CN103936281B - A kind of rare earth doped luminescent glass and preparation method thereof - Google Patents
A kind of rare earth doped luminescent glass and preparation method thereof Download PDFInfo
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- CN103936281B CN103936281B CN201410038959.4A CN201410038959A CN103936281B CN 103936281 B CN103936281 B CN 103936281B CN 201410038959 A CN201410038959 A CN 201410038959A CN 103936281 B CN103936281 B CN 103936281B
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Abstract
The invention discloses a kind of rare earth doped luminescent glass and preparation method thereof.The glass matrix of this rare earth doped luminescent glass be mainly composed of B2O3、Al2O3、ZnO、CaF2, CaO and Na2O, rare earth ion Tb3+、Sm3+、Eu3+、Dy3+And Tm3+For the centre of luminescence, rare earth ion list is mixed, double-doped or three mix in glass matrix, coordinate UV LED chip to send visible ray；Melt cooling method is used to prepare fluorescent glass.Fluorescent glass disclosed by the invention can be by the ultraviolet excitation of 350 400nm, produce visible ray, by changing glass matrix component, rare earth ion concentration and excitation wavelength, the emission spectrum of fluorescent glass, chromaticity coordinates and colour temperature etc. can be regulated and controled, thus realize the Intelligent luminous of material, meet the different use environment requirements to luminescent properties；Fluorescent glass disclosed by the invention has good luminescent properties, is a kind of novel light-converting material with the highest using value, can be used for LED, poor to solve current LED color stability, the problems such as potting resin is the most aging.
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 resource consumption.The main product of traditional lighting is electric filament lamp and fluorescence
Lamp.The common drawback of both lamps is only sub-fraction electric energy to be transformed into visible ray, and other electric energy are transformed into infrared ray and heat,
Light efficiency is low, the life-span is short, and fluorescent lamp contains hydrargyrum, easily to environment.Light emitting diode (Light emitting
Diode, LED) it is a kind of light emitting semiconductor device converting electrical energy into luminous energy, its light radiation is concentrated mainly on visible region,
Decrease the harm to human body of the non-visible light district electromagnetic wave.Compared with electric filament lamp and fluorescent lamp, LED has energy-conservation, life-span length, ring
The features such as guarantor, low-voltage safety, white light emitting diode (W-LED) has replacement electric filament lamp and the trend of fluorescent lamp, thus becomes
Dominating of 21st century illumination.
Current business-like W-LED illuminating device is mainly by blue light InGaN semiconductor chip and excited by blue light and send Huang
Light or phosphor combination red, green glow form.This LED component has following deficiency: the uniformity of glow color is the most easily-controllable
System；Color rendering index is on the low side；Encapsulating epoxy resin is the most aging；It is easily generated temperature quenching effect, causes in use, partly lead
Body chip and light-emitting phosphor efficiency decline；Manufacturing cost is of a relatively high.The research of LED fluorescent material at present achieves the biggest
Progress, but, either traditional fluorescent material system is optimized, or develops new fluorescent material chemical composition, the most not
The inherent shortcoming of dusty material may be overcome.Rare earth ion doped fluorescent glass can be applicable to LED component, as the centre of luminescence
Rare earth ion can be evenly dispersed in glass, the colourity stay in grade of gained white light；Thermal stability is good, and holds
Easily it is processed into various required form, fluorescent glass can be made suitable shape and directly encapsulate with LED chip, it is not necessary to use epoxy
Resin, thus can make that the manufacturing process of LED illumination device is simple, constant product quality, cost reduce.Rare earth ion doped sends out
Light glass has good physics, chemistry and thermal stability, has prominent advantage for LED field.
Summary of the invention
The technical problem to be solved is open a kind of rare earth doped luminescent glass and preparation method thereof, as
Substitute the candidate material of the LED illumination of fluorescent material, relate generally to rear-earth-doped B2O3-Al2O3-ZnO-CaF2-CaO-Na2O
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 B2O3-Al2O3-ZnO-CaF2-CaO-Na2O system glass is as substrate, dilute
Rare earth ion in earth compounds is as the centre of luminescence, and described rare earth compound includes Eu2O3、Tb4O7、Dy2O3、Sm2O3With
Tm2O3, it is characterised in that: the molar percentage of described each component is: B2O3: 25%-60%, Al2O3: 0%-40%, ZnO:
0%-25%, CaF2: 0%-25%, CaO:0%-45%, Na2O:0%-25%, Eu2O3: 0%-1%, Tb4O7: 0%-
0.5%, Dy2O3: 0%-1%, Sm2O3: 0%-1%, Tm2O3: 0%-1%.
