CN105669023A - Glass scintillator, preparation method thereof and thermal neutron detection method - Google Patents

Glass scintillator, preparation method thereof and thermal neutron detection method Download PDF

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CN105669023A
CN105669023A CN201610015753.9A CN201610015753A CN105669023A CN 105669023 A CN105669023 A CN 105669023A CN 201610015753 A CN201610015753 A CN 201610015753A CN 105669023 A CN105669023 A CN 105669023A
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glass
time
glass scintillator
scintillator
founded
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CN105669023B (en
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朱永昌
李佳宇
刘峻
关铭
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China Building Materials Academy CBMA
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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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • 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
    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T3/00Measuring neutron radiation
    • G01T3/06Measuring neutron radiation with scintillation detectors

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Luminescent Compositions (AREA)
  • Measurement Of Radiation (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a glass scintillator, a preparation method thereof and a thermal neutron detection method. The glass scintillator is composed of the following components by weight: 20-30 parts of SiO2, 30-40 parts of <10>B2O3, 11-14 parts of Na2O, 6-10 parts of Al2O3, 7-11 parts of Ce2O3, 0.2-0.5 part of Sb2O3, and 1-2 parts of carbon powder. The glass scintillator solves the problem of low detection efficiency of glass scintillators to thermal neutrons in the prior art, improves the thermal neutron detection efficiency and luminous efficiency of the glass scintillator, and shortens the light decay time of the glass scintillator.

Description

A kind of glass scintillator and preparation method thereof and thermal neutron detection method
Technical field
The present invention relates to field of light emitting materials, be specifically related to a kind of glass scintillator and preparation method thereof and thermal neutron detection method.
Background technology
Scintillator is a kind of luminescent material that the ionization energy of X ray, gamma-rays or high energy particle can be converted to ultraviolet/visible light, is the conversion body of a kind of energy. Scintillator is of a great variety. Divide from state of matter and have solid scintillator, liquid scintillator and gas scintillator. Organic scintillator, scintillation crystal, glass scintillator etc. can be divided into again for solid scintillator. Glass scintillator is amorphous inorganic nonmetallic materials, it is simple that it has preparation process, chemical stability is good, thermal shock resistance is excellent, and volume and composition all can change in quite on a large scale, easily adapt to the advantages such as various different application requirements, be therefore a kind of excellent scintillator material, can be widely used for the detection of high energy particle.
The research of current glass scintillator is concentrated mainly on Ce3+On the glass of doping, it is primarily due to Ce3+Transmitting belong to 5d-4f transition, die-away time is shorter and between its 5d-4f energy level difference minimum in La system ion, it is appreciated that in the transmission of energy. Have been developed that the Ce of multiple systems at present both at home and abroad3+Doped-glass is for the detection to thermal neutron, but these Ce3+Doped-glass is all not high to the detection efficient of thermal neutron, and present stage does not develop a kind of comparatively ideal thermal neutron detection material yet.
Summary of the invention
It is an object of the invention to provide a kind of glass scintillator and preparation method thereof and thermal neutron detection method, solve in prior art glass scintillator to the inefficient problem of thermal neutron detection, improve thermal neutron detection efficiency and the luminous efficiency of glass scintillator, and shorten the optical attenuation time of glass scintillator.
On the one hand, the invention provides a kind of glass scintillator, be made up of the component of following weight portion:
SiO2: 20-30 part,
10B2O3: 30-40 part,
Na2O:11-14 part,
Al2O3: 6-10 part,
Ce2O3: 7-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part.
As preferably, described glass scintillator, it is made up of the component of following weight portion:
SiO2: 26-30 part,
10B2O3: 34-40 part,
Na2O:11-14 part,
Al2O3: 8-10 part,
Ce2O3: 9-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part.
