CN108193274B - Compound tungstate scintillation crystal and preparation method thereof - Google Patents

Compound tungstate scintillation crystal and preparation method thereof Download PDF

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CN108193274B
CN108193274B CN201711223821.1A CN201711223821A CN108193274B CN 108193274 B CN108193274 B CN 108193274B CN 201711223821 A CN201711223821 A CN 201711223821A CN 108193274 B CN108193274 B CN 108193274B
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scintillation crystal
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CN108193274A (en
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杜飞
潘建国
潘尚可
张建裕
章政
栗茹
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Ningbo University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/32—Titanates; Germanates; Molybdates; Tungstates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method

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Abstract

The invention discloses a compound tungstate scintillation crystal and a preparation method thereof, and is characterized in that the chemical structural formula of the scintillation crystal is CdGdxLa2‑x（WO4）4Wherein x =0.2,0.4,0.6,0.8 or 1.0, and the preparation method comprises the following specific steps: 1) mixing the raw materials of CdO and Gd2O3、La2O3And WO3Placing the raw materials in a muffle furnace to remove moisture, then weighing according to the molar ratio in the chemical formula, fully grinding and tabletting the powder, transferring the powder into a ceramic crucible, sintering the powder in the muffle furnace, and re-grinding and tabletting the sinter to obtain a polycrystalline ingot; 2) heating by adopting a single crystal pulling furnace and a medium-frequency induction heating mode, N2Adopting a platinum wire for spontaneous nucleation in a protective atmosphere; the pulling speed and the crystal are controlled in the growth stage, and the compound tungstate scintillation crystal is obtained after the growth is finished, and has the advantages of high density, fast attenuation, easy growth and good luminescence property.

