CN101928111A - Luminescent glass, making method and application thereof - Google Patents
Luminescent glass, making method and application thereof Download PDFInfo
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- CN101928111A CN101928111A CN200910108140XA CN200910108140A CN101928111A CN 101928111 A CN101928111 A CN 101928111A CN 200910108140X A CN200910108140X A CN 200910108140XA CN 200910108140 A CN200910108140 A CN 200910108140A CN 101928111 A CN101928111 A CN 101928111A
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Abstract
The invention provides luminescent glass, a making method and application thereof. The making method comprises the following steps of, firstly, dissolving organic fluorescence materials in a solvent to form an organic fluorescence material solution; secondly, immersing porous glass into the organic fluorescence material solution, and absorbing the organic fluorescence material solution; and thirdly, taking out the porous glass immersed with the organic fluorescence material solution, and drying to prepare the luminescent glass. The luminescent glass is prepared by the method and can be matched with a semiconductor light emitting diode within a range of 200-550 nm to make a light emitting device. The making method of the luminescent glass has simple making technology, and the luminescent glass prepared by the method can be directly applied to the light emitting device of the semiconductor light emitting diode as fluorescence conversion substances and packaging materials, thereby solving the problem of photochemical reaction between the organic fluorescence materials and the organic packaging materials.
Description
Technical field
The present invention relates to luminous and technique of display field, fluorescent glass of be specifically related to a kind of manufacture method of fluorescent glass, making by this method and uses thereof.
Background technology
Along with the development of semiconductor lighting technology (LED), this revolutionary new light sources has been come into our daily life gradually.As semiconductor illuminating light source, current consumption only is 1/10 of ordinary incandescent lamp under equal brightness with third generation semiconductor material gan, and the life-span can reach more than 100,000 hours.As novel lighting engineering, plurality of advantages such as that LED has is energy-conservation, environmental protection, applying flexible can be widely used in fields such as various indications, demonstration, decoration, backlight and general lighting, and this will cause the revolution of a lighting field.
At present, the making approach of white light LEDs generally adopts fluorescent material that the part blue light of blue-light LED chip is converted to red, green or gold-tinted, realizes by different colours light blended method.Wherein, used fluorescent material mostly is some inorganic fluorescent materials, as rare earth doped alkali metalsulphide, aluminate etc., but problems such as most inorganic fluorescent material exists, and excitation wavelength and led chip do not match, light conversion efficiency and brightness are lower have influenced the light output character and the efficient of whole luminescent device.Compare with phosphor, organic luminescent substance has the tunable wave length scope of broad, strong light absorpting ability, low excitation energy and high incomparable advantages such as conversion quantum efficiency.The technology of packaged material has now appearred organic fluorescence materials is mixed, as in Resins, epoxy, polymethylmethacrylate and the plastics as the light converting member, be made into white light LEDs.But easily with between the organic packaged material photochemical reaction takes place, so cause defectives such as device deterioration, work-ing life weak point, luminosity instability easily owing to be in the organic fluorescence materials of excited state.So, the someone proposes organic fluorescence materials is doped to and utilizes sol-gel method to make the generation that the organic/inorganic composite luminescent material is avoided above-mentioned phenomenon in the silica matrix again, but, in this method, the concentration of organic fluorescence materials, the pH value of reaction system, the ratio of water and tetraethoxy, parameters such as the temperature of reaction of system and reaction times have bigger influence to the performance of the organic/inorganic composite material of final acquisition, and because prepared material still is a powder body material, so also must cooperate just and can in LED, use with organic packaged material, therefore from the material preparation to the device package, whole technological process is comparatively complicated.
Summary of the invention
First purpose of the embodiment of the invention is to provide a kind of manufacture method of fluorescent glass, be intended to solve organic fluorescence materials is applied in the semiconductor lighting technology, photochemical reaction between luminous organic material that exists and the organic packaged material, and the problem of complex manufacturing technology.
Second purpose of the embodiment of the invention is to provide a kind of fluorescent glass by method for preparing.
The 3rd purpose of the embodiment of the invention is to provide a kind of purposes of above-mentioned fluorescent glass.
The manufacture method of the fluorescent glass of the embodiment of the invention comprises the steps:
(1) organic fluorescence materials is dissolved in the solvent, forms organic fluorescence materials solution;
(2) sintered glass is immersed in the organic fluorescence materials solution, absorbs organic fluorescence materials solution;
(3) sintered glass that will be soaked with organic fluorescence materials takes out after drying, makes fluorescent glass.
