CN103951222B - Rare earth ion doped SrBr 2devitrified glass and preparation method thereof - Google Patents
Rare earth ion doped SrBr 2devitrified glass and preparation method thereof Download PDFInfo
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- CN103951222B CN103951222B CN201410198132.XA CN201410198132A CN103951222B CN 103951222 B CN103951222 B CN 103951222B CN 201410198132 A CN201410198132 A CN 201410198132A CN 103951222 B CN103951222 B CN 103951222B
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Abstract
The invention discloses a kind of rare earth ion doped SrBr
2devitrified glass and preparation method thereof, its Mole percent consists of P
2o
5: 30-40mol%, B
2o
3: 25-30mol%, BaF
2: 7-15mol%, SrO:5-9mol%, SrBr
2: 15-20mol%, rare earth bromide: 1-4mol%, wherein rare earth bromide is EuBr
2, CeBr
3, TbBr
3in one, its preparation method first prepares P with scorification
2o
5-B
2o
3-BaF
2-SrO-SrBr
2-LnBr
2, P
2o
5-B
2o
3-BaF
2-SrO-SrBr
2-LnBr
3be glass, after heat treatment obtain transparent SrBr
2devitrified glass, SrBr of the present invention
2devitrified glass, energy Deliquescence-resistant, good mechanical property, short wavelength's royal purple light transmission rate are higher, have extremely strong twinkling light luminescence and export, the performances such as energy resolution is good.The preparation method of this devitrified glass is simple, and production cost is lower.
Description
Technical field
The present invention relates to a kind of rare earth ion doped devitrified glass, especially relate to a kind of rare earth ion doped SrBr being used as scintillation material
2devitrified glass and preparation method thereof.
Background technology
Scintillation material is a kind of lower optical function material that can send visible ray of exciting at energetic ray (as x-ray, gamma-rays) or other radioactive particle, is widely used in the fields such as the researchs of nuclear medicine diagnostic, high energy physics and nuclear physics experiment, industrial and geological prospecting.The requirement of difference to scintillator according to Application Areas is also not quite similar, but generally scintillation material should possess following properties: the features such as luminous efficiency is high, fluorescence decay is fast, density is comparatively large, cost is low and radiation resistance is good.Scintillation crystal generally has the advantage such as resistance to irradiation, fast decay, High Light Output, but scintillation crystal also exists following serious shortcoming: preparation difficulty, expensive.And although rare earth ion doped scintillation glass is with short production cycle, cost is low, be easy to batch production, can realize large size in preparation technology, it is difficult compared with crystal in light output, multiplicity etc., and therefore its application is also very limited.
SrBr
2crystal be a kind of can the scintillation crystal matrix of doping with rare-earth ions, Eu
2+the SrBr of doping
2crystal has abnormal high light output, and good energy resolution, can be applicable in low energy physics and the field such as safety check, medical imaging.Ce
3+the SrBr of doping
2crystal has High Light Output, the feature of fast decay, Tb
3+doping SrBr
2crystal can be used for scintillation fluor screen.But SrBr
2crystal is deliquescence, poor, the easy cleavage slabbing of mechanical property, its practical application of the large-size crystals growth disadvantages affect such as difficult, expensive very easily.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Deliquescence-resistant, good mechanical property, has stronger light output, fast decay, energy resolution and the good rare earth ion doped SrBr of temporal resolution
2devitrified glass and preparation method thereof.
The present invention solves the problems of the technologies described above adopted technical scheme: rare earth ion doped SrBr
2devitrified glass, its Mole percent consists of:
P
2O
5：30-40mol％B
2O
3：25-30mol％BaF
2：7-15mol％
SrO:5-9mol%SrBr
2: 15-20mol% rare earth bromide: 1-4mol%
Wherein rare earth bromide is EuBr
2, CeBr
3, TbBr
3in one.
This flicker devitrified glass material component is: P
2o
5: 35mol%, B
2o
3: 28mol%, BaF
2: 7mol%, SrO:6mol%, SrBr
2: 20mol%, EuBr
2: 4mol%.