Description

Compound tungstate scintillation crystal and preparation method thereof
Technical Field
The invention relates to a tungstate scintillation crystal, in particular to a compound tungstate scintillation crystal and a preparation method thereof.
Background
Inorganic scintillation crystals are optically functional materials that produce pulsed light emission under the action of high-energy radiation, often combined with photomultiplier
The detector elements such as a tube (PMT), a silicon photodiode and the like (SPD) can realize high-energy ray precise detection under various technical conditions based on the light-light conversion effect of the scintillation crystal, so that a series of modern high and new technologies based on ray detection imaging are developed, and the detector elements are widely applied to the fields of high-energy physics, nuclear physics, safety inspection, industrial nondestructive detection, nuclear medicine imaging, geological exploration and the like.
The compound tungstate scintillation crystal is an important intrinsic type scintillator, and can emit fluorescence under the activation of rays or high-energy particles without doping other active ions. Kroger just paired MWO since 19484(M = Ca, Cd, Li, Mg, Ba, Na, Pb, Zn, Sr) A series of studies on the luminescence properties of tungstates were made, indicating that CdWO4、ZnWO4、CaWO4、BaWO4Has good scintillation performance. Most tungstate crystals have the advantages of high density, high luminous efficiency, strong irradiation resistance, no deliquescence, low price and the like.
The existing compound tungstate scintillation crystal has CdLa2（WO4）4Crystals, which have excellent light emitting properties, are more suitable for application in the field of scintillation crystals, but are more difficult to grow. The national Bibi report CdGd2（WO4）4The structure and the magnetism of the compound are that CdGd is successfully grown out by a pulling method from the Sun Guifang2（WO4）4A single crystal which does not emit light under excitation of high-energy rays but grows relatively to CdLa2（WO4）4It is much easier. Nd was reported by foreign V. Baumer3+：CdLa2（WO4）4The crystal is used as a laser crystal and is grown by a pulling method, but the grown crystal is in a faint yellow ceramic shape and is opaque, and the surface of the crystal is provided with a layer of wrapping matter, so that the quality is poor.
Disclosure of Invention
The invention aims to provide a high-density and fast-attenuation compound tungstate scintillation crystal which is easy to grow and has good luminescence property and a preparation method thereof.
The present invention is adopted to solve the above technical problemsThe technical scheme is as follows: a composite tungstate scintillation crystal with CdGd as its chemical structural formulaxLa2-x（WO4）4Wherein x =0.2,0.4,0.6,0.8, or 1.0.
The preparation method of the compound tungstate scintillation crystal comprises the following specific steps:
(1) high-temperature solid-phase synthesis of polycrystalline material ingot
Mixing the raw materials of CdO and Gd2O3、La2O3And WO3Placing the raw materials in a muffle furnace, heating at 200 ℃ for 8-10 hours until a small amount of water adsorbed in the raw materials is removed, then weighing according to the molar ratio in the chemical formula, fully grinding the powder, pressing the ground powder into a wafer with the diameter of 40-60mm and the thickness of 4-6mm under the pressure of 10-15Mpa by using a tablet press, transferring the wafer into a ceramic crucible, sintering at 750 ℃ for 12 hours in the muffle furnace, re-grinding and tabletting the sinter, and sintering at 900 ℃ for 12 hours in the muffle furnace again to ensure that the raw materials react more fully to obtain a white compact polycrystalline ingot;
(2) crystal growth by Czochralski method
Growing the polycrystalline ingot obtained in the step (1) by adopting a single crystal pulling furnace, heating in a medium-frequency induction heating mode, and carrying out N2Performing spontaneous nucleation on the platinum wire in a protective atmosphere; controlling the pulling speed to be 2.0-2.5 mm/h and the crystal rotation speed to be 15-17r/min in the growth stage, and cooling to room temperature at the rate of 30-50 ℃ after the growth is finished to obtain the compound tungstate scintillation crystal, wherein the chemical structural formula of the compound tungstate scintillation crystal is CdGdxLa2-x（WO4）4X =0.2,0.4,0.6,0.8, or 1.0.
Compared with the prior art, the invention has the advantages that: the invention relates to a compound tungstate scintillation crystal and a preparation method thereof, and the quality of the scintillation crystal is higher than that of CdLa2（WO4）4Is easier to grow and has a higher luminous intensity ratio under X-rays than CdGd2（WO4）4It is much stronger. Its advantage is high density of 7.5g/cm3(ii) a Relatively fast decay, with x of 0.2, combiningThe decay time of the object was 410.5ns, whereas when x increased to 1.0, its decay time had decreased to 271.2 ns; the luminescent material has good luminescent property; the melting point is about 1100 ℃, so that the growth is easy and the energy consumption in the growth process is reduced; the photoluminescence/X-ray fluorescence spectrum can be well matched with a photomultiplier for application according to the range and peak value display of the photoluminescence spectrum and the X-ray excitation emission spectrum.
Drawings
FIG. 1 shows CdGd grown by CdGd pulling method according to the invention0.4La1.6(WO4)4A crystal structure diagram;
FIG. 2 shows CdGd grown by the pulling method of the invention0.6La1.4(WO4)4A crystal structure diagram;
FIG. 3 is an X-ray powder diffraction pattern of a double tungstate scintillation crystal prepared in examples 1-5 of this invention;
FIG. 4 is a density plot of a double tungstate scintillation crystal prepared in examples 1-5 of this invention;
FIG. 5 is an X-ray excitation emission spectrum of a double tungstate scintillation crystal prepared in examples 1-5 of this invention;
FIG. 6 is a graph of the photoluminescence decay curves of multiple tungstate scintillation crystals prepared in examples 1-5 of this invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Detailed description of the preferred embodiments
Example 1
A composite tungstate scintillation crystal with CdGd as its chemical structural formula0.2La1.8（WO4）4The preparation method comprises the following specific steps:
(1) high-temperature solid-phase synthesis of polycrystalline material ingot