The fluorescent glass of the embodiment of the invention is prepared from by above-mentioned manufacture method.
The fluorescent glass of the embodiment of the invention is used to cooperate the semiconductor light-emitting-diode in 200nm～550nm scope to make light-emitting device.
Compared with prior art, technique scheme is owing to be carrier with the sintered glass, by soaking the formulations prepared from solutions fluorescent glass of finite concentration organic fluorescence materials, this method not only technological process is very simple, and this fluorescent glass can directly be applied in the luminescent device of based semiconductor photodiode as fluorescence transformational substance and packaged material, has solved the difficulty that in the past organic fluorescence materials is used for the semiconductor lighting technology.In addition, the technical program, the organic fluorescence materials range of choice is wide, be convenient to regulate performance of composites, simultaneously, because sintered glass has strong unreactiveness, organic fluorescence materials and its interaction have been avoided and the non-radiative energy transfer that causes, in the quantum yield that has improved organic fluorescence materials, also improved the stability of this fluorescent glass integral body.Once more, the porous fluorescent glass that contains organic fluorescence materials of the present invention's preparation has high transparency, and because the tunable wave length wide ranges of organic fluorescence materials, selectable kind is many, therefore can cooperate the semiconductor light-emitting-diode in 200nm～550nm scope to be made into the light-emitting device that different colours is launched.Because organic fluorescence materials has strong light absorpting ability and high conversion quantum efficiency, this porous fluorescent glass of the present invention's preparation also has high light efficiency, has broad application prospects at semiconductor lighting and demonstration field.
Description of drawings
Fig. 1 is the excitation spectrum and the emmission spectrum of the porous fluorescent glass of embodiment 1 preparation;
Fig. 2 is the emmission spectrum of porous fluorescent glass under 485nm wavelength excitation of embodiment 2 preparations.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The embodiment of the invention provides a kind of method for preparing fluorescent glass in the glass medium that organic fluorescence materials is attached to, manufacture craft is simple, and the fluorescent glass of this method preparation can directly be applied in the luminescent device of based semiconductor photodiode as fluorescence transformational substance and packaged material.
Particularly, the manufacture method of embodiment of the invention fluorescent glass comprises the steps:
(1) organic fluorescence materials is dissolved in the solvent, forms organic fluorescence materials solution;
(2) sintered glass is immersed in the organic fluorescence materials solution, absorbs organic fluorescence materials solution;
(3) sintered glass that will be soaked with organic fluorescence materials takes out after drying, makes fluorescent glass.
In embodiments of the present invention, there is no particular restriction for the solvent that organic fluorescence materials adopted, and is selected from this area institute common solvent, for example can be selected from ethanol, methyl alcohol, chloroform, acetone, ether, normal hexane, hexanaphthene, tetrahydrofuran (THF) or benzene.
Generally speaking, there is no particular restriction for the concentration of organic fluorescence materials in solution, as long as can fully dissolve organic fluorescence materials.In embodiments of the present invention, the concentration range of organic fluorescence materials in solution is preferably 10
-6～10
-1Mol/L; Sintered glass dipping time in organic fluorescence materials solution is half an hour at least.
There is no particular restriction for the organic fluorescence materials of the embodiment of the invention, the organic fluorescence materials of using always for this area.For example, can be selected from one or more materials in coumarin kind compound, rhodamine compounds, compound of fluorene class, stilbene compound, azo compound, fluoresceins compound, aromatic fused ring compound, a metal-organic complex.
Above-mentioned coumarin kind compound, rhodamine compounds, compound of fluorene class, stilbene compound, azo compound, fluoresceins compound, aromatic fused ring compound, there is no particular restriction for a metal-organic complex, is this area organic fluorescence materials commonly used.For example:
Coumarin kind compound can be selected from tonka bean camphor 307 (Acros company), coumarin 6, tonka bean camphor 153, tonka bean camphor 343, tonka bean camphor 152, tonka bean camphor 153, tonka bean camphor 7, tonka bean camphor 334, tonka bean camphor 314, tonka bean camphor 102,7-ethoxy coumarin, 7-diethylin-3-(2-benzoglyoxaline) tonka bean camphor, 7-hydroxyl-4-trifluoromethyl tonka bean camphor, 7-diethyl amido-4-methylcoumarin etc.