Described rare earth ion list mixes, double-doped or three mix in glass matrix, coordinate UV LED chip to send visible ray.
The above-mentioned rear-earth-doped B that the present invention provides2O3-Al2O3-ZnO-CaF2-CaO-Na2O system fluorescent glass uses molten
Prepared by body cooling method, preparation method comprises the steps:
(1) molar percentage of each component contained by fluorescent glass is determined；
(2) dispensing: select boric acid, aluminium oxide or aluminium hydroxide, zinc oxide, calcium fluoride, calcium carbonate, sodium carbonate as glass
The raw material of substrate；Europium oxide, terbia. Diterbium trioxide, Disamarium trioxide, Dithulium trioxide and dysprosia are as the raw material introducing rare earth ion；According to step
(1) the glass composition various raw material of accurate weighing designed, grinds load weighted raw material 20-40 minute in agate mortar, mixed
Close uniformly, obtain glass batch；
(3) found: glass batch is loaded in corundum or platinum crucible, with the intensification of 2-10 DEG C/min in high temperature furnace
Speed is incubated 1-3 hour after being warming up to 1350-1550 DEG C, obtains vitreous humour；
(4) shape and anneal: vitreous humour is poured in warmed-up stainless steel mould shape, and send in Muffle furnace
400-550 DEG C of annealing 1-2h, cools to room temperature with the furnace, obtains fluorescent glass.
In described shaping and annealing process, stainless steel mould needs to preheat 15-in 300-500 DEG C in Muffle furnace
Use after 40min, to prevent glass rupture.
Preparation method according to above-mentioned rare earth doped luminescent glass prepare with Eu2O3As the raw material of introducing Eu ion, institute
There is Eu in the glass of preparation3+To Eu2+Conversion, this glass is founded in air atmosphere, illustrates that this glass can realize
Eu3+The reduction of ion, it is not necessary to take reducing atmosphere.
The invention has the beneficial effects as follows: the fluorescent glass prepared by the present invention has stable sending out under near ultraviolet excitation
Light, various photochromic can be compounded to form white light.By changing host glass composition, rare earth ion doped kind and concentration, excite
Optical wavelength can change each relative intensity launching band, thus adjusts chromaticity coordinates and colour temperature, thus realizes glass luminescent properties
Regulation and control, are suitable for the different use environment requirements to LED component luminescent properties.The fluorescent glass that the present invention relates to, preparation process
In do not use reducing atmosphere can realize Eu3+To Eu2+Conversion.The present invention technical bottleneck to solution LED illumination, avoids passing
Some inferior positions of system fluorescent material, promote the preparation of related device and practical, significant.
Accompanying drawing explanation
The present invention is further illustrated below in conjunction with the accompanying drawings.
Accompanying drawing 1 is the fluorescent glass of embodiment 1 emission spectrum under 372nm wavelength excites；
Accompanying drawing 2 is the fluorescent glass of embodiment 2 emission spectrum under 372nm wavelength excites；
Accompanying drawing 3 is the fluorescent glass of embodiment 3 emission spectrum under different wave length excites；
Accompanying drawing 4 is the fluorescent glass of embodiment 3 and embodiment 4 emission spectrum under 351nm wavelength excites；
Accompanying drawing 5 is the fluorescent glass of embodiment 5, embodiment 6 and embodiment 7 emission spectrum under 372nm wavelength excites；
Accompanying drawing 6 is under the fluorescent glass of embodiment 6 emission spectrum under 372nm wavelength excites and 544nm wavelength monitor
Excitation spectrum.
Detailed description of the invention
The present invention is further illustrated with specific embodiment below in conjunction with the accompanying drawings, but is not limited to the model of the present invention
Enclose.
