CN100336754C - Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method - Google Patents
Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method Download PDFInfo
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- CN100336754C CN100336754C CNB2004100665459A CN200410066545A CN100336754C CN 100336754 C CN100336754 C CN 100336754C CN B2004100665459 A CNB2004100665459 A CN B2004100665459A CN 200410066545 A CN200410066545 A CN 200410066545A CN 100336754 C CN100336754 C CN 100336754C
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- tin
- fluorine
- phosphate
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- 239000011521 glass Substances 0.000 title claims abstract description 39
- 229910019142 PO4 Inorganic materials 0.000 title claims description 10
- 239000010452 phosphate Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- SQAKQVFOMMLRPR-IWGRKNQJSA-N 2-[(e)-2-[4-[4-[(e)-2-(2-sulfophenyl)ethenyl]phenyl]phenyl]ethenyl]benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1\C=C\C1=CC=C(C=2C=CC(\C=C\C=3C(=CC=CC=3)S(O)(=O)=O)=CC=2)C=C1 SQAKQVFOMMLRPR-IWGRKNQJSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910008449 SnF 2 Inorganic materials 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 239000000155 melt Substances 0.000 claims abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 9
- 235000021286 stilbenes Nutrition 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 150000001629 stilbenes Chemical class 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 235000019504 cigarettes Nutrition 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 2
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 229920003222 semicrystalline poly(phosphazene) Polymers 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 abstract 1
- XJKSTNDFUHDPQJ-UHFFFAOYSA-N 1,4-diphenylbenzene Chemical compound C1=CC=CC=C1C1=CC=C(C=2C=CC=CC=2)C=C1 XJKSTNDFUHDPQJ-UHFFFAOYSA-N 0.000 description 11
- 229930184652 p-Terphenyl Natural products 0.000 description 11
- 238000004020 luminiscence type Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- MASVCBBIUQRUKL-UHFFFAOYSA-N POPOP Chemical compound C=1N=C(C=2C=CC(=CC=2)C=2OC(=CN=2)C=2C=CC=CC=2)OC=1C1=CC=CC=C1 MASVCBBIUQRUKL-UHFFFAOYSA-N 0.000 description 2
- 241000209456 Plumbago Species 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- PJANXHGTPQOBST-VAWYXSNFSA-N Stilbene Natural products C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000005658 nuclear physics Effects 0.000 description 2
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000146 host glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- MYWUZJCMWCOHBA-VIFPVBQESA-N methamphetamine Chemical compound CN[C@@H](C)CC1=CC=CC=C1 MYWUZJCMWCOHBA-VIFPVBQESA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
本发明公开了一种一种有机掺杂铅锡氟磷酸盐闪烁玻璃及其制备方法，其组成及组成的摩尔比为：52.2SnF2·10.5SnO·5.1PbF2·32.1NH4H2PO4·0.089芪420·0.066p-TP，制备方法如下：将SnF2、SnO、PbF2、NH4H2PO4原料混合并研磨均匀后，加入到坩埚中放在炉中熔化处理，当无大量白烟冒出时加入芪420，并加盖水平摇匀，加入p-TP并摇匀，将坩埚置于真空干燥箱中保温后取出坩埚。将熔体模具中，模具冷却至室温即获得透明的亚纳秒级超快p-TP和芪420双掺PTFP闪烁玻璃。本发明所采用的一步熔融法具有操作简单、方便、降低成本、提高闪烁玻璃透射率等优点。The invention discloses an organic-doped lead-tin fluorophosphate scintillation glass and a preparation method thereof. The composition and the molar ratio of the composition are: 52.2SnF 2 ·10.5SnO·5.1PbF 2 ·32.1NH 4 H 2 PO 4 0.089 stilbene 420 0.066p-TP, the preparation method is as follows: mix and grind SnF 2 , SnO, PbF 2 , NH 4 H 2 PO 4 raw materials evenly, add them into a crucible and melt them in a furnace. When white smoke comes out, add stilbene 420, cover it and shake it horizontally, add p-TP and shake it evenly, put the crucible in a vacuum drying oven for heat preservation, and then take out the crucible. Put the melt into the mold, and cool the mold to room temperature to obtain transparent subnanosecond ultrafast p-TP and stilbene 420 double-doped PTFP scintillation glass. The one-step melting method adopted in the present invention has the advantages of simple and convenient operation, reduced cost, improved scintillation glass transmittance and the like.
