CN1526673A - Quick flashing glass and its prepn process - Google Patents
Quick flashing glass and its prepn process Download PDFInfo
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- CN1526673A CN1526673A CNA031156223A CN03115622A CN1526673A CN 1526673 A CN1526673 A CN 1526673A CN A031156223 A CNA031156223 A CN A031156223A CN 03115622 A CN03115622 A CN 03115622A CN 1526673 A CN1526673 A CN 1526673A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
- C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The present invention discloses one kind of quick flashing glass for application in high-energy physics, nuclear physics, nuclear medicine, geophysics, industrial detection and other fields and its preparation process. The flashing glass material has silicate glass, germanate glass other heavy metal oxide as main component, and introduced high-density ZnO as luminescent center. It is prepared through three steps of preparing glass material; smelting the material; and heat treatment. Test shows that the serial glass material has the features of simple smelting process, powerful glass forming capacity, easy density regulation and high luminescent ion density. Compared with available Ce3+-doping quick flashing glass, the present invention has the features of high UV transmissibility, fast attenuation and high fluorescent strength.
Description
Technical field
The present invention relates to scintillator material and preparation method thereof, especially relating to ZnO is fast blink glass of luminescence center and preparation method thereof.
Background technology
Along with the expansion in mankind's activity field and the raising of scientific and technological level, the performance of scintillation material has been proposed new requirement, especially require scintillator to have high resolving power and high radiation hardness ability.Use for this type of, and some traditional scintillation materials (as NaI:Tl, CsI:Tl, BGO) grade can not satisfy its service requirements.Since the nineties in 20th century, the research of opening up and formulating the novel fast blink material that is applied to fields such as high energy physics there have been many reports both at home and abroad.Except scintillation crystal, the research and development of scintillation glass are also quite noticeable, and this is main because the preparation cost of glass is more much lower than crystal, the latter reaches tens cubic metres the required atmospheric shimmer body of calorimeter of new generation to the preparation volume, is an important factor that can not be ignored.In the scintillation glass of report, studying maximum is with Doped Rare Earth Ce
3+Ion is the scintillation glass of luminescence center.Ce
3+Galvanic couple allowed transition between the luminous genus of ionic 4f-5d, having, (50ns), can be used for the detection of quick incident the fall time of weak point.But, Ce
3+Ion doping has following limitation: because Ce
3+Ionic concentration quenching effect is obvious, its introducing amount is restricted, thereby influences its luminous intensity; Because Ce
3+The light basicity sensitivity of ion pair host glass easily makes the ultraviolet of glass and visible absorbance cutoff wavelength produce red shift, thereby influences the ultraviolet and visible perviousness of glass; Because Ce
3+Ion easily loses an electronics and becomes quadrivalent ion (Ce
4+), the latter can produce absorb in the visible region, therefore found process and must adopt reducing atmosphere, can not adopt platinum crucible, can only be with quartz crucible or ceramic crucible, and problems such as bubble and striped are difficult to solve, thereby influence the optical homogeneity of glass.
With zinc oxide (ZnO) is that the scintillation glass of luminescence center can be described as the revolution in the scintillator material R and D field.The efficient band edge exciton transition of zinc oxide (ZnO) is luminous on the one hand has than cerium ion (Ce
3+) shorter fluorescence lifetime, thereby can obtain the required more high time resolution of quick incident detection, on the other hand, because ZnO itself belongs to glass network intermediate, can in glass is formed, introduce, and keep even further improve original glass forming ability and other physical and chemical performances with very high concentration.In addition, can in glass matrix, separate out zinc oxide (ZnO) crystal grain of nanoscale, make it luminously be subjected to the effect of quantum confinement effect and significantly strengthen by suitable thermal treatment.Simultaneously, because zine ion (Zn
2+) have stable valence state, therefore can adopt platinum crucible fusion cast glass in air, melting technology is simple, and the material homogeneity of preparation is good, the purity height.
