M, the performance of the new LHCf detector for the damping windows [ C ]].Proceedings of 2016 International Conference on Ultra-High Energy Cosmic Rays(UHECR2016)，2018：011048]. GSO crystal doped with Ce 3+ Is a high-efficiency scintillation crystal. The first GSO was grown by Takagi et al (Hitachi, Inc.) in 1983 by the Czochralski method: ce crystal. GSO: the Ce crystal has high radiation hardness (10) 9 rad which is 2 to 3 orders of magnitude higher than BGO), fast light attenuation (30 to 60ns), no deliquescence, high light output (1.3 times of BGO) and the like, and is applied to the fields of oil well detection, nuclear medicine, high-energy physics and the like [ Cuimei seal, and the like. 136]. GSO crystal Yb doping 3+ After ionization, it can be used as a solid laser [ Yan C, ZHao G, Su L, et al, growth and spectroscopic characterization of Yb: GSO single crystal. Condensed Matter, 2006, 18 (4): 1325]. The low symmetry structure of GSO crystal is favorable for Yb 3+ The splitting of ion energy level is that Yb can be made at present 3+ One of the materials with the largest energy level splitting. Compared with commercial YAG: the Nd laser crystal has wider emission bandwidth and higher output power; its room temperature unpolarized absorption spectrum consists of four absorption bands: 897nm, 922nm, 940nm and 976 nm; wherein 976nm ( 2 F 7/2 - 2 F 5/2 Transition between energy levels) is absorbed by a zero line, the emission intensity of the zero line is low, and the half-peak width is 19nm (far larger than YAG: 4nm half-peak width of Nd), which is advantageous for performing laser diode pumping [ zhujiangfeng, et al, diode pumping all-solid-state femtosecond Yb laser oscillator chinese laser, 2017, 44 (9): 0900001]。
In recent years, a novel GSO-based crystalBody development has become one of the hot spots in the design of crystalline materials. Mainly focuses on the development of novel scintillators and laser crystals, such as: doping Lu, Y, Gd and other elements into the matrix to form LGSO, LGYSO, GYSO and other mixed crystal base phases so as to improve Ce 3+ Doped scintillators or Yb 3+ Performance of doped laser Crystal [ Linzhi, Nd-doped 3+ silicate (GYSO/LSO/LYSO) Crystal laser characteristics research of Xiamen university, 2017](ii) a The following steps are repeated: to carry out Ce 3+ 、Yb 3+ Doping with other rare earth elements, developing novel crystals such as: tm is 3+ [ yellow apricot Thulium doped gadolinium lutetium silicate crystal growth and performance study. river south university, 2019]、Dy 3+ [Lisiecki R，et al.Optical spectra and luminescence dynamics of the Dy-doped Gd 2 SiO 5 single crystal.Applied Physics B，2010，98(2)：337.]、Pr 3+ [Kuleshov N V，et al.Spectroscopy，excited-state absorption and stimulated emission in Pr 3+ -doped Gd 2 SiO 5 and Y 2 SiO 5 crystals.Journal of Luminescence，1997，71(1)：27]；Er 3+ [Xu X，Zhao G，Wu F，et al.Growth and spectral properties of Er：Gd 2 SiO 5 crystal.Journal of crystal growth，2008，310(1)：156-159.]. In addition, the GSO crystal has high growth temperature, easily segregated components, color center (oxygen vacancy crystal is yellowish, gadolinium vacancy crystal is light blue), shoulder cracking and slow growth speed (1-2 mm/h); optimizing the existing pulling method [ Zong Y, ZHao G, Yan C, et al, growth and spectral properties of Gd 2 SiO 5 crystal codoped with Er and Yb.Journal of crystal growth，2006，294(2)：416-419，]Xujun Yb doped gadolinium silicate laser crystal and its preparation method, CN1694322A P]，2005]Optical float zone method (Gaoming Yuan, et al. Gd) 2 SiO 5 ：Eu 3+ Optical float zone method preparation and luminous performance research of crystal, artificial crystal science, 2020, 49 (5): 785]The preparation process, which improves the growth quality of the single crystal, increases the size and improves the growth speed, is also an important direction for researching the GSO-based crystal.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide a europium-doped gadolinium silicate crystal used as a thermoluminescent crystal and a preparation method thereof, wherein the thermoluminescent crystal has good thermoluminescent performance and good radiation dose thermoluminescent linear response to gamma rays; can be used for the detection of the passage of cultural relics and the radiation dose.