This flicker devitrified glass material component is: P
2o
5: 30mol%, B
2o
3: 30mol%, BaF
2: 15mol%, SrO:5mol%, SrBr
2: 19mol%, CeBr
3: 1mol%.
This flicker devitrified glass material component is: P
2o
5: 40mol%, B
2o
3: 25mol%, BaF
2: 9mol%, SrO:9mol%, SrBr
2: 15mol%, TbBr
3: 2mol%.
Described rare earth ion doped SrBr
2the preparation method of devitrified glass, comprises the steps:
(1) P
2o
5-B
2o
3-BaF
2-SrO-SrBr
2-LnBr
2, P
2o
5-B
2o
3-NaF-SrO-SrBr
2-LnBr
3be founding of glass:
Analytically pure each raw material is taken by material component, raw material is mixed, then pours in quartz crucible or corundum crucible and melt, temperature of fusion 1360-1460 DEG C, insulation 1-2 hour, glass melt is poured in pig mold, be then placed in retort furnace and anneal, in glass transformation temperature Tg temperature after 2 hours, 50 DEG C are cooled to the speed of 10 DEG C/h, close retort furnace power supply and be automatically cooled to room temperature, take out glass, for micritization thermal treatment.
(2) SrBr
2prepared by devitrified glass:
According to thermal analyses (DTA) experimental data of glass, obtained glass is placed in nitrogen fine annealing stove heat-treated 4 ~ 6 hours near its first crystallization peak, and then be cooled to 50 DEG C with the speed of 5 DEG C/h, close fine annealing stove power supply, automatically be cooled to room temperature, obtain transparent rare earth ion doped SrBr
2devitrified glass.
Compared with prior art, the invention has the advantages that: this devitrified glass is made up of fluorine bromine oxygen compound, the through performance of short wavelength is good, has SrBr
2the feature that the superior scintillation properties of crystalline host material and the physical strength of oxide glass, stability and being easy to is processed, overcomes SrBr
2single crystal is the shortcoming such as deliquescence, poor, the easy cleavage slabbing of mechanical property very easily; The experiment proved that: by formula of the present invention and preparation method, separate out rare earth ion doped to SrBr
2crystalline phase, obtained rare earth ion doped SrBr
2devitrified glass is transparent, and energy Deliquescence-resistant, good mechanical property, short wavelength's royal purple light transmission rate are higher, and have extremely strong light output, decay soon, the performances such as good energy resolution and temporal resolution, can make scintillation detectors efficiency greatly improve.The preparation method of this devitrified glass is simple, and production cost is lower.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of sample after the thermal treatment of embodiment one micritization.
Fig. 2 is the Eu:SrBr of embodiment two excitation of X-rays
2the fluorescence spectrum of devitrified glass.
Fig. 3 is the Ce:SrBr of embodiment one excitation of X-rays
2the fluorescence spectrum of devitrified glass.
Fig. 4 is the Tb:SrBr of embodiment three excitation of X-rays
2the fluorescence spectrum of devitrified glass.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one: table 1 is glass formula and the first recrystallization temperature value of embodiment one.
Table 1
Concrete preparation process is as follows: the first step, weighs 50 grams of analytical pure raw materials by the formula in table 1, adds 2.5 grams of NH
4hF
2, 2.5 grams of NH
4hBr
2pour in corundum crucible after raw material is mixed and melt, temperature of fusion 1460 DEG C, be incubated 1 hour, glass melt poured in pig mold, be then placed in retort furnace and anneal, in glass transformation temperature Tg temperature after 2 hours, be cooled to 50 DEG C with the speed of 10 DEG C/h, close retort furnace power supply and be automatically cooled to room temperature, take out glass; Second step, according to thermal analyses (DTA) experimental data of glass, obtain the first recrystallization temperature 715 DEG C, obtained glass is placed in nitrogen fine annealing stove 735 DEG C of thermal treatments 4 hours, and then be cooled to 50 DEG C with the speed of 5 DEG C/h, close fine annealing stove power supply and be automatically cooled to room temperature, obtain transparent Eu
2+the SrBr of ion doping
2devitrified glass.