Summary of the invention
One of the object of the invention, a kind of fast blink glass that can be applied to fields such as high energy physics, nuclear physics, nuclear medicine, earth physics, industry detection is provided, replace present widely used scintillation crystal with part, the latter has the cost of manufacture height, weakness such as in enormous quantities and large size production difficulty is big are applied in to a great extent it and are restricted.
Two of the object of the invention provides a kind of method for preparing above-mentioned fast blink glass.
Inventive concept:
Silicon-dioxide (SiO
2) and germanium dioxide (GeO
2) be the traditional glass organizer, it is wide to have glass formation compositing range, the oxide compound that can introduce is wide, density is easy to regulate, advantages such as ultraviolet and visible through performance and other physical and chemical performances are good especially can be used general forming technique, as mold pressing, hot pressing and extrusion technique, the preparation process of scintillator is simplified, and cost significantly reduces.Zinc oxide (ZnO) belongs to semi-conductor, and the room temperature band-gap energy is about 3.3eV, and its luminous genus alms giver falls into the bound exciton transition, has near ultraviolet and visible through performance is good, and decay is fast, characteristics such as fluorescence intensity height.With cerium ion (Ce
3+) luminous comparing, zinc oxide (ZnO) is luminous, and to have an optical attenuation faster, and fluorescence is stronger, introduces concentration height and the lower advantage of cost, is particularly useful for the detection of the quick incident of high precision.
The present invention be a kind of be the silicate or the germanate scintillation glass of luminescence center with zinc oxide (ZnO).The composition design of this system glass has taken into account following factor: the formation ability of glass, the high optical transmission of near ultraviolet and visible region, higher density, radiation resistance, high fluorescent and short fluorescence lifetime preferably.
Technical scheme:
Fast blink glass of the present invention comprises following component and content (content is in molar percentage mol%):
SiO
2Or GeO
215-50
R
2O
3?????????????????10-30
ZnO?????????????????????20-60
BaO?????????????????????0-20
M
2O
3?????????????????0-10
SnO
2??????????????????0-5
F
-????????????????????0-5
Wherein: R=Ga, B or Al; M=Gd or La.
The method for preparing above-mentioned fast blink glass comprises the steps:
A) preparation of glass batch:
Raw material is made glass batch by above-mentioned component and content behind thorough mixing.B wherein
2O
3And F
-Introduce with the form of boric acid and fluorochemical respectively.
B) founding of admixtion:
To place container to melt by the glass batch that step (a) makes, temperature of fusion be 1300-1420 ℃, and fusing time is 3-5 hour.Pour the glass metal of fusing in mould curing molding.Glass behind the curing molding is moved in the retort furnace, be incubated half an hour, get glass specimen after the cooling at 500 ℃.
Wherein: mould therefor preferably is heated to 500 ℃ in advance, and retort furnace is warming up to 500 ℃ in advance.
C) thermal treatment:
To make glass specimen by step (b) and be reentered into retort furnace, be 300-600 ℃ in temperature, is incubated 3-10 hour, promptly gets fast blink glass of the present invention after the cooling.
Invent described fast blink glass and the existing cerium (Ce that mixes
3+) fast blink glassy phase ratio, it is good then to have a ultraviolet through performance, and decay is fast, characteristics such as fluorescence intensity height; Simultaneously, it is simple that fast blink glass of the present invention has the process of founding again, and glass forming ability is strong, and density is easy to adjust, and the luminescence center ion is introduced the high characteristics of concentration.Invent described fast blink glass and can be applicable to fields such as high energy physics, nuclear physics, nuclear medicine, earth physics, industry detection.
