CN103936281A - Rare earth doped luminescent glass, and preparation method thereof - Google Patents
Rare earth doped luminescent glass, and preparation method thereof Download PDFInfo
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- CN103936281A CN103936281A CN201410038959.4A CN201410038959A CN103936281A CN 103936281 A CN103936281 A CN 103936281A CN 201410038959 A CN201410038959 A CN 201410038959A CN 103936281 A CN103936281 A CN 103936281A
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- rare earth
- earth doped
- doped luminescent
- luminescent glass
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Abstract
The invention discloses rare earth doped luminescent glass, and a preparation method thereof. Main ingredients of glass matrix of the rare earth doped luminescent glass are B2O3, Al2O3, ZnO, CaF2, CaO and Na2O; and rare earth ions Tb<3+>, Sm<3+>, Eu<3+>, Dy<3+>, and Tm<3+> are luminescence centers. According to the preparation method, emitting of visible light is realized via single-doping, double-doping, or three-doping of the rare earth ions with glass matrix, and combination with ultraviolet LED chips; and the rare earth doped luminescent glass is prepared via melt cooling. Excitation of the rare earth doped luminescent glass can be realized by 350-400nm ultraviolet light, and emitting of visible light is realized; emission spectrum, chromaticity coordinate, and color temperature of the rare earth doped luminescent glass can be adjusted by changing the ingredients of the glass matrix, concentration of the rare earth ions, and excitation wavelength so as to realize material intelligent luminescence, and satisfy requirements of different using environments on luminescence performance; the rare earth doped luminescent glass possesses excellent luminescence performance, is a novel light conversion material with high application value, and can be used for LED luminescent devices so as to solve problems of existing LED luminescent devices that LED color stability is poor, and aging of encapsulating resin is easily caused.
Description
Technical field
The present invention relates to the luminescent material in luminescence display and illuminating engineering field and preparation method thereof, particularly a kind of rare earth doped luminescent glass and preparation method thereof.
Background technology
Illumination is the important component part of society energy consumption.The main product of traditional lighting is incandescent light and luminescent lamp.The common shortcoming of these two kinds of lamps is only sub-fraction electric energy to be transformed into visible ray, and other electric energy are transformed into infrared rays and heat, and light efficiency is low, the life-span is short, and luminescent lamp contains mercury, easily to environment.Photodiode (Light emitting diode, LED) is a kind of light emitting semiconductor device that electric energy is changed into luminous energy, and its optical radiation mainly concentrates on visible region, has reduced the harm of non-visible light district hertzian wave to human body.Compare with luminescent lamp with incandescent light, the features such as that LED has is energy-conservation, life-span length, environmental protection, low-voltage safety, white light emitting diode (W-LED) has the trend that replaces incandescent light and luminescent lamp, thereby becomes the leading of 21st century illumination.
Current business-like W-LED illuminating device is mainly by blue light InGaN semi-conductor chip and be subject to blue-light excitedly to send gold-tinted or phosphor combination red, green glow forms.This LED device has following deficiency: the homogeneity of glow color is wayward; Colour rendering index is on the low side; Encapsulating epoxy resin is easily aging; Easily produce temperature quenching effect, cause in use semi-conductor chip and light-emitting phosphor decrease in efficiency; Manufacturing cost is relatively high.LED makes great progress with the research of fluorescent material at present, but, no matter be that traditional fluorescent material system is optimized, or develop new fluorescent material chemical constitution, all can not overcome the inherent defect of powdered material.Rare earth ion doped fluorescent glass can be applicable to LED device, can be evenly dispersed in glass the colourity stay in grade of gained white light as the rare earth ion of luminescence center; Thermal stability is good, and be easily processed into various desired shapes, fluorescent glass can be made to suitable shape and LED chip and directly encapsulate, needn't adopt epoxy resin, thereby can make the manufacturing process of LED illuminating device simple, constant product quality, cost.Rare earth ion doped fluorescent glass has good physics, chemistry and thermal stability, has outstanding advantage for LED field.