Description
Technical field
The present invention relates to a kind of scintillation glass and preparation method thereof, relate in particular to a kind of organic blended lead-tin-fluorine-phosphate flash glass and preparation method thereof.
Background technology
Along with the fast development of high energy physics, nuclear physics and Application of Nuclear Technology, inorganic scintillation crystal commonly used will be difficult to satisfy the needs of superelevation counting rate in measuring, and various countries are actively developing the research of novel fast flashing body in recent years for this reason.In conjunction with the ultrafast fall time of organic scintillator, the output of high light and the high-density of inorganic scintillation glass, the advantage of good resistance radiation damage, to obtain novel fast flashing glass, this is a research focus of present scintillation material preparation field.For example, the people such as C.Smith of U.S. Lawrence Livermore National Laboratory in 1994 are at Mat.Res.Soc.Proc., 1994, Vol.348, the article of delivering on the P209 is to be matrix with low-melting lead-Xi-fluorophosphate (PTFP), organic activators such as doping stilbene, POPOP, stilbene 420 use open glass carbon crucible, prepare the compound scintillation glass of organic and inorganic by a step scorification.These glass have the decay of luminescence speed (less than 1ns) that is exceedingly fast, but luminous a little less than.The domestic Zhao Hong of Northwestern Polytechnical University gives birth to and waits the people at Nucl.Instr.and Meth.A, 2000, Vol.448, P550 and Northwestern Polytechnical University's journal, 2000, Vol.18, No.2, the article of delivering on the P225 is to use uncovered ceramic crucible, also develops some organic activators (as p-TP, p-QP and POPOP etc.) doped P TFP organic and inorganic compound glass in succession by two step scorifications.But its fall time, about 5ns showed the Weak-luminescence characteristic.
Up to now, domestic also not about the report of fall time in the organic blended fast flashing glass preparation of subnanosecond level.
Summary of the invention
One of purpose of the present invention is to provide a kind of organic blended lead-tin-fluorine-phosphate flash glass;
Another object of the present invention is to provide the preparation method of this scintillation glass.
Goal of the invention of the present invention is achieved by the following technical solution:
In order to obtain the fast flashing material of fall time in the subnanosecond level, the present invention adopts p-terphenyl (p-TP) and 420 pairs of stilbenes to mix preparation PTFP (lead-tin-fluorine-phosphate) fast flashing glass.The prepared glass that goes out reaches 0.48ns fall time, is better than the fastest inorganic scintillator commonly used---BaF at present on luminescence decay time
2Crystal (its luminous fast, composition fall time be 0.6ns).And the density height of this kind glass is (greater than 4g/cm
3), chemical stability is good.
Select for use analytically pure p-TP and stilbene 420 to be doping agent, analytically pure SnF
2, SnO, PbF
2, NH
4H
2PO
4Be the raw material of preparation PTFP host glass, the mol ratio of various compositions is: 52.2SnF
210.5SnO5.1PbF
232.1NH
4H
2PO
40.089 stilbene 4200.066p-TP adopts and adds a cover the fast flashing glass that a step scorification is prepared the subnanosecond level.
The preparation method is as follows: by the SnF of above-mentioned given mol ratio
2, SnO, PbF
2, NH
4H
2PO
4Raw material mixes and grinds evenly.Earlier, allow crucible naturally cool to after the room temperature again with the preheating 10～15 minutes under 300～350 ℃ temperature of plated film high purity graphite crucible.To join through the abrasive of drying treatment in the crucible, crucible places 400 ℃ stove melt processed 0.5～1 hour.From stove, take out crucible, open crucible cover, do not add stilbene 420 when a large amount of white cigarettes are emerged, and the level of adding a cover shakes up, then crucible is placed 245 ℃ loft drier constant temperature to handle 5～20 minutes when having.Take out crucible once more from stove, adding p-TP also shakes up, and crucible is placed 245 ℃ vacuum drying oven, is incubated and takes out crucible after 3～5 minutes.Melt is injected the copper mould of 60 ℃ of insulations, treated to send into after melt solidifies in 60 ℃ of baking ovens insulation 10 minutes, mold cools down to room temperature, is obtained transparent ultrafast p-TP of subnanosecond level and 420 pairs of stilbenes and mixes the PTFP scintillation glass.