As preferably, in the component of described glass scintillator, SiO2Corresponding raw material is glass sand,10B2O3Corresponding raw material is H3 10BO3Or/and10B2O3, Na2Raw material corresponding to O is sodium carbonate or/and sodium nitrate, Al2O3Corresponding raw material is alumina powder or/and aluminium hydroxide, Ce2O3Corresponding raw material is six nitric hydrate ceriums or/and Sedemesis., Sb2O3Corresponding raw material is its oxide itself, and the raw material corresponding to carbon dust is high-purity powdered carbon.
On the other hand, the preparation method that the invention provides above-mentioned glass scintillator, comprise the following steps:
(1) weigh corresponding raw material, mix homogeneously according to the component of following weight portion, obtain batch;
SiO2: 20-30 part,
10B2O3: 30-40 part,
Na2O:11-14 part,
Al2O3: 6-10 part,
Ce2O3: 7-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part;
(2) batch is founded, moulding by casting again after discharging, finally make annealing treatment, obtain described glass scintillator.
As preferably, when described batch is founded, batch first being put into enclosed 99 porcelain crucibles, carry out founding for the first time, first time is founded the vitreous humour shrend obtained, obtains a frit; After again a frit being dried, put into and platinum crucible carries out under strongly reducing atmosphere found for the second time, first cooling, discharging again after having founded.
As preferably, when described second time is founded, platinum crucible is placed in glass secondary and founds in device, and described glass secondary is founded device and is placed in Si-Mo rod stove; Described glass secondary is founded device and is nested with by double crucible and forms, outer crucible is clay pot with cover, inner crucible is the corundum crucible with ceramic cap, the interior bottom of described clay pot is equipped with graphite granule, described corundum crucible is placed on the graphite granule in clay pot, the interior bottom of described corundum crucible is equipped with graphite granule, and described platinum crucible is placed on the graphite granule in corundum crucible.
As preferably, the temperature that described first time founds is 1480-1510 DEG C, and the time that first time founds is 1.5-2.5h; The temperature that described second time is founded is 1480-1510 DEG C, and the time that second time is founded is 6-8h.
As preferably, the temperature of the mould that described moulding by casting adopts is 500-550 DEG C.
As preferably, the holding temperature of described annealing is 450-470 DEG C, and the temperature retention time of described annealing is 2-3h, and the rate of temperature fall of described annealing is 8-10 DEG C/h.
It addition, the embodiment of the present invention additionally provides a kind of thermal neutron detection method, described method is for adopting glass scintillator that thermal neutron is detected, and described glass scintillator is above-mentioned glass scintillator.
The glass scintillator that the embodiment of the present invention provides, except can be applicable to thermal neutron detection, also can be widely used to the fields such as neutron time of flight experiment, oil well logging, nondestructive inspection and neutron photography.
Compared with prior art, the beneficial effects of the present invention is:
Substantial amounts of abundance is high and thermal-neutron capture cross-section is higher by introducing in glass scintillator for the embodiment of the present invention10B, improves the thermal neutron detection efficiency of glass scintillator, simultaneously by optimizing glass ingredient design, in ensureing glass scintillator10B2O3High-load time, the Forming ability of glass, high fluorescence intensity and short fluorescence lifetime are taken into account, namely while improving the thermal neutron detection efficiency of glass scintillator, improve the luminous efficiency of glass scintillator and shorten luminescence decay time, thus improving visible detection sensitivity and the visible detection accuracy of glass scintillator.
Accompanying drawing explanation
Fig. 1 is the n-gamma-radiation pulse amplitude spectrogram of the glass scintillator of the embodiment of the present invention 1;
Fig. 2 is the optical attenuation kinetic curve figure of the glass scintillator of the embodiment of the present invention 1;
Fig. 3 is the emission spectrum figure of the glass scintillator of the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as a limitation of the invention.
