CN101602571A - A kind of scintillation glass and preparation method thereof - Google Patents
A kind of scintillation glass and preparation method thereof Download PDFInfo
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- CN101602571A CN101602571A CNA2009100548161A CN200910054816A CN101602571A CN 101602571 A CN101602571 A CN 101602571A CN A2009100548161 A CNA2009100548161 A CN A2009100548161A CN 200910054816 A CN200910054816 A CN 200910054816A CN 101602571 A CN101602571 A CN 101602571A
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Abstract
A kind of scintillation glass and preparation method thereof the present invention relates to SnO
2Be scintillation glass of luminescence center and preparation method thereof.Scintillation crystal has obtained broad research, but its preparation cost height, difficulty of preparation technology is big.In this case, the research of scintillation glass has obtained attention, and this is that preparation technology is also simpler because the preparation cost of glass is more much lower than crystal.What at present, research was more is doped Ce
3+Scintillation glass for luminescence center.But, because Ce
3+The concentration quenching effect is big, and luminous intensity is restricted, and it causes the ABSORPTION EDGE red shift to the matrix sensitivity simultaneously, influences UV, visible light perviousness etc.And with SnO
2For the scintillation glass of luminescence center can remedy above-mentioned shortcoming.SnO
2Belong to the network intermediate, can introduce by higher concentration, have higher luminous intensity, simultaneously, the UV, visible light through performance of glass is good.The introducing of stannic oxide can keep even further improve original glass forming ability and other physical and chemical performances.
Description
Technical field
The present invention relates to scintillator material and preparation thereof, especially relate to SnO
2Be scintillation glass of luminescence center and preparation method thereof.
Background technology
In the last few years, along with continuous progress in science and technology, the further expansion in mankind's activity field, at high energy physics, nuclear physics, the fast development of aspects such as industry detection has proposed new requirement to the performance of scintillation material, especially requires scintillation material to have high resolving power and high radiation hardness ability.For now, most traditional scintillation material (as NaI:Tl, CsI:Tl, BGO etc.) is not well positioned to meet existing demand.Since the nineties in last century, the research that both at home and abroad developing and preparation is applied to the novel fast blink material in field such as high energy physics has had many reports.Except scintillation crystal, the research and development of scintillation glass are also quite noticeable, and this mainly is because the preparation cost of glass is more much lower than crystal, for the needed atmospheric shimmer body of calorimeter of new generation that the preparation volume reaches tens cubic metres, the saving of cost is considerable.In the scintillation glass of having reported at present, studying more is that rear-earth-doped ion is the scintillation glass of luminescence center.But, Ce
3+The doping scintillation glass has following limitation: the concentration quenching effect is comparatively remarkable, makes its introducing amount be subjected to bigger restriction, thereby influences its luminous intensity; Some rare earth ion easily makes the ultraviolet of glass and visible absorbance cutoff wavelength produce red shift to the light basicity sensitivity of host glass, thereby influences the ultraviolet and visible perviousness of glass; Some rare earth ion doped glass smelting process must adopt reducing atmosphere, can not adopt platinum crucible, can only be with quartz crucible or ceramic crucible, and problems such as bubble and bubble are difficult to solve, thereby influence the optical homogeneity of glass.
With stannic oxide (SnO
2) can remedy Ce for the scintillation glass of luminescence center
3+The above-mentioned shortcoming of ion doping scintillation glass.Stannic oxide (SnO
2) belong to the network intermediate, can in glass is formed, introduce, thereby can make scintillation glass have higher luminous intensity with higher concentration, and, stannic oxide (SnO
2) introducing can keep even further improve original glass forming ability and other physical and chemical performances.In addition, owing to the tin ion as luminescence center is the high price form, so can adopt platinum crucible to found in air, preparation technology is simple, and the material homogeneity that obtains is good, the purity height.
Summary of the invention
One of purpose of the present invention, provide a kind of can application and the scintillation glass in fields such as high energy physics, nuclear physics, nuclear medicine, earth physics, industry detection, replace present widely used scintillation crystal with part, the latter has the cost of manufacture height, in enormous quantities and large size generates the big shortcoming of difficulty, makes it be subjected to bigger restriction in the application of reality.
Two of the object of the invention provides a kind of method for preparing above-mentioned scintillation glass.
Inventive concept:
Silicon-dioxide (SiO
2), germanium dioxide (GeO
2), boron trioxide (B
2O
3), Vanadium Pentoxide in FLAKES (P
2O
5) be traditional glass-former, it is wide to have glass formation regional extent, the oxide compound kind that can introduce is many, density is easy to regulate, advantages such as ultraviolet and visible through performance and other physical and chemical performances are good, and can pass through general forming technique, as mold pressing, hot pressing and extrusion technique, the preparation process of scintillator is simplified, and cost significantly reduces.With stannic oxide (SnO
2) for the oxide glass of luminescence center has near ultraviolet and visible through performance is good, decay is very fast, characteristics such as fluorescence intensity height.Compare stannic oxide (SnO with rare earth luminescence
2) luminously have UV, visible light to see through the zone wideer, fluorescence intensity is strong, and the cheaper advantage of cost, especially is useful for the detection of split-second precision.