Adopt the prepared glass that goes out of the present invention, exciting down relatively at gamma-rays, light output is about 0.9% of plastic scintillator ST401; Aspect decay of luminescence speed, be better than at present the fastest commonly used inorganic scintillator for reaching 0.48ns the fall time of this kind glass
BaF
2Crystal (its luminous fast composition fall time be 0.6ns).This kind glass has also that melt temperature is low, density is high (greater than 4g/cm simultaneously
3), and series of advantages such as good optical performance and chemical stability.Therefore this p-TP and 420 pairs of stilbenes are mixed the big irradiation dose that PTFP glass is specially adapted to fields such as high energy physics, nuclear physics and nuclear technique, the measurement in the superelevation counting rate.
Aspect preparation technology, adopt and to add a cover plated film high purity graphite crucible, prepare the ultrafast p-TP of subnanosecond level and 420 pairs of stilbenes are mixed the PTFP scintillation glass by a step scorification.A step scorification that is adopted has simple, convenient advantage.Scintillation glass is founded and is carried out vacuum heat-preserving in the process, has improved the transmissivity of glass in ultraviolet-visible region.Crucible is added a cover in use, is convenient to reduce the component volatilization in the glass smelting process, can also be with NH
4H
2PO
4The ammonia that thermal degradation produces is founded black SnO and the yellow PbO that generates because of oxidation in the process as the restitutive protection's gas in the glass smelting process with minimizing, reaches the purpose that improves the scintillation glass transmissivity.The plated film high purity graphite crucible that is adopted helps increasing the compactness of plumbago crucible, avoids graphite on the sidewall of crucible to come off and the impurity introduced; Because fluorine and phosphorus in the PTFP glass are extremely strong to the corrosive nature of crucible, with respect to the vitreous carbon crucible, plumbago crucible is more cheap, thereby can reduce the preparation cost of glass.
Embodiment
How further specify this civilization below in conjunction with specific embodiment realizes:
Embodiment
Raw materials used is analytically pure SnF
2, SnO, PbF
2, NH
4H
2PO
4, stilbene 420 and p-TP, 52.2SnF in molar ratio
210.5SnO5.1PbF
232.1NH
4H
2PO
4Take by weighing each constituent element, make its gross weight be about 15 grams.
Raw material mixing and grinding is even.Earlier about 10 minutes, allow crucible naturally cool to after the room temperature in preheating under 300 ℃ the temperature again in plated film high purity graphite crucible.To join through the abrasive of drying treatment in the crucible, crucible places 400 ℃ stove melt processed 45 minutes.Take out crucible from stove, open crucible cover, when there not being the stilbene 420 that adds 0.5 milligram when a large amount of white cigarettes are emerged, and the level of adding a cover shakes up, and then crucible placed 245 ℃ loft drier constant temperature to handle 10 minutes.From stove, take out crucible once more, add 24 milligrams p-TP and shake up, crucible is placed 245 ℃ vacuum drying oven, be incubated and take out crucible after 3 minutes.Melt is injected the copper mould of 60 ℃ of insulations, treated to send into after melt solidifies in 60 ℃ of baking ovens insulation 10 minutes, mold cools down to room temperature, is obtained transparent ultrafast p-TP of subnanosecond level and 420 pairs of stilbenes and mixes the PTFP scintillation glass.
Claims (4)
1, a kind of organic blended lead-tin-fluorine-phosphate flash glass, the mol ratio of its composition and composition is: SnF
2: SnO: PbF
2: NH
4H
2PO
4: stilbene 420: p-TP=52.2: 10.5: 5.1: 32.1: 0.089: 0.066.