The glass scintillator that the embodiment of the present invention provides is a kind of Ce3+Boron-10 glass scintillator of doping, this glass scintillator is to neutron detection based on nuclear reaction method, and its principle is, during neutron this glass scintillator of incidence, quilt10B nuclear capture produces following nuclear reaction:
n+10B=α+7Li+2.792MeVⅠ
=α+7Li*+2.31MeVⅡ
7Li+γ+480KeV
The product core of this nuclear reaction constantly excites glass scintillator in motor process, absorbs the activator ion Ce of nuclear reaction energy in glass scintillator3+Produce flicker and launch ultraviolet or visible ray, so the detection of thermal neutron just be can be exchanged into the measurement to visible ray, owing to having multiple effective ways available the measurement of visible ray, so just complicated neutron detection process is converted into simple detection process.This nuclear reaction is high to thermal neutron interface nuclear reaction cross section, up to 3840 bars.
The component of the glass scintillator that the embodiment of the present invention provides and content are as shown in table 1, wherein SiO2Corresponding raw material is glass sand,10B2O3Corresponding raw material is H3 10BO3Or/and10B2O3, Na2Raw material corresponding to O is sodium carbonate or/and sodium nitrate, Al2O3Corresponding raw material is alumina powder or/and aluminium hydroxide, Ce2O3Corresponding raw material is six nitric hydrate ceriums or/and Sedemesis., Sb2O3Corresponding raw material is its oxide itself, and the raw material corresponding to carbon dust is high-purity powdered carbon.
Embodiment 1
Following raw material is weighed: 30g glass sand, 53.3gH by the weight portion content of the glass scintillator component shown in table 13 10BO3, 23.9g sodium carbonate, 10g alumina powder, 35.3g six nitric hydrate cerium, 0.2gSb2O3, the high-purity powdered carbon of 2g; By these raw material mix homogeneously, obtain batch;
Batch is put into enclosed 99 porcelain crucibles, 99 porcelain crucibles are placed in Si-Mo rod stove, carry out founding for the first time, the temperature that first time founds is 1480 DEG C, the time that first time founds is 2.5h, first time is founded the vitreous humour shrend obtained, directly pours into by the vitreous humour taken out from Si-Mo rod stove the water of room temperature so as to quickly cool down, obtain a frit of white;
Frit is placed in baking oven and is dried, and the temperature of drying is 100-200 DEG C; Frit after drying is put in platinum crucible, this platinum crucible is placed in glass secondary and founds in device, and this glass secondary is founded device and is placed in Si-Mo rod stove, carries out second time and founds, the temperature that second time is founded is 1500 DEG C, and the time that second time is founded is 6h; Wherein glass secondary is founded device and is nested with by double crucible and forms, outer crucible is clay pot with cover, inner crucible is the corundum crucible with ceramic cap, the interior bottom of clay pot is equipped with graphite granule, corundum crucible is placed on the graphite granule in clay pot, the interior bottom of corundum crucible is equipped with graphite granule, and platinum crucible is placed on the graphite granule in corundum crucible. After second time founds end, the temperature of vitreous humour is down to 1450 DEG C, discharging again after maintenance 1h.
Vitreous humour after discharging is poured in the heat-resisting cast iron mould of preheating and carry out moulding by casting, the temperature of heat-resisting cast iron mould is 550 DEG C, after vitreous humour solidifies, the glass of formation is quickly put in Muffle furnace and is annealed processing, the temperature of Muffle furnace is 470 DEG C, after glass is incubated 2h in Muffle furnace, closes Muffle furnace, it is cooled to room temperature with the speed of 8 DEG C/h, obtains glass scintillator.
Embodiment 2
Following raw material is weighed: 26g glass sand, 40g by the weight portion content of the glass scintillator component shown in table 110B2O3, 32.9g sodium nitrate, 15.3g aluminium hydroxide, 28.5g Sedemesis., 0.5gSb2O3, the high-purity powdered carbon of 1g; These raw materials are prepared glass scintillator according to the step that same embodiment 1 is identical, the temperature that wherein first time founds is 1510 DEG C, the time that first time founds is 1.5h, the temperature that wherein second time is founded is 1480 DEG C, and the time that second time is founded is 8h, and the temperature of discharging front glass liquid is down to 1400 DEG C, the temperature of heat-resisting cast iron mould is 500 DEG C, during annealing, the temperature of Muffle furnace is 450 DEG C, and glass temperature retention time in Muffle furnace is 3h, and the rate of temperature fall of glass is 10 DEG C/h.
