CN108892377B - Ultrafast decay time scintillation glass and preparation method thereof - Google Patents

Ultrafast decay time scintillation glass and preparation method thereof Download PDF

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CN108892377B
CN108892377B CN201810875133.1A CN201810875133A CN108892377B CN 108892377 B CN108892377 B CN 108892377B CN 201810875133 A CN201810875133 A CN 201810875133A CN 108892377 B CN108892377 B CN 108892377B
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decay time
melting
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sio
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CN108892377A (en
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李德源
牛蒙青
李华
张小东
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China Institute for Radiation Protection
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00Compositions for glass with special properties
    • C03C4/12Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/02Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths

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Abstract

The invention relates to ultrafast decay time scintillation glass, which comprises SiO as a material component2,Li2O,Al2O3,Ce2O3Wherein, SiO260 to 80 percent by mass of Li28-20% of O and Al2O35 to 20 percent of Ce2O3The mass percentage of the component (A) is 1-4%. The preparation method of the ultrafast decay time scintillation glass comprises the following steps: (a) flash glass compounding with SiO2,Li2O,Al2O3,Ce2O3The raw materials are fully mixed according to the content to obtain glass ingredients; (b) melting the scintillation glass, namely putting the ingredients prepared in the step (a) into a container for melting, stirring during melting, and pouring the molten glass into a mold for solidification; (c) and (4) annealing the scintillation glass, namely moving the glass sample solidified in the step (b) into a muffle furnace for annealing for 3-4 hours, and cooling to obtain the glass sample. The invention designs a new matrix glass component, takes Ce as a luminescence center, and prepares ultrafast decay time scintillation glass with short decay time of 7.5ns and long decay time of 34.3 ns.