To the SrBr of preparation
2devitrified glass carries out X-ray diffraction test, and obtain the XRD figure of glass after micritization process as shown in Figure 1, its result is as follows: the XRD diffraction peak of the sample obtained through Overheating Treatment and SrBr
2the main diffraction peak of the standard x RD figure of crystalline phase all conforms to, and the material therefore obtained is SrBr
2the devitrified glass of crystallization phase.The Eu of excitation of X-rays
2+ion doping SrBr
2as shown in Figure 2, fluorescence peak intensity is very large for the fluorescence spectrum of devitrified glass.Mix Eu
2+ion SrBr
2devitrified glass light output can reach 94000ph/MeV.
Embodiment two: table 2 is glass formula and the first recrystallization temperature value of embodiment two.
Table 2
Concrete preparation process is as follows: the first step, weighs 50 grams of analytical pure raw materials by the formula in table 2, adds 2.5 grams of NH
4hF
2, 2.5 grams of NH
4hBr
2pour in quartz crucible after raw material is mixed and melt, temperature of fusion 1360 DEG C, be incubated 2 hours, glass melt poured in pig mold, be then placed in retort furnace and anneal, in glass transformation temperature Tg temperature after 2 hours, be cooled to 50 DEG C with the speed of 10 DEG C/h, close retort furnace power supply and be automatically cooled to room temperature, take out glass; Second step, according to thermal analyses (DTA) experimental data of glass, obtain the first recrystallization temperature 705 DEG C, obtained glass is placed in nitrogen fine annealing stove 725 DEG C of thermal treatments 6 hours, and then be cooled to 50 DEG C with the speed of 5 DEG C/h, close fine annealing stove power supply and be automatically cooled to room temperature, obtain transparent Ce
3+the SrBr of doping
2devitrified glass.
To the SrBr of preparation
2the spectral quality test of devitrified glass, the Ce of excitation of X-rays
3+ion doping SrBr
2as shown in Figure 3, its result shows to produce Ce:SrBr after Overheating Treatment the fluorescence spectrum of devitrified glass
2crystallite luminous intensity compared with corresponding glass basis is significantly improved, and Ce:SrBr is described
2the luminosity of crystallite is better.
Embodiment three: table 3 is glass formula and the first recrystallization temperature value of embodiment three.
Table 3
Concrete preparation process is as follows: the first step, weighs 50 grams of analytical pure raw materials by the formula in table 3, adds 2.5 grams of NH
4hF
2, 2.5 grams of NH
4hBr
2pour in quartz crucible after raw material is mixed and melt, temperature of fusion 1410 DEG C, be incubated 1.5 hours, glass melt poured in pig mold, be then placed in retort furnace and anneal, in glass transformation temperature Tg temperature after 2 hours, be cooled to 50 DEG C with the speed of 10 DEG C/h, close retort furnace power supply and be automatically cooled to room temperature, take out glass.Second step, according to thermal analyses (DTA) experimental data of glass, obtain the first recrystallization temperature 723 DEG C, obtained glass is placed in nitrogen fine annealing stove 756 DEG C of thermal treatments 5 hours, and then be cooled to 50 DEG C with the speed of 5 DEG C/h, close fine annealing stove power supply and be automatically cooled to room temperature, obtain transparent Tb
3+the SrBr of ion doping
2devitrified glass.
To the SrBr of preparation
2the spectral quality test of devitrified glass, the Tb of excitation of X-rays
3+ion doping SrBr
2as shown in Figure 4, its result shows that after Overheating Treatment, produce Tb:SrBr2 crystallite luminous intensity compared with corresponding glass basis is significantly improved, and illustrates Tb:SrBr to the fluorescence spectrum of devitrified glass
2the luminosity of crystallite is better; The rare earth ion doped SrBr obtained by above-mentioned preparation process
2devitrified glass is transparent and physical and chemical performance is excellent.
Claims (5)
1. a rare earth ion doped SrBr
2devitrified glass, its Mole percent consists of:
P
2O
5：30-40mol％B
2O
3：25-30mol％BaF
2：7-15mol％
SrO:5-9mol%SrBr
2: 15-20mol% rare earth bromide: 1-4mol%
Wherein rare earth bromide is EuBr
2, CeBr
3, TbBr
3in one.