Embodiment 3
Following raw material is weighed: 28g glass sand, 53.3gH by the weight portion content of the glass scintillator component shown in table 13 10BO3, 7g boric anhydride, 22.2g sodium carbonate, 9g alumina powder, 30.3g six nitric hydrate cerium, 15.8g Sedemesis., 0.3gSb2O3, the high-purity powdered carbon of 2g;These raw materials are prepared glass scintillator according to the step that same embodiment 1 is identical, the temperature that wherein first time founds is 1490 DEG C, the time that first time founds is 2h, the temperature that wherein second time is founded is 1510 DEG C, and the time that second time is founded is 7h, and the temperature of discharging front glass liquid is down to 1430 DEG C, the temperature of heat-resisting cast iron mould is 530 DEG C, during annealing, the temperature of Muffle furnace is 460 DEG C, and glass temperature retention time in Muffle furnace is 2.5h, and the rate of temperature fall of glass is 9 DEG C/h.
Embodiment 4
Following raw material is weighed: 20g glass sand, 71gH by the weight portion content of the glass scintillator component shown in table 13 10BO3, 18.8g sodium carbonate, 3g alumina powder, 4.6g aluminium hydroxide, 37.9 6 nitric hydrate ceriums, 0.5gSb2O3, the high-purity powdered carbon of 1.5g; These raw materials are prepared glass scintillator according to the identical step of same embodiment 1 and condition.
Embodiment 5
Following raw material is weighed: 30g glass sand, 60.4gH by the weight portion content of the glass scintillator component shown in table 13 10BO3, 12g sodium carbonate, 19.2g sodium nitrate, 8g alumina powder, 42.9g six nitric hydrate cerium, 0.5gSb2O3, the high-purity powdered carbon of 2g; These raw materials are prepared glass scintillator according to the identical step of same embodiment 1 and condition.
The glass scintillator embodiment of the present invention prepared is cleaved, surface grinding, polishing post-treatment to 40mm × 40mm × 3mm size, carry out the performance test of glass scintillator. Wherein adopting cathode ray fluorescence power characteristics of luminescence tester to measure luminous efficiency, adopt single photon time spectrometer to measure luminescence decay time, adopt thermal neutron detection to measure thermal neutron Absolute detection efficiency, test result is table 1 such as.
The component of table 1. glass scintillator and the performance test results thereof
As can be seen from Table 1, the thermal neutron Absolute detection efficiency of the glass scintillator that the embodiment of the present invention provides reaches 100%, the 14% of luminous efficiency >=NaI (T1) crystal, luminescence decay time≤58ns, illustrate that the thermal neutron Absolute detection efficiency of this glass scintillator does not only reach the highest, and luminous efficiency is high, luminescence decay time is short, namely has high visible detection sensitivity and visible detection accuracy. Fig. 1 is the n-gamma-radiation pulse amplitude spectrogram of the glass scintillator of the embodiment of the present invention 1, and as can be seen from Figure 1 the n-gamma-rays of this glass scintillator screens function admirable; Fig. 2 is the optical attenuation kinetic curve figure of the glass scintillator of the embodiment of the present invention 1, this optical attenuation kinetic curve can obtain luminescence decay time; Fig. 3 is the emission spectrum figure of the glass scintillator of the embodiment of the present invention 1, this emission spectrum can obtain Emission Spectrum Peals and emission spectrum scope.