Summary of the invention
Technical problem to be solved by this invention is open a kind of rare earth doped luminescent glass and preparation method thereof, and the illuminating candidate material of the LED of fluorescent material, relates generally to rear-earth-doped B as an alternative
2o
3-Al
2o
3-ZnO-CaF
2-CaO-Na
2o system fluorescent glass and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of rare earth doped luminescent glass, with B
2o
3-Al
2o
3-ZnO-CaF
2-CaO-Na
2o system glass is as matrix, and the rare earth ion in rare earth compound is as luminescence center, and described rare earth compound comprises Eu
2o
3, Tb
4o
7, Dy
2o
3, Sm
2o
3and Tm
2o
3, it is characterized in that: the molar percentage of described each component is: B
2o
3: 25%-60%, Al
2o
3: 0%-40%, ZnO:0%-25%, CaF
2: 0%-25%, CaO:0%-45%, Na
2o:0%-25%, Eu
2o
3: 0%-1%, Tb
4o
7: 0%-0.5%, Dy
2o
3: 0%-1%, Sm
2o
3: 0%-1%, Tm
2o
3: 0%-1%.
Described rare earth ion list mixes, twoly mix or three mix in glass matrix, coordinates ultraviolet LED chip to send visible ray.
Above-mentioned rear-earth-doped B provided by the invention
2o
3-Al
2o
3-ZnO-CaF
2-CaO-Na
2o system fluorescent glass adopts melt cooling legal system standby, and preparation method comprises the steps:
(1) determine the molar percentage of the contained each component of fluorescent glass;
(2) batching: select boric acid, aluminum oxide or aluminium hydroxide, zinc oxide, Calcium Fluoride (Fluorspan), calcium carbonate, the sodium carbonate raw material as glass matrix; Europium sesquioxide, terbium sesquioxide, Samarium trioxide, trioxide and dysprosium oxide are as the raw material of introducing rare earth ion; According to the various raw materials of glass composition accurate weighing of step (1) design, load weighted raw material is ground to 20-40 minute in agate mortar, mix, obtain glass batch;
(3) found: glass batch is packed in corundum or platinum crucible, be incubated 1-3 hour be warming up to 1350-1550 DEG C with the heat-up rate of 2-10 DEG C/min in High Temperature Furnaces Heating Apparatus after, obtain glass metal;
(4) be shaped and annealing: glass metal is poured in the stainless steel mould of preheating and be shaped, and send in retort furnace at 400-550 DEG C of annealing 1-2h, cool to room temperature with the furnace, obtain fluorescent glass.
In described shaping and annealing process, stainless steel mould need to use in retort furnace after 300-500 DEG C of preheating 15-40min, to prevent glass rupture.
Prepare according to the preparation method of above-mentioned rare earth doped luminescent glass with Eu
2o
3as the raw material of introducing Eu ion, in prepared glass, there is Eu
3+to Eu
2+conversion, this glass is founded under air atmosphere, illustrates that this glass can realize Eu
3+the reduction of ion, needn't take reducing atmosphere.
The invention has the beneficial effects as follows: the prepared fluorescent glass of the present invention has stable luminous under near ultraviolet excitation, variously photochromicly can be compounded to form white light.By changing host glass composition, rare earth ion doped kind and concentration, excitation wavelength can change the relative intensity of each emission band, adjust thus chromaticity coordinates and colour temperature, thereby realize the regulation and control of glass luminescent properties, be applicable to the requirement of different environments for use to LED device luminescent properties.The fluorescent glass the present invention relates to, does not adopt reducing atmosphere can realize Eu in preparation process
3+to Eu
2+conversion.The present invention, to solving the technical bottleneck of LED illumination, avoids some inferior positions of conventional fluorescent powder, the preparation of promotion related device and practical, significant.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is further illustrated.
The emmission spectrum of the fluorescent glass that accompanying drawing 1 is embodiment 1 under 372nm wavelength excites;
Accompanying drawing 2 is the fluorescent glass of embodiment 2 emmission spectrum under 372nm wavelength excites;
Accompanying drawing 3 is the fluorescent glass of embodiment 3 emmission spectrum under different wave length excites;
The emmission spectrum of the fluorescent glass that accompanying drawing 4 is embodiment 3 and embodiment 4 under 351nm wavelength excites;
The emmission spectrum of the fluorescent glass that accompanying drawing 5 is embodiment 5, embodiment 6 and embodiment 7 under 372nm wavelength excites;
Excitation spectrum under emmission spectrum and the 544nm wavelength monitor of the fluorescent glass that accompanying drawing 6 is embodiment 6 under 372nm wavelength excites.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated, but be not used for limiting the scope of the invention.