Embodiment
Be better understanding content 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 silicon boron zinc three-part system.Design of components is as follows:
The glass of table 1 embodiment 1 is formed (mol%)
| SiO 2 | ?B 2O 3 | ?ZnO |
| 25 | ??15 | ??60 |
The admixtion preparation:
Adopt high purity (＞99.9%) quartz sand respectively, boric acid (H
3BO
3) and zinc oxide (ZnO) for introducing SiO
2, B
2O
3With the raw material of ZnO, carry out formula calculation and admixtion preparation 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 1350 ℃, and fusing time is 5 hours, glass metal is carried out hand mixing 3 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 500 ℃ in advance.Glass specimen after solidifying is moved in the retort furnace.Retort furnace is warming up to 500 ℃ in advance.Insulation after half an hour 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, is heated to through preferred determined temperature and insulation.Heating temperature is 450 ℃, and soaking time is 8 hours.Insulation after finishing is closed retort furnace, and glass specimen cools to room temperature with the furnace.
Test-results:
Resulting glass specimen is done the mensuration of fluorescence property test and density after surface grinding, polished finish.Test-results sees Table 2.
The fluorescence property of table 2 embodiment 1 glass and density test result
| Density (g/cm 3) | Excitation wavelength (nm) | Emission wavelength (nm) | Optical attenuation (ns) |
| ??4.1 | ??262 | ??393 | ??10 |
Embodiment 2-6
In each of the embodiments described below, the preparation method of glass is with embodiment 1, and the different glass composition that is adopted and temperature of fusion, thermal treatment temp/time and density and fluorescence property test-results are listed in table 3 and table 4 respectively.
The glass of table 3 embodiment 2-6 is formed (mol%)
| Sequence number | SiO 2 | ?GeO 2 | ?Ga 2O 3 | ?Al 2O 3 | ?B 2O 3 | ?BaO | ?M 2O 3 * | F - | ZnO |
| ?2 | ?30 | ?- | ?10 | ?- | ?- | ?- | ?- | ?- | ?60 |
| ?3 | ?30 | ?- | ?- | ?5 | ?- | ?5 | ?5 | ?- | ?55 |
| ?4 | ?- | ?25 | ?15 | ?- | ?- | ?5 | ?5 | ?- | ?50 |
| ?5 | ?- | ?35 | ?- | ?5 | ?- | ?10 | ?5 | ?- | ?45 |
| ?6 | ?- | ?30 | ?- | ?- | ?10 | ?15 | ?4 | ?1 | ?40 |
*M=Gd or La
The fluorescence property and the density test result of table 4 embodiment 2-6 glass
| Sequence number | Temperature of fusion (℃) | Thermal treatment temp/time (℃/hr) | Density (g/cm 3) | Excitation wavelength (nm) | Emission wavelength (nm) | Optical attenuation (ns) |
| ??2 | ??1380 | ??400/6 | ??4.30 | ??262 | ??393-400 | ??10-20 |
| ??3 | ??1400 | ??420/5 | ??4.35 | |||
| ??4 | ??1380 | ??350/8 | ??4.75 | |||
| ??5 | ??1380 | ??500/5 | ??4.70 | |||
| ??6 | ??1350 | ??450/10 | ??4.50 |
Claims (3)
1, a kind of fast blink glass is characterized in that, described glass comprises following component and content (content is in molar percentage):
SiO
2Or GeO
215-50
R
2O
3???????????????????????????????10-30
ZnO???????????????????????????????????20-60
BaO???????????????????????????????????0-20
M
2O
3???????????????????????????????0-10
SnO
2?????????????????????????????????0-5
F
-???????????????????????????????????0-5
Wherein: R=Ga, B or Al; M=Gd or La.