The embodiment of the present invention is using boron-10 as target nuclear nuclide, Ce3+For activator ion, B-Al-Si is glass matrix, by optimizing glass ingredient design, prepares high performance glass scintillator. It addition, the performance of glass scintillator is also played decisive role by the melting technology of glass. The glass scintillator that the embodiment of the present invention provides need to be founded under strongly reducing atmosphere and obtain, and is due to Ce3+Instability, is very easily oxidized to Ce4+, but in glass scintillator, only have Ce3+Luminescence, Ce4+Not luminous and Ce4+Existence the luminescence of glass scintillator is had strong inhibitory action, fusion cast glass under strongly reducing atmosphere, Ce in component can be prevented3+It is oxidized to Ce4+, by adding high-purity powdered carbon in glass ingredient raw material, glass ingredient can be made to be in strongly reducing atmosphere in melting process.But in glass melting process, it is poisoning that strongly reducing atmosphere is easily caused platinum crucible, and adopt other crucible such as corundum crucible or silica crucible to found, glass easily occurs microbubble and striped, thus affecting the optical homogeneity of glass, the embodiment of the present invention is by glass secondary melting technology and adopts special glass secondary to found device, reduces the strongly reducing atmosphere impact on platinum crucible, ensure that Ce simultaneously3+Stablizing of single valence, efficiently solves microbubble and the stripes problem of glass scintillator, wherein glass secondary melting technology refers to and batch is first put into enclosed 99 porcelain crucibles, carries out founding for the first time, first time is founded the vitreous humour shrend obtained, obtains a frit, after again a frit being dried, put into and platinum crucible carries out under strongly reducing atmosphere found for the second time, wherein platinum crucible is placed in glass secondary and founds in device, glass secondary is founded device and is placed in Si-Mo rod stove, glass secondary is founded device and is nested with by double crucible and forms, outer crucible is clay pot with cover, inner crucible is the corundum crucible with ceramic cap, the interior bottom of clay pot is equipped with graphite granule, corundum crucible is placed on the graphite granule in clay pot, the interior bottom of corundum crucible is equipped with graphite granule, platinum crucible is placed on the graphite granule in corundum crucible, the glass ingredient raw material including high-purity powdered carbon is first put into enclosed 99 porcelain crucibles and is carried out founding for the first time by the embodiment of the present invention, and high-purity powdered carbon is founded for first time and provided strongly reducing atmosphere, it is prevented that Ce in melting process3+It is oxidized to Ce4+, after first time founds end, vitreous humour shrend is obtained frit, it is prevented that Ce in the process of platinum crucible transferred to by vitreous humour3+It is oxidized to Ce4+, simultaneously after first time founds, the carbon dust in vitreous humour is sufficiently mixed with other component of vitreous humour, can weaken the carbon dust corrosion to platinum crucible when second time is founded; When second time is founded, glass secondary is founded device and graphite granule therein and is provided strongly reducing atmosphere for founding for the second time, it is ensured that Ce3+Stablizing of single valence, will not cause corrosion to platinum crucible again, efficiently solves microbubble and the stripes problem of glass scintillator simultaneously.
The glass scintillator that the embodiment of the present invention provides is except can be used for thermal neutron detection, it is also possible to the rays such as detection α, β, γ, the glass scintillator through special handling also has n-γ waveform and screens ability. The glass scintillator that the embodiment of the present invention provides can be widely applied to the fields such as neutron time of flight experiment, oil well logging, nothing flaw detection and neutron photography.
In the component of the glass scintillator that the embodiment of the present invention provides, silicon dioxide is the important formation body of glass, simultaneously the performance such as scalable chemical durability of glass and heat shock resistance. The weight portion content of silicon dioxide controls, when 20-30 part, to can effectively ensure that the stability of glass, be conducive to glass ware forming; When the weight portion content of silicon dioxide is less than 20 parts, thermal stability is very poor, is that glass is easy to fragmentation; When the weight portion content of silicon dioxide is more than 30 parts, causing that glass overall fusion temperature promotes, glass ingredient causes that volatile quantity substantially increases, and is unfavorable for the stability of glass.