Embodiment 1:
(1) design glass molar percentage consists of 60B
2o
3-20CaF
2-10CaO-10Na
2o:0.05Eu
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 26.8826g, Calcium Fluoride (Fluorspan) 5.6572g, calcium carbonate 3.6264g, sodium carbonate 3.8402g and europium sesquioxide 0.0638g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1450 DEG C, and insulation 1h, obtains glass metal;
(4) glass metal is poured in the stainless steel mould of 400 DEG C of preheating 30min and be shaped, put into subsequently retort furnace in 450 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 1 is the emmission spectrum of the fluorescent glass prepared of embodiment 1 under 372nm wavelength excites, and while preparing this glass, we use Eu
2o
3introduce Eu ion, and emmission spectrum presents Eu
2+and Eu
3+the emission band of ion, illustrates a part of Eu
3+change into Eu
2+ion; This glass is founded under air atmosphere, illustrates that this glass can realize Eu
3+the reduction of ion, needn't take reducing atmosphere; It can also be seen that from emmission spectrum, this glass, under ultraviolet excitation, has emission band in blue light, green glow, orange-colored light and ruddiness region, and these several emission bands are compound can produce white light; Chromaticity coordinates is (x=0.32, y=0.28), and colour temperature is 6448K (seeing attached list 1).
Embodiment 2:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-20CaF
2-10CaO-10Na
2o:0.05Eu
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 16.4880g, aluminum oxide 9.7105g, Calcium Fluoride (Fluorspan) 5.9482g, calcium carbonate 3.8130g, sodium carbonate 4.0377g and europium sesquioxide 0.0670g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1450 DEG C, and insulation 1 h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 400 DEG C of preheating 30min and be shaped, put into subsequently retort furnace in 450 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
The emmission spectrum of the glass that accompanying drawing 2 is prepared for embodiment 2 under the exciting of 372nm UV-light, emission band derives from Eu
2+and Eu
3+transition of electron, in this glass, also there is Eu
3+to Eu
2+conversion, but transformation efficiency is lower than the glass of embodiment 1.
Embodiment 3:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-20CaF
2-20CaO:0.05Tm
2o
3, 0.125Dy
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 16.5069g, aluminum oxide 9.7216g, Calcium Fluoride (Fluorspan) 5.9550g, calcium carbonate 7.6346g, trioxide 0.0736g and dysprosium oxide 0.1778g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1450 DEG C, and insulation 1h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 450 DEG C of preheating 30min and be shaped, put into subsequently retort furnace in 450 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
The glass that accompanying drawing 3 is prepared for embodiment 3 351,358,364 and the exciting of 388nm UV-light under emmission spectrum, emmission spectrum comprises indigo plant, yellow emission band, derives from respectively Tm
3+and Dy
3+transition of electron, each emission band is compound can produce white light; The relative intensity ratio difference of the each emission band of emmission spectrum under different wave length excites, causes different chromaticity coordinatess and colour temperature (seeing attached list 1).
Embodiment 4:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-20ZnO-20CaF
2: 0.05Tm
2o
3, 0.125Dy
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 17.1071g, aluminum oxide 10.0751g, zinc oxide 6.4340g, Calcium Fluoride (Fluorspan) 6.1715g, trioxide 0.0763g and dysprosium oxide 0.1843g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1450 DEG C, and insulation 1h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 450 DEG C of preheating 30min and be shaped, put into subsequently retort furnace in 450 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
The emmission spectrum of the glass that accompanying drawing 4 is prepared for embodiment 4 under 351nm wavelength excites, emmission spectrum shows blue light and yellow emission band, can produce white light, for ease of comparing, the emmission spectrum of the glass in embodiment 3 under 351nm wavelength excites is also listed in accompanying drawing 4.Can find out the Tm of the glass of embodiment 4 from accompanying drawing 4
3+luminous intensity is apparently higher than embodiment 3, and this explanation can form to adjust by changing glass matrix the relative intensity of the each emission band of emmission spectrum, thereby adjusts chromaticity coordinates and the colour temperature of fluorescent glass.