The present invention is a kind of with stannic oxide (SnO
2) be the phosphoric acid salt scintillation glass of luminescence center, the composition design of this system glass has taken into account following factor: glass forming ability, the high optical transmission of near ultraviolet and visibility region, higher density, radiation resistance preferably, high fluorescent and short fluorescence lifetime.
Technical scheme:
Scintillation glass of the present invention comprises following component and content (content calculates with molar percentage mol%):
Glass-former oxide compound (SiO
2, GeO
2, B
2O
3, P
2O
5): 10-70
RO：10-50
SnO
2：1-10
R=Ca wherein, Sr, Ba
The method for preparing above-mentioned fast blink glass comprises the steps:
A) preparation of glass batch
Raw material is made glass batch according to above-mentioned component and content behind thorough mixing.Wherein glass-former oxide compound and RO introduce with corresponding oxide compound or other compound forms respectively.
B) founding of admixtion:
To place container to melt by the glass batch that step (a) makes, temperature of fusion be 1200-1500 ℃, and fusing time is 1-4 hour.Pour the glass metal of fusing in mould curing molding, the glass behind the curing molding is moved in the retort furnace, be incubated half an hour, obtain glass specimen after the cooling at 450-600 ℃.
Wherein: mould therefor preferably is heated to about 450 ℃ in advance, and retort furnace is warming up to about 450 ℃ in advance.
C) thermal treatment:
To make glass specimen by step (b) and be reentered into retort furnace, be 350-600 ℃ in temperature, is incubated 3-10 hour, promptly obtains scintillation glass of the present invention after the cooling.
Scintillation glass of the present invention is compared with rear-earth-doped scintillation glass, and it is good then to have a ultraviolet through performance, characteristics such as fluorescence intensity height; Simultaneously, scintillation glass of the present invention has again that the process of founding is simple, and glass forming ability is strong, and density is easy to adjust, and the luminescence center ion is introduced the high characteristics of concentration.Scintillation glass of the present invention can be applied to fields such as high energy physics, nuclear physics, nuclear medicine, earth physics, industry detection.
Embodiment
Content for a better understanding of the present invention, the invention will be further described below by implementing, but illustrated embodiment does not limit protection scope of the present invention.
Embodiment 1
Formulating of recipe:
Adopt phosphate system.Design of components is as follows:
The glass of table 1 embodiment 1 is formed (mol%)
| P 2O 5 | SrO | SnO 2 |
| 75 | 25 | 2 |
The admixtion preparation:
Adopt high purity (99.9%) primary ammonium phosphate (NH respectively
4H
2PO
4), Strontium carbonate powder (SrCO
3) and stannic oxide for introducing P
2O
5, SrO and SnO
2Raw material, carry out the preparation of formula calculation and admixtion by the composition shown in the table 1.The admixtion compound method is identical with conventional glass batch compound method.Admixtion needs thorough mixing.
Glass smelting:
The admixtion that mixes is put into platinum crucible, fusion cast glass in electric furnace.Founding atmosphere is air, and temperature of fusion is 1250 ℃, and fusing time is 2 hours, glass is carried out hand mixing 2 times between soak, with fusing and the clear quality of improving glass metal.
Pour natural moulding in the mould of heat-resistance stainless steel into melting good glass metal.Stainless steel mould is heated to 450 ℃ in advance, and the glass specimen after solidifying is moved in the retort furnace.Retort furnace is warming up to 450 ℃ in advance.Insulation half hour time is closed electric furnace in retort furnace, and glass specimen cools to room temperature with the furnace.
Thermal treatment:
Cooled glass specimen is reentered into retort furnace, and Heating temperature is 450 ℃, and soaking time is 6 hours.Insulation after finishing is closed retort furnace, and glass specimen cools to room temperature with the furnace.
Experimental result:
Resulting glass specimen is done the mensuration of fluorescence property test and density after cutting, surface grinding, polished finish.
Test result sees Table 2.
The fluorescence property of table 2 embodiment 1 glass and density experiment result
| Density (g/cm 3) | Excitation wavelength (nm) | Emission wavelength (nm) | Optical attenuation (μ s) |
| 3.80 | 267 | 420 | 10 |
Embodiment 2-4
In each of the embodiments described below, the preparation method of glass is with embodiment 1, and the different glass composition that is adopted, density and fluorescence property test result are listed in table 3 and table 4. respectively
The glass of table 3 embodiment 2-4 is formed (mol%)
| Sequence number | P 2O 5 | SrO | BaO | CaO | SnO 2 |
| 2 | 75 | 25 | 5 | ||
| 3 | 60 | 40 | 2 | ||
| 4 | 75 | 25 | 2 |
The fluorescence property and the density measurement result of table 4 embodiment 2-4 glass
Embodiment 5
In the following embodiments, the preparation method of glass is with embodiment 1, and the different glass composition that is adopted, density and fluorescence property test result are listed in table 5 and table 6. respectively
Formulating of recipe:
Adopt the germanate system.Design of components is as follows:
The glass of table 5 embodiment 5 is formed (mol%)
| GeO 2 | SrO | SnO 2 |
| 70 | 30 | 5 |
The admixtion preparation:
Adopt high purity (99.9%) germanium oxide (GeO respectively
2), Strontium carbonate powder (SrCO
3) and stannic oxide (SnO
2) for introducing P
2O
5, SrO and SnO
2Raw material, carry out the preparation of formula calculation and admixtion by the composition shown in the table 1.The admixtion compound method is identical with conventional glass batch compound method.Admixtion needs thorough mixing.