Embodiment 1:
(1) design glass molar percentage consists of 60B2O3-20CaF2-10CaO-10Na2O:0.05Eu2O3；
(2) according to the glass composition of design in step (1), boric acid 26.8826g, calcium fluoride 5.6572g, carbon are accurately weighed
These raw materials are fully ground 20min in agate mortar by acid calcium 3.6264g, sodium carbonate 3.8402g and europium oxide 0.0638g,
Glass batch is obtained after mix homogeneously；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1450 DEG C,
Insulation 1h, obtains vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 400 DEG C of preheating 30min and shape, be subsequently placed in Muffle furnace in 450
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 1 is the fluorescent glass of embodiment 1 preparation emission spectrum under 372nm wavelength excites, when preparing this glass
We use Eu2O3Introduce Eu ion, and emission spectrum presents Eu2+And Eu3+The transmitting band of ion, illustrates a part of Eu3+Change into
Eu2+Ion；This glass is founded in air atmosphere, illustrates that this glass can realize Eu3+The reduction of ion, it is not necessary to adopt
Take reducing atmosphere；From emission spectrum it can also be seen that this glass is under ultraviolet excitation, in blue and green light, orange-colored light and HONGGUANG
There is transmitting band in region, and these several transmitting bands are combined and can produce white light；Chromaticity coordinates is (x=0.32, y=0.28), and colour temperature is
6448K (sees attached list 1).
Embodiment 2:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-20CaF2-10CaO-10Na2O:0.05Eu2O3；
(2) according to the glass composition of design in step (1), boric acid 16.4880g, aluminium oxide 9.7105g, fluorine are accurately weighed
Changing calcium 5.9482g, calcium carbonate 3.8130g, sodium carbonate 4.0377g and europium oxide 0.0670g, by these raw materials in agate mortar
It is fully ground 20min, after mix homogeneously, obtains glass batch；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1450 DEG C,
It is incubated 1 h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 400 DEG C of preheating 30min and shape, be subsequently placed in Muffle furnace in 450
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 2 is the glass lower emission spectrum that excites at 372nm ultraviolet light of embodiment 2 preparation, and transmitting band derives from
Eu2+And Eu3+Electron transition, this glass there is also Eu3+To Eu2+Conversion, but transformation efficiency is less than the glass of embodiment 1.
Embodiment 3:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-20CaF2-20CaO:0.05Tm2O3,
0.125Dy2O3；
(2) according to the glass composition of design in step (1), boric acid 16.5069g, aluminium oxide 9.7216g, fluorine are accurately weighed
Change calcium 5.9550g, calcium carbonate 7.6346g, Dithulium trioxide 0.0736g and dysprosia 0.1778g, by these raw materials in agate mortar
It is fully ground 20min, after mix homogeneously, obtains glass batch；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1450 DEG C,
Insulation 1h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 450 DEG C of preheating 30min and shape, be subsequently placed in Muffle furnace in 450
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 3 is the glass of embodiment 3 preparation emission spectrum under 351,358,364 and the exciting of 388nm ultraviolet light,
Emission spectrum comprises indigo plant, yellow emission band, is respectively derived from Tm3+And Dy3+Electron transition, each launch that band is compound can be produced
White light；Different wave length excite under emission spectrum respectively to launch the relative intensity ratio of band different, cause different chromaticity coordinates and colour temperature
(seeing attached list 1).
Embodiment 4:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-20ZnO-20CaF2: 0.05Tm2O3,
0.125Dy2O3；
(2) according to the glass composition of design in step (1), boric acid 17.1071g, aluminium oxide 10.0751g, oxygen are accurately weighed
Change zinc 6.4340g, calcium fluoride 6.1715g, Dithulium trioxide 0.0763g and dysprosia 0.1843g, by these raw materials in agate mortar
It is fully ground 20min, after mix homogeneously, obtains glass batch；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1450 DEG C,
Insulation 1h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 450 DEG C of preheating 30min and shape, be subsequently placed in Muffle furnace in 450
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 4 is the glass of embodiment 4 preparation emission spectrum under 351nm wavelength excites, emission spectrum display blue light
With yellow emission band, white light can be produced, for ease of comparing, the emission spectrum under 351nm wavelength excites of the glass in embodiment 3
Also arrange in figure 4.From accompanying drawing 4 it can be seen that the Tm of the glass of embodiment 43+Luminous intensity is apparently higher than embodiment 3, and this says
Bright can adjust emission spectrum respectively launch the relative intensity of band by changing glass matrix composition, thus adjust fluorescent glass
Chromaticity coordinates and colour temperature.