Description

Ultrafast decay time scintillation glass and preparation method thereof
Technical Field
The invention relates to a scintillator material and a preparation method thereof, in particular to ultrafast decay time scintillation glass taking Ce as a luminescence center and a preparation method thereof.
Background
With the development of new technologies in the fields of high-energy physics and nuclear physics, scientists have put forward new requirements on scintillators, and especially put forward higher requirements on the irradiation resistance, decay time characteristic and the like of the scintillators in high-intensity radiation fields. The traditional scintillation crystal (such as NaI: Tl, CsI: Tl) and the like can not meet the requirements. The scintillation glass taking rare earth ions as a luminescence center has the characteristics of difficult deliquescence, thermal shock resistance and capability of drawing a scintillation panel, and is widely applied to the fields of high-energy physics and nuclear physics.
The scintillation glass with Ce as the luminescence center has the characteristic of short decay time, mainly because the emission of Ce belongs to 5d-4f transition, and the energy level difference is the smallest in lanthanide, and is widely used for rapid time measurement. However, the decay time of the existing scintillation glass taking Ce as a luminescence center is about 50ns-100ns, and the decay time is mainly influenced by the components and the pH value of the matrix glass.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides ultrafast decay time scintillation glass capable of being applied to the requirements of fast time resolution experiments in the fields of high-energy physics and nuclear physics and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
an ultrafast decay time scintillation glass comprises SiO as material component2,Li2O,Al2O3,Ce2O3Wherein, SiO260 to 80 percent by mass of Li28-20% of O and Al2O35 to 20 percent of Ce2O3The mass percentage of the component (A) is 1-4%.
Further, the SiO2,Al2O3、Li2O、Ce2O3The mass percentages of the components are respectively 60%, 18%, 19.6% and 2.4%.
Further, the SiO2,Al2O3、Li2O、Ce2O3The mass percentages of the components are respectively 72.9%, 8.5%, 16.5% and 2.1%.
Further, the SiO2,Al2O3、Li2O、Ce2O3Respectively 75.5%, 10%, 12% and 2.5%.
Further, the SiO2,Al2O3、Li2O、Ce2O3Mass ofThe percentages are 77%, 7%, 15% and 1%, respectively.
Further, the SiO2,Al2O3、Li2O、Ce2O3Respectively 80%, 7%, 11.1% and 1.9% by mass.
The preparation method of the ultrafast decay time scintillation glass comprises the following steps:
(a) flash glass compounding with SiO2,Li2O,Al2O3,Ce2O3The glass batch is obtained by fully mixing the raw materials according to the content.
(b) Melting the scintillation glass, namely putting the ingredients prepared in the step (a) into a container for melting, stirring during melting, and pouring the molten glass into a mold for solidification;
(c) and (4) annealing the scintillation glass, namely moving the glass sample solidified in the step (b) into a muffle furnace for annealing for 3-4 hours, and cooling to obtain the glass sample.
Further, the melting temperature of the melting process in the step (b) is 1200-1400 ℃, and the melting time is 3-4 hours.
Further, the container of the melting process in the step (b) comprises a platinum crucible and an electric furnace, and the ingredients prepared in the step (a) are placed in the platinum crucible and heated by the electric furnace.
Further, the mold is a stainless steel mold.
The invention has the beneficial effects that: the invention designs a new matrix glass component, takes Ce as a luminescence center, and prepares ultrafast decay time scintillation glass with short decay time of 7.5ns and long decay time of 34.3 ns. The ultrafast decay time scintillation glass has the advantages of simple melting process, good uniformity of prepared materials and the like, can meet the requirement of fast time detection, and can also be used for preparing scintillation fiber panels for the experimental requirements of fast time resolution and high spatial resolution.
Drawings
FIG. 1 is an emission spectrum of example 1;
FIG. 2 is a graph of the decay time of example 1;
fig. 3 is a decay time table of example 1.
Detailed Description
The invention is further described with reference to the accompanying drawings and the detailed description below:
an ultrafast decay time scintillation glass comprises SiO as material component2,Li2O,Al2O3,Ce2O3Wherein, SiO260 to 80 percent by mass of Li210 to 20 percent of O and Al2O35 to 20 percent of Ce2O3The mass percentage of the component (A) is 1-4%.
The preparation method of the ultrafast decay time scintillation glass comprises the following steps:
(a) preparing scintillation glass: the amount of the introduced material (raw material) was calculated according to the weight percentage of the glass composition of the formulation design. Wherein SiO is2Introduced as high-purity quartz sand, Al2O3Introduced as analytically pure aluminum hydroxide, Li2O was introduced as analytically pure lithium carbonate, Ce2O3The cerium nitrate was introduced as analytically pure hexahydrate and the raw materials were put into a mill and mixed thoroughly.
(b) Melting the flash glass, namely putting the ingredients prepared in the step (a) into a container for melting, stirring the ingredients during melting, pouring the melted glass into a mold for solidification, wherein the mold is a stainless steel mold;
(c) and (4) annealing the scintillation glass, namely moving the glass sample solidified in the step (b) into a muffle furnace for annealing for 3-4 hours, and cooling to obtain the glass sample.
Further, the melting temperature of the melting process in the step (b) is 1200-.
The specific embodiment is as follows:
example 1
The formula design is that SiO in the formula2,Al2O3、Li2O、Ce2O3The mass percent of the components is 77 percent,7%,15%,1%。
Preparing scintillation glass: high-purity quartz sand, analytically pure aluminum hydroxide, analytically pure aluminum carbonate and analytically pure cerous nitrate hexahydrate are adopted, and the raw materials are put into grinding and fully mixed.
Melting glass:
placing the glass ingredients into a platinum crucible, melting the glass in an electric furnace in air atmosphere at 1500 ℃ for 1.5 hours, and pouring the melted glass into a stainless steel mold for natural molding.
Glass annealing:
the glass mold was placed in a muffle furnace at a heating temperature of 450 ℃. The incubation time was 1 hour. After the incubation was finished, the sample was cooled to room temperature.
Glass sample emission spectra and decay time measurements
The emission spectrum of the ultrafast decay time scintillating glass is shown in figure 1, and the excitation wavelength of the scintillating glass is 300 nm. The emission wavelength is around 375 nm.
The decay time measurement of the ultrafast decay time scintillating glass of the present invention is shown in fig. 2. As shown in FIG. 3, the fast decay time of the scintillation glass was 7.5ns and the long decay time was 34.3ns after the fitting analysis.
Examples 2 to 5
The components used in examples 2-5 are shown in Table 1.
TABLE 1
Figure BDA0001753053390000041
Figure BDA0001753053390000051
Examples 2 to 5 used the same melt processing regime and test conditions as in example 1. The results of obtaining the luminescence spectra and the scintillation decay times of examples 2-5 are shown in Table 2.
TABLE 2
Figure BDA0001753053390000052
The invention designs a new matrix glass component, takes Ce as a luminescence center, and prepares ultrafast decay time scintillation glass with short decay time of 7.5ns and long decay time of 34.3 ns. The ultrafast decay time scintillation glass has the advantages of simple melting process, good uniformity of prepared materials and the like, can meet the requirement of fast time detection, and can also be used for preparing scintillation fiber panels for the experimental requirements of fast time resolution and high spatial resolution.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (3)

1. A preparation method of ultrafast decay time scintillation glass is characterized by comprising the following steps:
(a) flash glass compounding with SiO2,Li2O,Al2O3,Ce2O3Fully mixing the raw materials according to the corresponding content to obtain a glass ingredient;
wherein, SiO272.9-75.5% by mass of Li216.5 to 20 percent of O and Al2O35-8.5% by mass of Ce2O3The mass percentage of the component (A) is 1-4%;
(b) melting the scintillation glass, namely putting the ingredients prepared in the step (a) into a container for melting, stirring during melting, and pouring the molten glass into a mold for solidification;
(c) annealing the scintillation glass, namely moving the glass sample solidified in the step (b) into a muffle furnace for annealing for 3-4 hours, and cooling to obtain the glass sample;
the melting temperature of the melting procedure in the step (b) is 1200-1400 ℃, and the melting time is 3-4 hours;
the container of the melting procedure in the step (b) comprises a platinum crucible and an electric furnace, and the ingredients prepared in the step (a) are placed in the platinum crucible and heated by the electric furnace.
2. The method of claim 1, wherein the mold is a stainless steel mold.
3. The method of claim 1, wherein the SiO is in the form of a glass with ultra-fast decay time2,Al2O3、Li2O、Ce2O3The mass percentages of the components are respectively 72.9%, 8.5%, 16.5% and 2.1%.
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JPH0940440A (en) * 1995-07-25 1997-02-10 Nikon Corp Scintillator glass
CN100526244C (en) * 2006-08-09 2009-08-12 中国建筑材料科学研究总院 Glass scintillator for thermal neutron detection and its preparation method

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