CN104743885A - Rare earth-doped oxyfluoride germanate microcrystalline glass and preparation method thereof - Google Patents
Rare earth-doped oxyfluoride germanate microcrystalline glass and preparation method thereof Download PDFInfo
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- CN104743885A CN104743885A CN201510123499.XA CN201510123499A CN104743885A CN 104743885 A CN104743885 A CN 104743885A CN 201510123499 A CN201510123499 A CN 201510123499A CN 104743885 A CN104743885 A CN 104743885A
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- 239000011521 glass Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 238000007669 thermal treatment Methods 0.000 claims abstract description 7
- UOBPHQJGWSVXFS-UHFFFAOYSA-N [O].[F] Chemical compound [O].[F] UOBPHQJGWSVXFS-UHFFFAOYSA-N 0.000 claims description 15
- 239000000156 glass melt Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 7
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 4
- 238000004455 differential thermal analysis Methods 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- -1 rare earth ions Chemical class 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000004020 luminiscence type Methods 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 abstract 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910001632 barium fluoride Inorganic materials 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- 238000007578 melt-quenching technique Methods 0.000 abstract 1
- 239000002159 nanocrystal Substances 0.000 abstract 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- VLIDWTIBMJLJIS-UHFFFAOYSA-N [Bi]=O.[F] Chemical compound [Bi]=O.[F] VLIDWTIBMJLJIS-UHFFFAOYSA-N 0.000 description 3
- 239000005383 fluoride glass Substances 0.000 description 3
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 3
- 238000004031 devitrification Methods 0.000 description 2
- 239000000146 host glass Substances 0.000 description 2
- 238000001748 luminescence spectrum Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 241000024287 Areas Species 0.000 description 1
- 229910004379 HoF 3 Inorganic materials 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- LVEULQCPJDDSLD-UHFFFAOYSA-L cadmium fluoride Chemical compound F[Cd]F LVEULQCPJDDSLD-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000002498 deadly effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000006017 silicate glass-ceramic Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Glass Compositions (AREA)
Abstract
The invention discloses rare earth-doped oxyfluoride germanate microcrystalline glass and a preparation method thereof, and belongs to the technical field of luminescent materials. The microcrystalline glass comprises the following components in percentage by mole: 39-55% of GeO2, 5-15% of ZnO, 5-15% of AlF3, 10-25% of BaF2, 1-10% of Na2O, 1-20% of NaF and 0.5-5% of RF2 (R is rare earth elements). The preparation method comprises the following steps: firstly preparing oxyfluoride germanate glass by using a melt quenching method; and then, carrying out micro-crystallization on matrix glass by virtue of a thermal treatment process to obtain transparent oxyfluoride germanate microcrystalline glass, wherein the prepared oxyfluoride germanate microcrystalline glass has good transmission of light in a range from near-infrared rays to visible light, and the up-conversion luminescence of rare earth ions is remarkably enhanced. The prepared rare earth-doped oxyfluoride germanate microcrystalline glass containing NaBaAlF6 nano-crystals is simple in preparation method, high in environmental-friendly safety and relatively low in production cost.
Description
Technical field
The present invention relates to a kind of rear-earth-doped fluorine oxygen germanate devitrified glass and preparation method thereof, devitrified glass up-conversion luminescent material that particularly a kind of rear-earth-doped fluoride is nanocrystalline and preparation method thereof, belongs to luminescent material technical field.
Background technology
Rear-earth-doped frequency inverted luminescence technology has huge potential using value in fields such as solid-state laser, data storage, general illumination, 3 D stereo display, micro-imaging, sensing technology, solar cell, anti-counterfeiting technology and military confrontations, therefore, extensive research has been carried out to rear-earth-doped luminous material both at home and abroad.