Embodiment 5:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-40CaO:0.125Dy2O3；
(2) according to the glass composition of design in step (1), boric acid 15.8539g, aluminium oxide 9.3370g, carbon are accurately weighed
These raw materials are fully ground 20min in agate mortar by acid calcium 14.6652g and dysprosia 0.1708g, after mix homogeneously
To glass batch；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1470 DEG C,
Insulation 1h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 470 DEG C of preheating 20min and shape, be subsequently placed in Muffle furnace in 470
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Embodiment 6:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-40CaO:0.125Dy2O3, 0.025Tb4O7；
(2) according to the glass composition of design in step (1), boric acid 15.8539g, aluminium oxide 9.3370g, carbon are accurately weighed
These raw materials are fully ground in agate mortar by acid calcium 14.6652g, dysprosia 0.1708g and terbia. Diterbium trioxide 0.0685g
20min, obtains glass batch after mix homogeneously；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1470 DEG C,
Insulation 1h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 470 DEG C of preheating 20min and shape, be subsequently placed in Muffle furnace in 470
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 6 is under the fluorescent glass of embodiment 6 emission spectrum under 372nm wavelength excites and 544nm wavelength monitor
Excitation spectrum, in the range of wavelength 470-505nm, emission spectrum and excitation spectrum have overlap, illustrate, in this glass, to exist
Dy3+To Tb3+Energy transmission.
Embodiment 7:
(1) design glass molar percentage consists of 35B2O3-25Al2O3-40CaO:0.125Dy2O3, 0.025Tb4O7,
0.05Sm2O3；
(2) according to the glass composition of design in step (1), boric acid 15.8539g, aluminium oxide 9.3370g, carbon are accurately weighed
Acid calcium 14.6652g, dysprosia 0.1708g, terbia. Diterbium trioxide 0.0685g and Disamarium trioxide 0.0639g, by these raw materials at agate mortar
In be fully ground 20min, obtain glass batch after mix homogeneously；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1470 DEG C,
Insulation 1h, obtains uniform vitreous humour；
(4) vitreous humour is poured in the stainless steel mould of 470 DEG C of preheating 20min and shape, be subsequently placed in Muffle furnace in 470
DEG C annealing 2h, cool to room temperature with the furnace and obtain fluorescent glass.
Accompanying drawing 5 is embodiment 5, embodiment 6 and the transmitting under 372nm wavelength excites of the embodiment 7 prepared fluorescent glass
Spectrum, table 1 is colour temperature and the chromaticity coordinates of the fluorescent glass of embodiment 1,3,4,5,6 and 7 preparation.
The glass luminescent properties parameter of table 1 embodiment 1,3,4,5,6 and 7
Each raw material cited by the present invention and the bound value of each raw material, and the bound of each technological parameter takes
Value, can realize the present invention, embodiment numerous to list herein.
Claims (1)
1. rare earth doped luminescent glass and preparation method thereof, it is characterised in that: comprise the steps:
(1) design glass molar percentage consists of 35B2O3 −25Al2O3 −20CaF2 −10CaO −10Na2O:0.05Eu2O3；
(2) according to the glass composition of design in step (1), boric acid 16.4880g, aluminium oxide 9.7105g, calcium fluoride are accurately weighed
5.9482g, calcium carbonate 3.8130 g, sodium carbonate 4.0377 g and europium oxide 0.0670 g, by these raw materials in agate mortar
It is fully ground 20 min, after mix homogeneously, obtains glass batch；
(3) pouring in corundum crucible by glass batch, put in high temperature furnace and melt, fusion temperature is 1450oC, is incubated 1
H, obtains uniform vitreous humour；
(4) vitreous humour is poured into 400oC preheats in the stainless steel mould of 30 min and shapes, and is subsequently placed in Muffle furnace in 450oC
Anneal 2 h, cools to room temperature with the furnace and obtains fluorescent glass.
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| EP2990390A1 (en) * | 2014-08-27 | 2016-03-02 | D. Swarovski KG | 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 |
| EP4114805A4 (en) * | 2020-03-03 | 2024-03-06 | Ir Scient Inc | Glass composition |
| US20230150864A1 (en) * | 2020-03-09 | 2023-05-18 | Ir Scientific Inc. | Glass composition |
| 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 |
| 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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| NL8501107A (en) * | 1985-04-16 | 1986-11-17 | Philips Nv | LUMINESCENT ALUMINO BORATE AND / OR ALUMINOSILICATE GLASS AND LUMINESCENT SCREEN EQUIPPED WITH SUCH A GLASS. |
| CN1211305C (en) * | 2001-06-14 | 2005-07-20 | 湖南师范大学 | Agricultural double-energy light-converting glass and its making process and usage |
| CN102030472B (en) * | 2009-09-28 | 2012-09-05 | 海洋王照明科技股份有限公司 | Borate luminescent glass and preparation method thereof |
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