Mixing the raw materials of CdO and Gd2O3、La2O3And WO3Placing the raw material in a muffle furnace, heating at 200 deg.C for 8-10 hr to remove small amount of water adsorbed in the raw material, weighing according to the molar ratio in the chemical formula, and weighingFully grinding the powder, pressing the ground powder into a wafer with the diameter of 40-60mm and the thickness of 4-6mm under the pressure of 10-15Mpa by using a tablet press, transferring the wafer into a ceramic crucible, sintering the wafer in a muffle furnace at 750 ℃ for 12 hours, re-grinding and tabletting the sintered material, and sintering the sintered material in the muffle furnace at 900 ℃ for 12 hours to ensure that the raw materials react more fully to obtain a white compact polycrystalline ingot; wherein the initial raw materials are respectively CdO with the purity of 99.95 percent and Gd2O3Purity of 99.995%, La2O3Purity of 99.999%, WO3The purity is 99.999%;
(2) crystal growth by Czochralski method
Growing the polycrystalline ingot obtained in the step (1) by adopting an LJ-J50 type single crystal pulling furnace, heating in a medium-frequency induction heating mode, and carrying out N2Performing spontaneous nucleation on the platinum wire in a protective atmosphere; controlling the pulling speed to be 2.0-2.5 mm/h and the crystal rotation speed to be 15-17r/min in the growth stage, and cooling to room temperature at the rate of 30-50 ℃ after the growth is finished to obtain the compound tungstate scintillation crystal, wherein the chemical structural formula of the compound tungstate scintillation crystal is CdGd0.2La1.8（WO4）4。
Example 2
The difference from the above example 1 is that: the chemical structural formula of the scintillation crystal is CdGd0.4La1.6（WO4）4。
Example 3
The difference from the above example 1 is that: the chemical structural formula of the scintillation crystal is CdGd0.6La1.4（WO4）4。
Example 4
The difference from the above example 1 is that: the chemical structural formula of the scintillation crystal is CdGd0.8La1.2（WO4）4。
Example 5
The difference from the above example 1 is that: the chemical structural formula of the scintillation crystal is CdGdLa (WO)4）4。
Second, analysis of experimental results
Will be at the topCdGd synthesized in the following examples 1 to 5xLa2-x（WO4）4Wherein X is 0.2,0.4,0.6,0.8 or 1.0, respectively, and the synthesized CdLa is subjected to X-ray powder diffractometer type Bruker D8 Foucus, Germany2(WO4)4XRD test is carried out on the raw material powder, a radiation source is Cu target K α for radiation, the working current is 40 mA, the voltage is 40kV, the scanning range is 10-80 degrees, an F-4500 type fluorescence spectrometer produced by Nippon Hitachi company is used for testing the photoluminescence spectrum of the crystal at room temperature, the excitation wavelength is 296nm, an X-ray excitation emission spectrometer is automatically built for testing the X-ray excitation emission spectrum, a tungsten target X-ray tube is used as an excitation light source, a photomultiplier tube is used for detecting the emission light, and an FL3-111 fluorescence spectrometer is used for testing the photoluminescence attenuation time.
FIG. 1 and FIG. 2 show CdGd spontaneously nucleated by CdGd growth according to the present invention using CdLaw method0.4La1.6(WO4)4With CdGd0.6La1.4(WO4)4The two crystals are semitransparent and have cracks inside, and can be adjusted and controlled by the process technologies of pulling speed, rotating speed, temperature field and the like in the growth process, and the light transmittance and mass ratio of the crystals are reported as CdLa2（WO4）4The yellowish ceramic shape is obviously improved. In addition, CdGd0.6La1.4(WO4)4The top of (a) is light yellow, which should be such that during growth the material evaporates onto the platinum wire, which then sinks into solution, and the diffusion of the volatiles results in the formation of a coating on the shoulder. XRD test is carried out on the volatile matter obtained in the growth process, and the volatile matter is mainly CdO.
FIG. 3 shows a series of CdGd produced by sintering at 900 deg.CxLa2-x（WO4）4XRD contrast of (x =0.2,0.4,0.6,0.8, 1.0). From the figure we can see that the position of the peak in the curve does not change significantly with the increase of x, indicating that CdLa2（WO4）4With CdGd2（WO4）4Has the same crystal form, belongs to a tetragonal scheelite structure, and can form consistent melting at high temperatureThe compound is beneficial to the growth of crystals.
FIG. 4 is a density curve calculated from the crystal structure and unit cell parameters, and it can be seen that the density of the crystals is 7.5g/cm3The above is higher in density than general halide crystals, germanates and the like, and the density tends to increase as x increases, and the high density has a relatively strong ability to block charged particles.
FIG. 5 is an X-ray excited emission spectrum of mixed crystal, the whole spectrum has a relatively wide luminescence band in the wavelength range of 300-600nm, and is a symmetrical structure, the peak position is about 470nm, the luminescence band is generated by the radiative transition generated by the transition of the electron on the 2P orbital of the oxygen atom in tungstate ion to the 5d orbital of tungsten atom, and then the electron returns to the ground state from the excited state, which is the luminescence mechanism of the series of compound tungstate. The luminescence mechanism, because of the electron transition in tungstate radical, can emit light under the excitation of X-ray, and can be used as scintillation crystal, which is an important performance parameter of scintillation crystal.
FIG. 6 shows CdGdxLa2-x（WO4）4Fitted by single photon counting. It can be seen from the figure that when x is 0.2, the decay time of the compound is 410.5ns, and when x is increased to 1.0, the decay time is reduced to 271.2ns, which is more than the CdWO widely used in the field of security inspection4(842ns) is fast, and fast decay reduces clogging in the crystal due to energy build-up, maintains good signal-to-noise ratio, improves temporal resolution, and is therefore beneficial for scintillation crystals.
In summary, the invention provides the tungstate oxide mixed crystal CdGd growing togetherxLa2-x（WO4）4(x =0.2,0.4,0.6,0.8, 1.0) material has excellent properties of high density, fast decay, easy growth and good light emitting properties.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.