The glass scintillator component that the embodiment of the present invention provides contains10B2O3, partly in order to introduce10B, uses it to capture neutron, plays the effect of glass former on the other hand. Due to10The abundance of B reaches 90%, and it is high to thermal-neutron capture cross-section, introduces in glass scintillator10B can greatly improve the detection efficient of neutron,10B content in glass scintillator component is more big, and the thermal neutron detection efficiency of glass scintillator is more high, and substantial amounts of10B2O3Join in glass scintillator component, the Forming ability of glass can be affected.The embodiment of the present invention is by optimizing glass ingredient design, in ensureing glass scintillator10B2O3High-load time, take into account the Forming ability of glass, while improving the neutron detection efficiency of glass scintillator, improve the luminous efficiency of glass scintillator and shorten luminescence decay time, namely improving visible detection sensitivity and the visible detection accuracy of glass scintillator. When10B2O3Weight portion content control when 30-40 part, can meet to thermal neutron capturing requirement and be conducive to glass ware forming, improve luminous efficiency and shorten luminescence decay time. When10B2O3Weight portion content less than 30 parts time, due to10The minimizing of the content of B, can be decreased obviously thermal capture efficiency; When10B2O3Weight portion content more than 40 parts time, cause that glass overall fusion temperature promotes, the volatile quantity of glass ingredient substantially increases, and is unfavorable for the stability of glass, and the luminous efficiency of glass scintillator reduces and luminescence decay time is elongated simultaneously.
Sodium oxide in the glass scintillator component that the embodiment of the present invention provides plays the effect of flux, makes the fusion temperature of glass reduce, and reduces the requirement to glass smelting equipment. Wherein the weight portion content of sodium oxide controls when 11-14 part, and the molding effect making glass is best; When the weight portion content of sodium oxide is less than 11 parts, DeGrain of fluxing, when the weight portion content of sodium oxide is more than 14 parts, the easy crystallize of glass.
Aluminium oxide in the glass scintillator component that the embodiment of the present invention provides is a kind of stabilizer, it is possible to prevent glass devitrification. When the weight portion content of aluminium oxide controls when 6-10 part, stability, glass effect is best; When the weight portion content of aluminium oxide is less than 6 parts, stability, glass is poor, when the weight portion content of aluminium oxide is higher than 10 parts, it is easy to cause glass to have the not fusant matter of residual, thus causing glass devitrification.
Cerium sesquioxide in the glass scintillator component that the embodiment of the present invention provides is to introduce Ce3+, Ce3+Glass scintillator plays the effect of activator, due to Ce3+Instability, is very easily oxidized to Ce4+, Ce is therefore increased in glass as far as possible when not producing cancellation3+, to strengthen luminous intensity. When the weight portion content of cerium sesquioxide controls when 7-11 part, it is ensured that activation effect is best; When the weight portion content of cerium sesquioxide is less than 7 parts, illumination effect is not good, when the weight portion content of cerium sesquioxide is more than 11 parts, it is easy to cause glass devitrification.
Antimony oxide in the glass scintillator component that the embodiment of the present invention provides plays the effect of glass fining agent. When the weight portion content of antimony oxide controls when 0.2-0.5 part, it is ensured that good clarifying effect; When the weight portion content of antimony oxide is less than 0.2 part, clarifying effect is remarkably decreased, and when the weight portion content of antimony oxide is more than 0.5 part, clarifying effect does not promote, especially when the weight portion content of antimony oxide is more than 1 part, it is easy to cause glass devitrification.
Carbon dust in the glass scintillator component that the embodiment of the present invention provides plays the effect of reducing agent, can effectively prevent Ce3+It is oxidized to Ce4+. When the weight portion content of carbon dust controls when 1-2 part, it is ensured that reduction effect is best; When the weight portion content of carbon dust is less than 1 part, reduction effect is poor, it is impossible to ensure Ce3+High-load, when the weight portion content of carbon dust is more than 2 parts, can cause that glass colour tends to Lycoperdon polymorphum Vitt, have a strong impact on the transmitance of glass.