The fluorescence property of table 6 embodiment 6 glass and density measurement result
| Density (g/cm 3) | Excitation wavelength (nm) | Emission wavelength (nm) | Optical attenuation (μ s) |
| 5.35 | 267 | 420 | 12 |
Claims (3)
1. a scintillation glass is characterized in that, described glass comprises following component and content (content calculates with molar percentage):
Glass-former oxide compound (SiO
2, GeO
2, B
2O
3, P
2O
5): 10-70
RO：10-50
SnO
2：1-10
R=Ca wherein, Sr, Ba
2. prepare the method for the described glass of claim 1, it is characterized in that, described preparation method comprises the steps:
A) preparation of glass batch
Raw material is made glass batch according to described composition of claim 1 and content behind thorough mixing;
B) admixtion founds
To place container to melt by the glass batch that step (a) makes, temperature of fusion be 1200-1500 ℃, and fusing time is 1-4 hour.Pour the glass metal of fusing in mould curing molding, the glass after the moulding is moved on in the retort furnace, about 450 ℃-600 ℃, be incubated half hour, obtain glass specimen after the cooling.
C) thermal treatment
To be reentered into retort furnace by the glass specimen that step (b) makes, be 350-600 ℃ in temperature, is incubated 3-10 hour, obtains scintillation glass of the present invention after the cooling.
3. preparation method as claimed in claim 2 is characterized in that, wherein mould therefor is preheated to about 450 ℃ in the step (b), and retort furnace is warming up to about 450 ℃ in advance.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100548161A CN101602571A (en) | 2009-07-15 | 2009-07-15 | A kind of scintillation glass and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100548161A CN101602571A (en) | 2009-07-15 | 2009-07-15 | A kind of scintillation glass and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857363A (en) * | 2010-06-18 | 2010-10-13 | 华东理工大学 | White light glass and preparation method thereof |
| CN102584014A (en) * | 2010-08-03 | 2012-07-18 | 宁波大学 | Rare earth doped oxyfluoride tellurite scintillation glass and preparation method thereof |
| CN102826753A (en) * | 2012-09-28 | 2012-12-19 | 井冈山大学 | Gd2O3-rich borogermanate scintillation glass, and preparation method and application thereof |
| CN103951221A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped CaI2 microcrystalline glass and preparation method thereof |
| CN103951220A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped BaBr2 microcrystalline glass and preparation method thereof |
| CN104944771A (en) * | 2015-04-22 | 2015-09-30 | 华东理工大学 | Deep-ultraviolet excited manganese ion-doped luminescent glass |
| CN109574505A (en) * | 2018-12-29 | 2019-04-05 | 上海应用技术大学 | A kind of production method of green fluorescence glass ceramics |
-
2009
- 2009-07-15 CN CNA2009100548161A patent/CN101602571A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857363A (en) * | 2010-06-18 | 2010-10-13 | 华东理工大学 | White light glass and preparation method thereof |
| CN102584014A (en) * | 2010-08-03 | 2012-07-18 | 宁波大学 | Rare earth doped oxyfluoride tellurite scintillation glass and preparation method thereof |
| CN102584014B (en) * | 2010-08-03 | 2014-04-16 | 宁波大学 | Rare earth doped oxyfluoride tellurite scintillation glass and preparation method thereof |
| CN102826753A (en) * | 2012-09-28 | 2012-12-19 | 井冈山大学 | Gd2O3-rich borogermanate scintillation glass, and preparation method and application thereof |
| CN102826753B (en) * | 2012-09-28 | 2015-10-14 | 井冈山大学 | Be rich in Gd 2o 3borogermanates scintillation glass and preparation method thereof and application |
| CN103951221A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped CaI2 microcrystalline glass and preparation method thereof |
| CN103951220A (en) * | 2014-05-08 | 2014-07-30 | 宁波大学 | Rare-earth-ion-doped BaBr2 microcrystalline glass and preparation method thereof |
| CN103951221B (en) * | 2014-05-08 | 2016-02-03 | 宁波大学 | Rare earth ion doped CaI 2devitrified glass and preparation method thereof |
| CN103951220B (en) * | 2014-05-08 | 2016-05-25 | 宁波大学 | Rare earth ion doped BaBr2Devitrified glass and preparation method thereof |
| CN104944771A (en) * | 2015-04-22 | 2015-09-30 | 华东理工大学 | Deep-ultraviolet excited manganese ion-doped luminescent glass |
| CN109574505A (en) * | 2018-12-29 | 2019-04-05 | 上海应用技术大学 | A kind of production method of green fluorescence glass ceramics |
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Open date: 20091216 |