Claims (2)

1. A double tungstate scintillation crystal, characterized in that: the chemical structural formula of the scintillation crystal is CdGdxLa2-x（WO4）4Wherein x =0.2,0.4,0.6,0.8, or 1.0.
2. A method for preparing a double tungstate scintillation crystal as recited in claim 1, which comprises the following steps:
(1) high-temperature solid-phase synthesis of polycrystalline material ingot
Mixing the raw materials of CdO and Gd2O3、La2O3And WO3Placing the raw materials in a muffle furnace, heating at 200 ℃ for 8-10 hours until a small amount of water adsorbed in the raw materials is removed, then weighing according to the molar ratio in the chemical formula, fully grinding the powder, pressing the ground powder into a wafer with the diameter of 40-60mm and the thickness of 4-6mm under the pressure of 10-15Mpa by using a tablet press, transferring the wafer into a ceramic crucible, sintering at 750 ℃ for 12 hours in the muffle furnace, re-grinding and tabletting the sinter, and sintering at 900 ℃ for 12 hours in the muffle furnace again to ensure that the raw materials react more fully to obtain a white compact polycrystalline ingot;
(2) crystal growth by Czochralski method
Growing the polycrystalline ingot obtained in the step (1) by adopting a single crystal pulling furnace, heating in a medium-frequency induction heating mode, and carrying out N2Performing spontaneous nucleation on the platinum wire in a protective atmosphere; controlling the pulling speed to be 2.0-2.5 mm/h and the crystal rotation speed to be 15-17r/min in the growth stage, and cooling to room temperature at the rate of 30-50 ℃ after the growth is finished to obtain the compound tungstate scintillation crystal, wherein the chemical structural formula of the compound tungstate scintillation crystal is CdGdxLa2-x（WO4）4X =0.2,0.4,0.6,0.8, or 1.0.
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