What finally illustrate is, above example is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from objective and the scope of technical solution of the present invention, it all should be encompassed in the middle of scope of the presently claimed invention.

Claims (10)

1. a glass scintillator, it is characterised in that be made up of the component of following weight portion:
SiO2: 20-30 part,
10B2O3: 30-40 part,
Na2O:11-14 part,
Al2O3: 6-10 part,
Ce2O3: 7-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part.
2. glass scintillator according to claim 1, it is characterised in that be made up of the component of following weight portion:
SiO2: 26-30 part,
10B2O3: 34-40 part,
Na2O:11-14 part,
Al2O3: 8-10 part,
Ce2O3: 9-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part.
3. glass scintillator according to claim 1 and 2, it is characterised in that in the component of described glass scintillator, SiO2Corresponding raw material is glass sand,10B2O3Corresponding raw material is H3 10BO3Or/and10B2O3, Na2Raw material corresponding to O is sodium carbonate or/and sodium nitrate, Al2O3Corresponding raw material is alumina powder or/and aluminium hydroxide, Ce2O3Corresponding raw material is six nitric hydrate ceriums or/and Sedemesis., Sb2O3Corresponding raw material is its oxide itself, and the raw material corresponding to carbon dust is high-purity powdered carbon.
4. the preparation method of the glass scintillator described in claim 1, it is characterised in that comprise the following steps:
(1) weigh corresponding raw material, mix homogeneously according to the component of following weight portion, obtain batch;
SiO2: 20-30 part,
10B2O3: 30-40 part,
Na2O:11-14 part,
Al2O3: 6-10 part,
Ce2O3: 7-11 part,
Sb2O3: 0.2-0.5 part,
Carbon dust: 1-2 part;
(2) batch is founded, moulding by casting again after discharging, finally make annealing treatment, obtain described glass scintillator.
5. the preparation method of glass scintillator according to claim 4, it is characterised in that when described batch is founded, batch is first put into enclosed 99 porcelain crucibles, carry out founding for the first time, first time is founded the vitreous humour shrend obtained, obtains a frit; After again a frit being dried, put into and platinum crucible carries out under strongly reducing atmosphere found for the second time, first cooling, discharging again after having founded.
6. the preparation method of glass scintillator according to claim 5, it is characterised in that when described second time is founded, platinum crucible is placed in glass secondary and founds in device, and described glass secondary is founded device and is placed in Si-Mo rod stove; Described glass secondary is founded device and is nested with by double crucible and forms, outer crucible is clay pot with cover, inner crucible is the corundum crucible with ceramic cap, the interior bottom of described clay pot is equipped with graphite granule, described corundum crucible is placed on the graphite granule in clay pot, the interior bottom of described corundum crucible is equipped with graphite granule, and described platinum crucible is placed on the graphite granule in corundum crucible.
7. the preparation method of glass scintillator according to claim 5, it is characterised in that the temperature that described first time founds is 1480-1510 DEG C, the time that first time founds is 1.5-2.5h; The temperature that described second time is founded is 1480-1510 DEG C, and the time that second time is founded is 6-8h.
8. the preparation method of glass scintillator according to claim 4, it is characterised in that the temperature of the mould that described moulding by casting adopts is 500-550 DEG C.
9. the preparation method of glass scintillator according to claim 4, it is characterised in that the holding temperature of described annealing is 450-470 DEG C, the temperature retention time of described annealing is 2-3h, and the rate of temperature fall of described annealing is 8-10 DEG C/h.
10. a thermal neutron detection method, thermal neutron is detected by described method for adopting glass scintillator, it is characterised in that described glass scintillator is the glass scintillator described in any one of claim 1-9.
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CN108249757A (en) * 2018-02-11 2018-07-06 井冈山大学 A kind of water white transparency cerium activation borosilicate scintillation glass and preparation method thereof
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CN114133137B (en) * 2021-12-15 2023-10-20 中国建筑材料科学研究总院有限公司 Neutron detection glass scintillator and preparation method and application thereof

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