The rhodamine compounds can be selected from rhodamine 6G (Acros company), rhodamine 123, rhodamine B, rhodamine 110 etc.
Compound of fluorene class can be selected from 9, two (4-aminophenyl) fluorenes (Acros company), 2 of 9-, 7-nitrofluorene, 9, two (4-aminophenyl) fluorenes, 9 of 9-, two (4-hydroxyphenyl) fluorenes, 9 of 9-, two (4-amino-3-aminomethyl phenyl) fluorenes, 9 of 9-, two (4-amino-3-fluorophenyl) fluorenes of 9-etc.
Stilbene compound can be selected from Pterostilene (Aldrich company), to two o-methyl styrene base benzene, 1,1 ' '-two (diphenylamino) styryl benzene etc.
Azo compound can be selected from dimethyl yellow (Aldrich company), 4,4 '-chrysoidine, 4-(dimethyl amine)-4 '-methyl-benzene, DISPERSE ORANGE 30 200 3 etc.
The plain sodium (Shanghai traditional Chinese medicines group company) of the optional autofluorescence of fluoresceins compound, fluorescent yellow, diacetic acid fluorescein, the amino fluorescein, 2 of 5-', 7 '-dichlorofluorescein, fluorescein diacetate, tetraiodofluorescein, 6-Fluoresceincarboxylic acid, 4 ', 5 '-dibromofluorescein etc.
Aromatic fused ring compound can be selected from rubrene (Acros company), coronene, perylene, anthracene, benzanthrene etc.
A metal-organic complex can be selected from three (oxine) aluminium (Aldrich company), (oxine) zinc, (8-ethyl porphyrin) platinum (Frontiers company), single (1, the 10-phenanthrolene) europium (Aldrich company) of three (phenyl phenacyl ketones), three (2-phenyl pyrimidine) iridium (Aldrich company) etc.
Wherein, preferred one or more materials in the organic coordination compound of the organic coordination compound of d district transition element, lanthanon and Al of above-mentioned a metal-organic complex.Be central metal ion beta-diketon class, fragrant ketone, heterocyclic binary or multicomponent complex with Eu, Sm, Tb, Dy, Pt, Ir, Ru, Os, Al, Zn, Cu or Ni certainly more preferably.
In embodiments of the present invention, there is no particular restriction for sintered glass, is this area sintered glass commonly used, and the volume in hole accounts for 25～40% of fluorescent glass cumulative volume, and pore size is 4～100nm, for example, can select the Vycor of Corning Incorporated series sintered glass.
Sintered glass contains the SiO of 94.0%～98wt% in embodiments of the present invention
2, the B of 1.0～3.0wt%
2O
3, 1.0～3.0wt%Al
2O
3Sintered glass, can also contain other composition certainly, for example 0～1% Na
2O, 0～1% ZrO
2
It is a kind of by the above-mentioned fluorescent glass of stating the manufacture method preparation that the present invention also provides, this fluorescent glass can cooperate the semiconductor light-emitting-diode in 200nm～550nm scope, be made into the light-emitting device of different colours emission, can thoroughly solve the photochemical reaction problem between luminous organic material and the organic packaged material, and preparation technology is simple.
Pore size is 4～100nm in the sintered glass of selecting for use in following examples, repeats no more.
Embodiment 1
Get coumarin kind compound tonka bean camphor 307 (Acros company) 0.1mmol, be dissolved in the ethanolic soln of 10ml, be mixed with 10
-2The solution of mol/L, 25% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 8 hours, with carrying out drying after the ethanolic soln clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.Excitation spectrum and the emmission spectrum of the porous fluorescent glass of present embodiment preparation are seen Fig. 1, from Fig. 1 we as can be seen, the suitable 450nm blue-ray LED of this material excites, and can launch the green glow of 500nm.
Embodiment 2
Get rhodamine compounds rhodamine 6G (Acros company) 0.01mmol, be dissolved in the ethanolic soln of 100ml, be mixed with 10
-4The solution of mol/L, 25% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 8 hours, with carrying out drying after the ethanolic soln clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.The porous fluorescent glass that Fig. 2 has provided the present embodiment preparation is a emmission spectrum under the 485nm excitation at wavelength, can launch the gold-tinted of 565nm under the exciting of the light of 485nm wavelength.This test adopts Tianjin, island RF-5301PC spectrophotofluorometer to carry out under 1.5nm slit, muting sensitivity condition.