Embodiment 5:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-40CaO:0.125Dy
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 15.8539g, aluminum oxide 9.3370g, calcium carbonate 14.6652g and dysprosium oxide 0.1708g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1470 DEG C, and insulation 1h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 470 DEG C of preheating 20min and be shaped, put into subsequently retort furnace in 470 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Embodiment 6:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-40CaO:0.125Dy
2o
3, 0.025Tb
4o
7;
(2) according to the glass composition of design in step (1), accurately take boric acid 15.8539g, aluminum oxide 9.3370g, calcium carbonate 14.6652g, dysprosium oxide 0.1708g and terbium sesquioxide 0.0685g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1470 DEG C, and insulation 1h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 470 DEG C of preheating 20min and be shaped, put into subsequently retort furnace in 470 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Excitation spectrum under emmission spectrum and the 544nm wavelength monitor of the fluorescent glass that accompanying drawing 6 is embodiment 6 under 372nm wavelength excites, within the scope of wavelength 470-505nm, it is overlapping that emmission spectrum and excitation spectrum have, and illustrates in this glass, has Dy
3+to Tb
3+transmission ofenergy.
Embodiment 7:
(1) design glass molar percentage consists of 35B
2o
3-25Al
2o
3-40CaO:0.125Dy
2o
3, 0.025Tb
4o
7, 0.05Sm
2o
3;
(2) according to the glass composition of design in step (1), accurately take boric acid 15.8539g, aluminum oxide 9.3370g, calcium carbonate 14.6652g, dysprosium oxide 0.1708g, terbium sesquioxide 0.0685g and Samarium trioxide 0.0639g, these raw materials are fully ground in agate mortar to 20min, after mixing, obtain glass batch;
(3) glass batch is poured in corundum crucible, put into High Temperature Furnaces Heating Apparatus and melt, temperature of fusion is 1470 DEG C, and insulation 1h, obtains uniform glass metal;
(4) glass metal is poured in the stainless steel mould of 470 DEG C of preheating 20min and be shaped, put into subsequently retort furnace in 470 DEG C of annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
The emmission spectrum of the fluorescent glass that accompanying drawing 5 makes for embodiment 5, embodiment 6 and embodiment 7 372nm wavelength excites under, table 1 is colour temperature and the chromaticity coordinates of the fluorescent glass prepared of embodiment 1,3,4,5,6 and 7.
The glass luminescent properties parameter of table 1 embodiment 1,3,4,5,6 and 7
Each raw material that the present invention is cited and the bound value of each raw material, and the bound value of each processing parameter, can realize the present invention, do not enumerate embodiment at this.
Claims (5)
1. a rare earth doped luminescent glass, with B
2o
3-Al
2o
3-ZnO-CaF
2-CaO-Na
2o system glass is as matrix, and the rare earth ion in rare earth compound is as luminescence center, and described rare earth compound comprises Eu
2o
3, Tb
4o
7, Dy
2o
3, Sm
2o
3and Tm
2o
3, it is characterized in that: the molar percentage of described each component is: B
2o
3: 25%-60%, Al
2o
3: 0%-40%, ZnO:0%-25%, CaF
2: 0%-25%, CaO:0%-45%, Na
2o:0%-25%, Eu
2o
3: 0%-1%, Tb
4o
7: 0%-0.5%, Dy
2o
3: 0%-1%, Sm
2o
3: 0%-1%, Tm
2o
3: 0%-1%.
2. a kind of rare earth doped luminescent glass according to claim 1, is characterized in that: described rare earth ion list mixes, twoly mix or three mix in glass matrix.
3. the preparation method of a kind of rare earth doped luminescent glass according to claim 1, adopts melt cooling legal system for rare earth doped luminescent glass, it is characterized in that: comprise the steps:
(1) determine the molar percentage of the contained each component of fluorescent glass;
(2) batching: choose boric acid, aluminum oxide or aluminium hydroxide, zinc oxide, Calcium Fluoride (Fluorspan), calcium carbonate, sodium carbonate, europium sesquioxide, terbium sesquioxide, dysprosium oxide, Samarium trioxide and trioxide as raw material, according to the glass composition of design in step (1), the various raw materials of accurate weighing, these raw materials are ground to 20-40 min in agate mortar, mix, obtain glass batch;
(3) found: glass batch is packed in corundum or platinum crucible, in High Temperature Furnaces Heating Apparatus with 2-10
othe heat-up rate of C/min is warming up to 1350-1550
oafter C, be incubated 1-3 hour, obtain glass metal;
(4) be shaped and annealing: glass metal is poured in the stainless steel mould of preheating and be shaped, and send in retort furnace at 400-550
oc annealing 1-2 h, cools to room temperature with the furnace, obtains fluorescent glass.