2. rare earth ion doped SrBr according to claim 1
2devitrified glass, is characterized in that this devitrified glass material component is: P
2o
5: 35mol%, B
2o
3: 28mol%, BaF
2: 7mol%, SrO:6mol%, SrBr
2: 20mol%, EuBr
2: 4mol%.
3. rare earth ion doped SrBr according to claim 1
2devitrified glass, is characterized in that this devitrified glass material component is: P
2o
5: 30mol%, B
2o
3: 30mol%, BaF
2: 15mol%, SrO:5mol%, SrBr
2: 19mol%, CeBr
3: 1mol%.
4. rare earth ion doped SrBr according to claim 1
2devitrified glass, is characterized in that this devitrified glass material component is: P
2o
5: 40mol%, B
2o
3: 25mol%, BaF
2: 9mol%, SrO:9mol%, SrBr
2: 15mol%, TbBr
3: 2mol%.
5. rare earth ion doped SrBr according to claim 1
2the preparation method of devitrified glass, is characterized in that comprising following concrete steps:
(1) P
2o
5-B
2o
3-BaF
2-SrO-SrBr
2-LnBr
2, P
2o
5-B
2o
3-BaF
2-SrO-SrBr
2-LnBr
3be founding of glass, wherein LnBr
2for EuBr
2, LnBr
3for CeBr
3or TbBr
3: take analytically pure each raw material by material component, raw material is mixed, then pours in quartz crucible or corundum crucible and melt, temperature of fusion 1360-1460 DEG C, insulation 1-2 hour, glass melt is poured in pig mold, then glass is placed in retort furnace and anneals, in glass transformation temperature Tg temperature after 2 hours, 50 DEG C are cooled to the speed of 10 DEG C/h, close retort furnace power supply and be automatically cooled to room temperature, take out glass, for micritization thermal treatment;
(2) SrBr
2the preparation of devitrified glass: according to thermal analyses (DTA) experimental data of glass, obtained glass is placed in nitrogen fine annealing stove heat-treated 4 ~ 6 hours near its first crystallization peak, and then be cooled to 50 DEG C with the speed of 5 DEG C/h, close fine annealing stove power supply, automatically be cooled to room temperature, obtain transparent rare earth ion doped SrBr
2devitrified glass.
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|---|---|---|---|
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|---|---|---|---|
| CN201410198132.XA CN103951222B (en) | 2014-05-08 | 2014-05-08 | Rare earth ion doped SrBr 2devitrified glass and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
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| CN103951222B true CN103951222B (en) | 2016-04-06 |
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| CN105461230A (en) * | 2015-11-16 | 2016-04-06 | 宁波大学 | Glass film containing divalent europium ion doped strontium bromide microcrystals and preparation method thereof |
| CN105384344A (en) * | 2015-11-16 | 2016-03-09 | 宁波大学 | Preparation method of glass film containing rare-earth ion doped barium bromide microcrystals |
| CN108840571B (en) * | 2018-07-03 | 2020-12-29 | 中国科学院福建物质结构研究所 | Double-crystal-phase glass ceramic for fluorescent temperature probe and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786792A (en) * | 2008-09-04 | 2010-07-28 | Hoya株式会社 | Fluorophosphate glass, and manufacture method thereof and use thereof |
| CN102557458A (en) * | 2012-01-11 | 2012-07-11 | 宁波大学 | Microcrystalline glass containing rare earth mixing yttrium aluminum garnet (YAG) phase and preparation method thereof |
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| US20090190214A1 (en) * | 2008-01-29 | 2009-07-30 | Nicholas Francis Borrelli | Polarizing photorefractive glass |
| JP4611438B2 (en) * | 2008-11-27 | 2011-01-12 | 日本山村硝子株式会社 | High extinction ratio polarizing glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786792A (en) * | 2008-09-04 | 2010-07-28 | Hoya株式会社 | Fluorophosphate glass, and manufacture method thereof and use thereof |
| CN102557458A (en) * | 2012-01-11 | 2012-07-11 | 宁波大学 | Microcrystalline glass containing rare earth mixing yttrium aluminum garnet (YAG) phase and preparation method thereof |
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