The invention is realized by the following technical scheme:
the invention provides an application of europium-doped gadolinium silicate crystals, wherein the europium-doped gadolinium silicate crystals are used as thermoluminescent crystals, and the chemical expression is as follows: gd (Gd) 2-x SiO 5 : xEu, wherein x is 0.03-0.07.
The pyroelectric crystal has two pyroelectric centers, one low temperature pyroelectric peak (at 143 deg.C, wavelength 585nm, trap depth 1.16eV, and frequency factor 2.76 × 10 9 s -1 ) A high-temperature heat release peak (at 352 deg.C, emission wavelength 978nm, trap depth 1.61eV, frequency factor 3.84 × 10 12 s -1 ). The low-temperature thermoluminescence peak (143 ℃) has good radiation dose thermoluminescence linear response to gamma rays.
The thermoluminescent crystal is prepared by adopting an optical floating zone method, and comprises four steps of powder preparation, material rod preparation, crystal growth and annealing treatment, and specifically comprises the following steps:
(1) preparing powder: weighing a certain amount of Gd according to a stoichiometric ratio 2 O 3 (AR)、Eu 2 O 3 (AR) and SiO (AR) raw materials are mixed for 3 hours by ball milling; calcining for 2h after the temperature is increased to 1300 ℃ at the heating rate of 5 ℃/min, and cooling to the room temperature along with the furnace; grinding the mixture to form powder with a particle size interval of 1.17-11.0 mu m and a median particle size of 4.19 mu m, and determining the phase of the powder to be Gd by XRD characterization 2 SiO 5 ；
(2) Preparing a material rod: carrying out cold isostatic pressing on the powder prepared in the step (1) under the condition of more than 100Mpa to form a right cylindrical rod body with uniform thickness and diameter of phi 6mm and length of about 70-80 mm; then presintering at 1500 ℃ for 3h to obtain a material bar;
(3) crystal growth: loading a blanking rod and a feeding rod into the optical floating zone method furnace, and adjusting the centers of the feeding rod and the blanking rod to be in a vertical central line; sealing the growth chamber by using a quartz tube, and rotating at the rotating speed of 15r/min in the air atmosphere; the pulling speed is 15mm/h, the growth direction is [212] when the crystal grows, so that a melting zone keeps a stable bowl-shaped model in the crystal growth, and the crystal does not crack in the crystal growth;
(4) annealing treatment: in the air atmosphere, the heating rate is 50-100 ℃/h, the cooling rate is 30-50 ℃/h, and the temperature is maintained at 1400 ℃ for 20 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the europium-doped gadolinium silicate thermoluminescent crystal has good thermoluminescent performance and good radiation dose thermoluminescent linearity corresponding to gamma rays; can be used for the detection of the passage of cultural relics and the radiation dose.
(2) The europium-doped gadolinium silicate thermoluminescent crystal preparation process is simple in process and high in speed.
Drawings
FIG. 1 is Gd in example 1 of the present invention 1.95 SiO 5 : 0.05Eu thermoluminescent crystal slice.
FIG. 2 is Gd in example 1 of the present invention 1.95 SiO 5 : 0.05Eu thermoluminescent crystal growth time melting zone photograph.
FIG. 3 is Gd in example 1 of the present invention 1.95 SiO 5 : 0.05Eu thermoluminescent crystal at gamma dose of 0.1kGy and temperature rise rate of 5 ℃ s -1 A pyroelectric spectrum under the condition, wherein (a) the pyroelectric spectrum is three-dimensional (temperature-intensity-wavelength), and (b) the pyroelectric spectrum is corresponding to two-dimensional (temperature-intensity).