4. the preparation method of a kind of rare earth doped luminescent glass according to claim 3, is characterized in that: stainless steel mould need to be in 300-500 in retort furnace
oafter C preheating 15-40 min, use.
5. the preparation method of a kind of rare earth doped luminescent glass according to claim 1 and a kind of rare earth doped luminescent glass claimed in claim 3, is characterized in that: with Eu
2o
3as the raw material of introducing Eu ion, in prepared glass, there is Eu
3+to Eu
2+conversion.
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|---|---|---|---|
| CN201410038959.4A CN103936281B (en) | 2014-01-26 | 2014-01-26 | A kind of rare earth doped luminescent glass and preparation method thereof |
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|---|---|---|---|
| CN201410038959.4A CN103936281B (en) | 2014-01-26 | 2014-01-26 | A kind of rare earth doped luminescent glass and preparation method thereof |
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ID=51184204
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106458712A (en) * | 2014-08-27 | 2017-02-22 | 施华洛世奇股份有限公司 | Luminescent glass composition |
| CN107010829A (en) * | 2017-04-18 | 2017-08-04 | 哈尔滨工业大学深圳研究生院 | Phosphate novel white-light fluorescent glass of rare earth ion codope and preparation method thereof |
| CN107043209A (en) * | 2017-02-07 | 2017-08-15 | 江西理工大学 | A kind of boron bismuth white light glass for matching blue-light LED chip and preparation method thereof |
| WO2021174353A1 (en) * | 2020-03-03 | 2021-09-10 | Ir Scientific Inc. | Glass composition |
| WO2021179071A1 (en) * | 2020-03-09 | 2021-09-16 | Ir Scientific Inc. | Glass composition |
| CN114230182A (en) * | 2021-12-16 | 2022-03-25 | 桂林电子科技大学 | Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof |
| CN114276012A (en) * | 2020-09-28 | 2022-04-05 | 天津工业大学 | Rare earth element Dy-doped fluoborate luminescent glass and preparation method thereof |
| CN116285982A (en) * | 2023-03-24 | 2023-06-23 | 成都理工大学 | Wavelength-adjustable color-changing luminescent material and preparation method thereof |
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| CN102030472A (en) * | 2009-09-28 | 2011-04-27 | 海洋王照明科技股份有限公司 | Borate luminescent glass and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106458712A (en) * | 2014-08-27 | 2017-02-22 | 施华洛世奇股份有限公司 | Luminescent glass composition |
| CN106458712B (en) * | 2014-08-27 | 2022-03-18 | 施华洛世奇股份有限公司 | Luminescent glass composition |
| CN107043209A (en) * | 2017-02-07 | 2017-08-15 | 江西理工大学 | A kind of boron bismuth white light glass for matching blue-light LED chip and preparation method thereof |
| CN107010829B (en) * | 2017-04-18 | 2019-07-16 | 哈尔滨工业大学深圳研究生院 | The preparation method of the phosphate white fluorescence glass of rare earth ion codope |
| CN107010829A (en) * | 2017-04-18 | 2017-08-04 | 哈尔滨工业大学深圳研究生院 | Phosphate novel white-light fluorescent glass of rare earth ion codope and preparation method thereof |
| WO2021174353A1 (en) * | 2020-03-03 | 2021-09-10 | Ir Scientific Inc. | Glass composition |
| EP4114805A4 (en) * | 2020-03-03 | 2024-03-06 | Ir Scient Inc | Glass composition |
| WO2021179071A1 (en) * | 2020-03-09 | 2021-09-16 | Ir Scientific Inc. | Glass composition |
| CN114276012A (en) * | 2020-09-28 | 2022-04-05 | 天津工业大学 | Rare earth element Dy-doped fluoborate luminescent glass and preparation method thereof |
| CN114276012B (en) * | 2020-09-28 | 2023-12-01 | 天津工业大学 | Rare earth element Dy doped fluoborate luminescent glass and preparation method thereof |
| CN114230182A (en) * | 2021-12-16 | 2022-03-25 | 桂林电子科技大学 | Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof |
| CN114230182B (en) * | 2021-12-16 | 2023-12-01 | 桂林电子科技大学 | Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof |
| CN116285982A (en) * | 2023-03-24 | 2023-06-23 | 成都理工大学 | Wavelength-adjustable color-changing luminescent material and preparation method thereof |
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| CN103936281B (en) | 2016-09-28 |
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