2, at the preparation method of the described a kind of organic blended lead-tin-fluorine-phosphate flash glass of claim 1, step is as follows:
A, by the analytically pure SnF of given mol ratio
2, SnO, PbF
2, NH
4H
2PO
4Raw material mixes and also to grind evenly, earlier with the preheating of plated film high purity graphite crucible, allow crucible naturally cool to room temperature again after, will join through the abrasive of drying treatment in the crucible, crucible places 400 ℃ stove melt processed 0.5～1 hour;
B, from stove, take out crucible, open crucible cover, do not add stilbene 420 when a large amount of white cigarettes are emerged, and the level of adding a cover shakes up, then crucible is placed 245 ℃ loft drier constant temperature to handle 5～20 minutes when having;
C, from stove, take out crucible once more, add analytically pure p-TP and shake up, crucible is placed 245 ℃ vacuum drying oven, be incubated and take out crucible after 3～5 minutes;
D, melt is injected the copper mould of 60 ℃ of insulations, treat to send into after melt solidifies in 60 ℃ of baking ovens after the insulation, mold cools down to room temperature, is obtained transparent ultrafast p-TP of subnanosecond level and 420 pairs of stilbenes and mixes lead-tin-fluorine-phosphate flash glass.
3, the preparation method of a kind of organic blended lead-tin-fluorine-phosphate flash glass according to claim 2 is characterized in that: the preheating temperature of the plated film high purity graphite crucible in the described A step is 300～350 ℃.
4, the preparation method of a kind of organic blended lead-tin-fluorine-phosphate flash glass according to claim 2 is characterized in that: send into behind the melt solidifying in the described D step that soaking time is 10 minutes in 60 ℃ of baking ovens.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100665459A CN100336754C (en) | 2004-09-21 | 2004-09-21 | Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100665459A CN100336754C (en) | 2004-09-21 | 2004-09-21 | Organic blended lead-tin-fluorine-phosphate flash glass and its preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1587141A CN1587141A (en) | 2005-03-02 |
| CN100336754C true CN100336754C (en) | 2007-09-12 |
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|---|---|---|---|
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099095A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Neodymium-and-ytterbium-codoped stannic fluoride glass up-conversion luminescent material, and preparation method and application thereof |
| CN106324658B (en) * | 2015-06-30 | 2019-04-23 | 中国辐射防护研究院 | The method adulterated the plastic scintillant of neutron-sensitive substance cadmium and its measure thermal neutron |
| CN116606068A (en) * | 2023-05-23 | 2023-08-18 | 中国科学院高能物理研究所 | Glass scintillator and preparation method thereof, scintillation optical fiber, scintillation detector |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087066A (en) * | 1992-11-17 | 1994-05-25 | 浙江大学 | High-density, radiotolerant fast flash inorganic glass |
| CN1246452A (en) * | 1998-09-02 | 2000-03-08 | 西北工业大学 | Lead halophosphate glass |
| CN1400193A (en) * | 2001-07-30 | 2003-03-05 | 通用电气公司 | Flashing agent composite of alkali metal and rare earth metal tungstate |
-
2004
- 2004-09-21 CN CNB2004100665459A patent/CN100336754C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087066A (en) * | 1992-11-17 | 1994-05-25 | 浙江大学 | High-density, radiotolerant fast flash inorganic glass |
| CN1246452A (en) * | 1998-09-02 | 2000-03-08 | 西北工业大学 | Lead halophosphate glass |
| CN1400193A (en) * | 2001-07-30 | 2003-03-05 | 通用电气公司 | Flashing agent composite of alkali metal and rare earth metal tungstate |
Non-Patent Citations (3)
| Title |
|---|
| 掺杂p-TP和POPOP的闪烁玻璃的研究 朱冬梅，赵宏生，周万城，西北工业大学学报，第19卷第2期 2001 * |
| 掺杂对三联苯的铅-锡-氟磷酸盐闪烁玻璃的研究 赵宏生，周万城，西北工业大学学报，第18卷第2期 2000 * |
| 闪烁玻璃的研究进展 赵宏生，周万城，材料导报，第15卷第1期 2001 * |
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| CN1587141A (en) | 2005-03-02 |
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