Result of study shows, heat-treats rare earth institute doped substrate glass, and after crystalline phase appears in inside glass, rare earth ion preferentially in the inner enrichment of precipitation crystalline phase, can improve the frequency inverted luminous efficiency of rare earth ion greatly.Based on this, rear-earth-doped oxy-fluoride glass obtains large quantifier elimination at visible ray to the up-conversion luminescence near infrared wavelength region, and achieves abundant meaningful achievement.But the preparation of oxy-fluoride glass generally needs the deadly poisonous compound such as plumbous fluoride and cadmium fluoride as nucleator, consider from environmental angle, this severely limits its practical application.Therefore, people have developed alkaline including earth metal fluorochemical and the nanocrystalline devitrified glass of heavy metal fluoride sodium salt, to solve above-mentioned environmental issue.
In addition, fluorine oxygen bismuth germanate glass combines the advantage of bismuth germanate glass and crystal of fluoride, and maximum phonon energy is low, near infrared to visible wavelength range, have good light transmission, makes this component glass become the hot-candidate material of the Application Areass such as laser.At present, the Hu of domestic Kunming University of Science and Technology is said and rich is waited people to have reported for work Tm
3+/ Er
3+/ Yb
3+three mix containing BaF
2the fluorine oxygen germanate microcrystal glass material of nanometer crystalline phase.In addition, the people such as Xu Shiqing of the China Measures Institute has reported for work and has comprised β-NaGdF
4: Er
3+the fluorine oxygen silicate glass-ceramics of nanometer crystalline phase.But the research of separating out alkaline-earth metal fluoride sodium salt nanometer crystalline phase in rear-earth-doped fluorine oxygen bismuth germanate glass is not yet seen in report.
Summary of the invention
The object of this invention is to provide a kind of transparent rear-earth-doped oxy-fluoride glass, this devitrified glass has excellent thermostability and Safety and Environmental Protection, in visible ray near infrared wavelength region, there is good light transmission, and rare earth luminescence intensity obtains large increase; This rear-earth-doped glass frequency inverted luminescent material is obtained by following raw material, and each raw material and molar percentage are: GeO
239 ~ 55 mol %, ZnO 5 ~ 15 mol %, AlF
35 ~ 15 mol %, BaF
210 ~ 25 mol %, Na
2o 1 ~ 10 mol %, NaF1 ~ 20 mol %, RF
30.5 ~ 5 mol %, wherein R is one or more in rare earth element y b, Er, Tm, Nb, Ho, Tb.
Another object of the present invention is to the preparation method that above-mentioned rear-earth-doped fluorine oxygen germanate devitrified glass is provided, specifically comprise the steps:
(1) raw material is fully mixed be placed in crucible with cover, 30 ~ 60 min are founded at 1350 ~ 1450 DEG C, raw material is made to be melting into glass melt, glass melt is cast to fast on the Stainless Molding Board being preheating to 300 ~ 400 DEG C, after shaping, insulation 4 ~ 8 h carry out annealing and naturally cooling to room temperature at lower than glass transformation temperature 20 ~ 50 DEG C, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish;
(2) glass containing rare earth ion step (1) prepared carries out differential thermal analysis, according to differential thermal analysis experiment, the obtained glass containing rare earth ion is placed in annealing furnace and heat-treats 15 ~ 60 min within the scope of T ~ T-50 DEG C, wherein T is the second crystallization peak temperature, and namely high temperature taking-up obtains rear-earth-doped containing NaBaAlF
6nanocrystalline transparent fluorine oxygen germanate devitrified glass.
Beneficial effect of the present invention is:
(1) what prepared by the present invention is rear-earth-doped containing NaBaAlF
6nanocrystalline fluorine oxygen germanate devitrified glass luminescent properties is good, and the experiment proved that, the devitrified glass after thermal treatment significantly improves than the Up-conversion Intensity of host glass;
(2) what prepared by the present invention is rear-earth-doped containing NaBaAlF
6nanocrystalline fluorine oxygen germanate devitrified glass has good light transmission near infrared to visible wavelength range;
(3) what prepared by the present invention is rear-earth-doped containing NaBaAlF
6nanocrystalline fluorine oxygen germanate devitrified glass preparation method is simple, and environmental safety is high, and production cost is lower.
Accompanying drawing explanation
Fig. 1 is doped in fluorine oxygen germanate presoma glass and contains NaBaAlF in embodiment 2
6er in nanocrystalline fluorine oxygen germanate devitrified glass
3+the up-conversion luminescence spectrum comparison diagram of ion.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described, but protection scope of the present invention is not limited to described content.