FIG. 4 is Gd in example 1 of the present invention 1.95 8iO 5 : linear response curve of low-temperature heat release peak intensity of 0.05Eu thermoluminescent crystal under different gamma doses.
FIG. 5 is Gd in example 1 of the present invention 1.95 SiO 5 : 0.05Eu thermoluminescent crystal, wherein (a) is after annealing and (b) is before annealing.
FIG. 6 shows the temperature rise rate of 5 ℃ s at γ dose of 0.1kGy in examples 1, 2 and 3 of the present invention -1 Two-dimensional (temperature-intensity) pyroelectric spectrum under the condition.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1 Gd 1.95 SiO 5 : preparation and performance of 0.05Eu thermoluminescent crystal
Gd 1.95 SiO 5 : the preparation steps of the 0.05Eu thermoluminescent crystal comprise:
(1) preparation of powder with Gd 2 O 3 (AR)、Eu 2 O 3 (AR), SiO (AR) as raw materials; weighing the corresponding amount of powder in a stoichiometric ratio (Gd/Eu/Si ═ 95/5/100); ball milling and mixing for 3 h; calcining at 1300 deg.C for 2h (heating rate of 5 deg.C/min), and furnace cooling to room temperature; grinding to form powder with a particle size interval of 1.17-11.0 μm and a median particle size of 4.19 um;
(2) preparing a material rod: carrying out cold isostatic pressing on the powder under the condition of more than 100Mpa to form a right cylindrical rod body with uniform thickness and diameter of phi 6mm and length of about 70-80 mm; then presintering at 1500 ℃ for 3h to obtain a material bar;
(3) crystal growth: the seed crystal rod is a blanking rod, the feeding rod is a feeding rod, and the center of the feeding rod is adjusted to be on a vertical central line; sealing the growth chamber by a quartz tube; growing the material bar into a crystal at a rotating speed of 15r/min and a drawing speed of 15mm/h in an air atmosphere, wherein the growth direction of the crystal is [212 ];
(4) annealing treatment: under the air atmosphere, the heating rate is 50-100 ℃/h, the cooling rate is 30-50 ℃/h, and the temperature is maintained at 1400 ℃ for 20 hours.
The crystal was sliced axially for subsequent testing using a diamond wire cutter model UNIPOL-810, the slices being shown in fig. 1.
Adopting FJ-427ALTL measuring instrument (Beijing nuclear instrument factory) of Beijing nuclear instrument factory with a heating rate of 5 ℃ s -1 The pyroelectric spectrum (300-675K) measured under the gamma dose of 0.1kGy is shown in figure 2, the linear response characteristic of the low-temperature pyroelectric peak intensity under the gamma dose is shown in figure 3, and the residual stress test is shown in figure 4.
Example 2 Gd 1.95 SiO 5 : 0.07Eu thermoluminescent crystal preparation and performance.
Gd 1.95 SiO 5 : the preparation steps of the 0.07Eu thermoluminescent crystal comprise:
(1) powder preparation: with Gd 2 O 3 (AR)、Eu 2 O 3 (AR), SiO (AR) as raw materials; weighing the corresponding amount of powder in a stoichiometric ratio (Gd/Eu/Si ═ 95/7/100); ball-milling and mixing for 3 h; calcining at 1300 deg.C for 2h (heating rate of 5 deg.C/min), and furnace cooling to room temperature; grinding to form powder with a particle size interval of 1.17-11.0 μm and a median particle size of 4.19 um;
(2) preparing a material rod: carrying out cold isostatic pressing on the powder under the condition of more than 100Mpa to form a right cylindrical rod body with uniform thickness and diameter of phi 6mm and length of about 70-80 mm; then presintering at 1500 ℃ for 3h to obtain a material bar;
(3) crystal growth: the seed crystal rod is a blanking rod, the feeding rod is a feeding rod, the center of the feeding rod is adjusted to be in a vertical central line, a quartz tube is used for sealing a growth chamber, the feeding rod grows into crystals at the rotating speed of 15r/min and the stretching speed of 15mm/h in the air atmosphere, and the growth direction is [212] during crystal growth;
(4) annealing treatment: under the air atmosphere, the heating rate is 50-100 ℃/h, the cooling rate is 30-50 ℃/h, and the temperature is maintained at 1400 ℃ for 20 hours.