2, preparation claim 1 described glass method, it is characterized in that described preparation method comprises the steps:
A) preparation of glass batch
Raw material is made glass batch by claim 1 is described by described component 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 1300-1420 ℃, and fusing time is 3-5 hour, pour the glass metal of fusing in mould curing molding, glass after the moulding is moved in the retort furnace, be incubated half an hour, get glass specimen after the cooling at 500 ℃;
C) thermal treatment
To make glass specimen by step (b) and be reentered into retort furnace, be 300-600 ℃ in temperature, is incubated 3-10 hour, promptly gets fast blink 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 500 ℃ in the step (b), and retort furnace is warming up to 500 ℃ in advance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031156223A CN100486923C (en) | 2003-03-03 | 2003-03-03 | Quick flashing glass and its preparation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031156223A CN100486923C (en) | 2003-03-03 | 2003-03-03 | Quick flashing glass and its preparation process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1526673A true CN1526673A (en) | 2004-09-08 |
| CN100486923C CN100486923C (en) | 2009-05-13 |
Family
ID=34284368
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031156223A Expired - Fee Related CN100486923C (en) | 2003-03-03 | 2003-03-03 | Quick flashing glass and its preparation process |
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| Country | Link |
|---|---|
| CN (1) | CN100486923C (en) |
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 |
| CN102826753A (en) * | 2012-09-28 | 2012-12-19 | 井冈山大学 | Gd2O3-rich borogermanate scintillation glass, and preparation method and application thereof |
| CN103693847A (en) * | 2013-11-06 | 2014-04-02 | 中国科学院上海光学精密机械研究所 | Gadolinium borosilicate scintillating glass and preparation method thereof |
| CN105481250A (en) * | 2015-12-04 | 2016-04-13 | 哈尔滨工程大学 | Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof |
| CN108892375A (en) * | 2017-12-21 | 2018-11-27 | 中国计量大学 | A kind of SiGe silicate glass and preparation method thereof |
| CN114716142A (en) * | 2022-04-12 | 2022-07-08 | 中国计量大学上虞高等研究院有限公司 | ZnS quantum dot doped luminescent glass and preparation method and application thereof |
| CN114772922A (en) * | 2022-04-14 | 2022-07-22 | 中国建筑材料科学研究总院有限公司 | Scintillator glass for electromagnetic energy device, and preparation method, melting device and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3993301B2 (en) * | 1997-12-16 | 2007-10-17 | 株式会社住田光学ガラス | Oxide glass with long afterglow and stimulated emission |
-
2003
- 2003-03-03 CN CNB031156223A patent/CN100486923C/en not_active Expired - Fee Related
Cited By (13)
| 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 |
| 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 |
| CN103693847B (en) * | 2013-11-06 | 2016-05-11 | 中国科学院上海光学精密机械研究所 | Gadolinium borosilicate scintillation glass and preparation method thereof |
| CN103693847A (en) * | 2013-11-06 | 2014-04-02 | 中国科学院上海光学精密机械研究所 | Gadolinium borosilicate scintillating glass and preparation method thereof |
| CN105481250B (en) * | 2015-12-04 | 2018-02-13 | 哈尔滨工程大学 | With the water white transparency devitrified glass and preparation method that the characteristics of luminescence is changed under long afterglow |
| CN105481250A (en) * | 2015-12-04 | 2016-04-13 | 哈尔滨工程大学 | Colorless transparent glass-ceramic with long after-glow down-conversion luminescence characteristics and preparation method thereof |
| CN108892375A (en) * | 2017-12-21 | 2018-11-27 | 中国计量大学 | A kind of SiGe silicate glass and preparation method thereof |
| CN108892375B (en) * | 2017-12-21 | 2021-02-09 | 中国计量大学 | Silicon silicate glass and preparation method thereof |
| CN114716142A (en) * | 2022-04-12 | 2022-07-08 | 中国计量大学上虞高等研究院有限公司 | ZnS quantum dot doped luminescent glass and preparation method and application thereof |
| CN114716142B (en) * | 2022-04-12 | 2023-09-05 | 中国计量大学上虞高等研究院有限公司 | ZnS-doped quantum dot luminescent glass and preparation method and application thereof |
| CN114772922A (en) * | 2022-04-14 | 2022-07-22 | 中国建筑材料科学研究总院有限公司 | Scintillator glass for electromagnetic energy device, and preparation method, melting device and application thereof |
| CN114772922B (en) * | 2022-04-14 | 2024-01-26 | 中国建筑材料科学研究总院有限公司 | Scintillator glass for electromagnetic energy device, preparation method thereof, melting device and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100486923C (en) | 2009-05-13 |
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