Embodiment 1
By composition 39GeO
220BaF
210ZnO10AlF
310Na
2o10NaF0.2ErF
30.3TmF
30.5YbF
3(mol%) GeO needed for total mass 10 grams is taken
2, BaF
2, ZnO, AlF
3, Na
2cO
3, NaF, ErF
3, TmF
3and YbF
3powder stock, abundant mixing load afterwards be placed in 1450 DEG C in crucible with cover at found 60min, then glass melt is cast to fast on the Stainless Molding Board being preheating to 400 DEG C, at the temperature lower than glass transformation temperature 20 DEG C, 4 h are incubated after shaping, Temperature fall is to room temperature, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish; By obtained glass thermal treatment 60 min at lower than the second crystallization peak temperature 50 DEG C, naturally cool to room temperature, namely obtain containing NaBaAlF
6nanocrystalline rear-earth-doped devitrified glass.
Embodiment 2
By composition 43.5GeO
225BaF
25ZnO5AlF
31Na
2o20NaF0.5ErF
3(mol%) GeO needed for total mass 10 grams is taken
2, BaF
2, ZnO, AlF
3, Na
2cO
3, NaF and ErF
3powder stock, abundant mixing load afterwards be placed in 1350 DEG C in crucible with cover at found 45min, then glass melt is cast to fast on the Stainless Molding Board being preheating to 300 DEG C, at the temperature lower than glass transformation temperature 50 DEG C, 8 h are incubated after shaping, Temperature fall is to room temperature, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish; By obtained glass thermal treatment 15min under the second crystallization peak temperature, naturally cool to room temperature, namely obtain containing NaBaAlF
6nanocrystalline rear-earth-doped devitrified glass.
Er in the present embodiment 2
3+doped with fluorine oxygen bismuth germanate glass and containing NaBaAlF
6the up-conversion luminescence spectrum of nanocrystalline fluorine oxygen germanate devitrified glass as shown in Figure 1; As can be seen from the figure, with Er in host glass
3+up-conversion luminescence compare, Er that devitrified glass adulterates in the present embodiment
3+up-conversion Intensity been significantly enhanced.
Embodiment 3
By composition 55GeO
210BaF
215ZnO15AlF
35Na
2o5NaF0.2ErF
30.8TbF
34YbF
3(mol%) GeO needed for total mass 10 grams is taken
2, BaF
2, ZnO, AlF
3, Na
2cO
3, NaF, ErF
3, TbF
3and YbF
3powder stock, abundant mixing load afterwards be placed in 1400 DEG C in crucible with cover at found 30 min, then glass melt is cast to fast on the Stainless Molding Board being preheating to 350 DEG C, at the temperature lower than the second crystallization peak temperature 30 DEG C, 5 h are incubated after shaping, Temperature fall is to room temperature, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish; By obtained glass thermal treatment 30 min at lower than devitrification of glass temperature 30 DEG C, naturally cool to room temperature, namely obtain containing NaBaAlF
6nanocrystalline rear-earth-doped devitrified glass.
Embodiment 4
By composition 48.5GeO
215BaF
212ZnO10AlF
310Na
2o1NaF0.5NbF
31HoF
32YbF
3(mol%) GeO needed for total mass 10 grams is taken
2, BaF
2, ZnO, AlF
3, Na
2cO
3, NaF, NbF
3, HoF
3and YbF
3powder stock, abundant mixing load afterwards be placed in 1380 DEG C in crucible with cover at found 40 min, then glass melt is cast to fast on the Stainless Molding Board being preheating to 380 DEG C, at the temperature lower than the second crystallization peak temperature 40 DEG C, 6 h are incubated after shaping, Temperature fall is to room temperature, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish; By obtained glass thermal treatment 45 min at lower than devitrification of glass temperature 40 DEG C, naturally cool to room temperature, namely obtain containing NaBaAlF
6nanocrystalline rear-earth-doped devitrified glass.