The crystal was sliced axially for subsequent testing using a UNIPOL-810 diamond wire cutter, and the two-dimensional heat release spectrum at a gamma dose of 0.1kGy at a temperature rise rate of 5 ℃/s is shown in fig. 5.
Example 3 Gd 1.95 SiO 5 : preparation and performance of 0.03Eu thermoluminescent crystal
Gd 1.95 SiO 5 : the preparation method of the 0.03Eu thermoluminescent crystal comprises the following steps:
(1) preparing powder: with Gd 2 O 3 (AR)、Eu 2 O 3 (AR), SiO (AR) as raw materials. Weighing the corresponding amount of powder in a stoichiometric ratio (Gd/Eu/Si ═ 95/3/100); ball milling and mixing for 3 h; calcining at 1300 deg.C for 2h (heating rate of 5 deg.C/min), and furnace cooling to room temperature; grinding to form powder with a particle size interval of 1.17-11.0 μm and a median particle size of 4.19 um;
(2) preparing a material rod: carrying out cold isostatic pressing on the powder under the condition of more than 100Mpa to form a right cylindrical rod body with uniform thickness and diameter of phi 6mm and length of about 70-80 mm; then presintering at 1500 ℃ for 3h to obtain a material bar;
(3) crystal growth: the seed crystal rod is a blanking rod, the feeding rod is a feeding rod, and the center of the feeding rod is adjusted to be on a vertical central line. A quartz tube is used for sealing a growth chamber, the charge bar is grown into a crystal at the rotating speed of 15r/min and the drawing speed of 15mm/h in the air atmosphere, and the growth direction of the crystal is [212 ];
(4) and (3) annealing treatment: under the air atmosphere, the heating rate is 50-100 ℃/h, the cooling rate is 30-50 ℃/h, and the temperature is maintained at 1400 ℃ for 20 hours.
The crystal was sliced axially for subsequent testing using a UNIPOL-810 diamond wire cutter, and the two-dimensional heat release spectrum at a gamma dose of 0.1kGy at a temperature rise rate of 5 ℃/s is shown in fig. 5.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (1)
1. Use of europium-doped gadolinium silicate crystals, characterized in that: the europium-doped gadolinium silicate crystal is used as a thermoluminescent crystal, and the chemical expression of the europium-doped gadolinium silicate crystal is Gd 2-x SiO 5 xEu, wherein x = 0.03-0.07; the pyroelectric crystal has two pyroelectric centers of a low-temperature pyroelectric peak and a high-temperature pyroelectric peak; the low-temperature heat release peak is at 143 deg.C, the wavelength is 585nm, the trap depth is 1.16eV, and the frequency factor is 2.76 × 10 9 s - (ii) a The high-temperature heat release peak is at 352 deg.C, the emission wavelength is 978nm, the trap depth is 1.61eV, and the frequency factor is 3.84 × 10 12 s -1 (ii) a The europium-doped gadolinium silicate crystal used as the thermoluminescent crystal is prepared by adopting an optical floating zone method, and comprises four steps of powder preparation, material rod preparation, crystal growth and annealing treatment, wherein the crystal growth is carried out in an air atmosphere, the pulling growth speed is 15mm/h, and the growth direction is [212]]。
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Non-Patent Citations (3)
| Title |
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| Gd2SiO5:Eu3+晶体的光学浮区法制备及发光性能研究;高明远等;《人工晶体学报》;20200531;第49卷(第5期);第785-793页 * |
| Luminescence and structural properties of Gd2SiO5:Eu3+ phosphors synthesized from the modified solid state method;Yogita Parganiha et al.;《Ceramics International》;20170411;第43卷;第9084-9091页 * |
| Thermally stimulated luminescence of undoped and Ce3+-doped Gd2SiO5 and (Lu,Gd)2SiO5 single crystals;V. Bondar et al.;《Journal of Luminescence》;20141127;第159卷;第229-237页 * |
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