Claims (2)
1. a rear-earth-doped fluorine oxygen germanate devitrified glass, is characterized in that: this rear-earth-doped glass frequency inverted luminescent material is obtained by following raw material, and each raw material and molar percentage are: GeO
239 ~ 55 mol %, ZnO 5 ~ 15 mol %, AlF
35 ~ 15 mol %, BaF
210 ~ 25 mol %, Na
2o 1 ~ 10 mol %, NaF1 ~ 20 mol %, RF
30.5 ~ 5 mol %, wherein R is one or more in rare earth element y b, Er, Tm, Nb, Ho, Tb.
2. the preparation method of rear-earth-doped fluorine oxygen germanate devitrified glass according to claim 1, is characterized in that, specifically comprise the steps:
(1) raw material is fully mixed be placed in crucible with cover, 30 ~ 60 min are founded at 1350 ~ 1450 DEG C, raw material is made to be melting into glass melt, glass melt is cast to fast on the Stainless Molding Board being preheating to 300 ~ 400 DEG C, after shaping, insulation 4 ~ 8 h carry out annealing and naturally cooling to room temperature at lower than glass transformation temperature 20 ~ 50 DEG C, obtain the glass containing rare earth ion, and obtained glass is carried out cut, grind and polished finish;
(2) glass containing rare earth ion step (1) prepared carries out differential thermal analysis, according to differential thermal analysis experiment, the obtained glass containing rare earth ion is placed in annealing furnace thermal treatment 15 ~ 60 min within the scope of T ~ T-50 DEG C, wherein T is the second crystallization peak temperature, and namely high temperature taking-up obtains rear-earth-doped containing NaBaAlF
6nanocrystalline transparent fluorine oxygen germanate devitrified glass.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107445478A (en) * | 2017-08-31 | 2017-12-08 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium of Tm sensitizations and preparation method thereof |
CN107601869A (en) * | 2017-08-31 | 2018-01-19 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium of Yb sensitizations and preparation method thereof |
CN108863087A (en) * | 2018-07-30 | 2018-11-23 | 吉林工程技术师范学院 | A kind of rear-earth-doped niobates transparent glass ceramics and preparation method thereof |
CN112010564A (en) * | 2020-08-25 | 2020-12-01 | 暨南大学 | Rare earth ion in-situ crystallization-based fluorine-oxygen microcrystalline glass and preparation method and application thereof |
CN116282928A (en) * | 2022-12-07 | 2023-06-23 | 中国计量大学 | Gallium/zinc aluminate doped near-infrared tellurium germanate nanocrystalline glass and preparation method thereof |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107445478A (en) * | 2017-08-31 | 2017-12-08 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium of Tm sensitizations and preparation method thereof |
CN107601869A (en) * | 2017-08-31 | 2018-01-19 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium of Yb sensitizations and preparation method thereof |
CN107445478B (en) * | 2017-08-31 | 2019-10-25 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium and preparation method thereof of Tm sensitization |
CN107601869B (en) * | 2017-08-31 | 2019-10-25 | 中国计量大学 | A kind of tellurate luminous glass of environment-friendly type germanium and preparation method thereof of Yb sensitization |
CN108863087A (en) * | 2018-07-30 | 2018-11-23 | 吉林工程技术师范学院 | A kind of rear-earth-doped niobates transparent glass ceramics and preparation method thereof |
CN112010564A (en) * | 2020-08-25 | 2020-12-01 | 暨南大学 | Rare earth ion in-situ crystallization-based fluorine-oxygen microcrystalline glass and preparation method and application thereof |
CN112010564B (en) * | 2020-08-25 | 2022-04-22 | 暨南大学 | Rare earth ion in-situ crystallization-based fluorine-oxygen microcrystalline glass and preparation method and application thereof |
CN116282928A (en) * | 2022-12-07 | 2023-06-23 | 中国计量大学 | Gallium/zinc aluminate doped near-infrared tellurium germanate nanocrystalline glass and preparation method thereof |
CN116282928B (en) * | 2022-12-07 | 2024-01-26 | 中国计量大学 | Gallium/zinc aluminate doped near-infrared tellurium germanate nanocrystalline glass and preparation method thereof |
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