Embodiment 3
Get compound of fluorene class 9, two (4-aminophenyl) fluorenes (Acros company) 0.1mmol of 9-are dissolved in the chloroformic solution of 100ml, are mixed with 10
-3The solution of mol/L, 40% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 8 hours, with carrying out drying after the chloroformic solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 4
Get stilbene compound Pterostilene (Aldrich company) 0.01mmol, be dissolved in the methanol solution of 1000ml, be mixed with 10
-5The solution of mol/L, 36% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 8 hours, with carrying out drying after the methanol solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Get azo compound dimethyl yellow (Aldrich company) 0.01mmol, be dissolved in the chloroformic solution of 1000ml, be mixed with 10
-5The solution of mol/L, 40% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 5 hours, with carrying out drying after the chloroformic solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 6
Get fluoresceins compound uranine (Shanghai traditional Chinese medicines group company) 0.01mmol, be dissolved in the acetone of 1000ml, be mixed with 10
-5The solution of mol/L, 25% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 10 hours, with carrying out drying after the acetone soln clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 7
Get aromatic fused ring compound rubrene (Acros company) 0.001mmol, be dissolved in the tetrahydrofuran solution of 1000ml, be mixed with 10
-6The solution of mol/L, 25% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 8 hours, with carrying out drying after the tetrahydrofuran solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 8
Get metal complexes three (oxine) aluminium (Aldrich company) 0.01mmol, be dissolved in the hexane solution of 100ml, be mixed with 10
-4The solution of mol/L, 35% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 3 hours, with carrying out drying after the hexane solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 9
Get metal complexes (oxine) zinc (Aldrich company) 0.01mmol, be dissolved in the diethyl ether solution of 100ml, be mixed with 10
-4The solution of mol/L, 35% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 5 hours, with carrying out drying after the diethyl ether solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Get metal complexes (8-ethyl porphyrin) platinum (Frontiers company) 0.01mmol, be dissolved in the cyclohexane solution of 100ml, be mixed with 10
-4The solution of mol/L, 22% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 9 hours, with carrying out drying after the cyclohexane solution clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 11
Get single (1, the 10-phenanthrolene) europium (Aldrich company) 0.01mmol of metal complexes three (phenyl phenacyl ketone), be dissolved in the benzole soln of 100ml, be mixed with 10
-4The solution of mol/L, 31% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 6 hours, with carrying out drying after the benzole soln clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
Embodiment 12
Get metal complexes three (2-phenyl pyrimidine) iridium (Aldrich company) 0.01mmol, be dissolved in the ethanolic soln of 100ml, be mixed with 10
-4The solution of mol/L, 30% the sintered glass that the volume in hole is accounted for the fluorescent glass cumulative volume is immersed in the above-mentioned solution and takes out after 7 hours, with carrying out drying after the ethanolic soln clean surface, can obtain containing the porous fluorescent glass of organic fluorescence materials.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the manufacture method of a fluorescent glass is characterized in that, it comprises the steps:
(1) organic fluorescence materials is dissolved in the solvent, forms organic fluorescence materials solution;
(2) sintered glass is immersed in the described organic fluorescence materials solution, absorbs organic fluorescence materials solution;
(3) sintered glass that will be soaked with organic fluorescence materials takes out after drying, makes described fluorescent glass.
2. the manufacture method of fluorescent glass according to claim 1 is characterized in that the concentration of described organic fluorescence materials solution is 10
-6～10
-1Mol/L, the dipping time of described sintered glass in this organic fluorescence materials solution is half an hour at least.
3. the manufacture method of fluorescent glass according to claim 1, it is characterized in that described organic fluorescence materials is selected from one or more materials in coumarin kind compound, rhodamine compounds, compound of fluorene class, stilbene compound, azo compound, fluoresceins compound, aromatic fused ring compound, a metal-organic complex.
4. as the manufacture method of fluorescent glass as described in the claim 3, it is characterized in that described a metal-organic complex is selected from one or more materials in the organic coordination compound of the organic coordination compound of d district transition element, lanthanon and Al.
5. as the manufacture method of fluorescent glass as described in the claim 4, it is characterized in that it is central metal ion beta-diketon class, fragrant ketone, heterocyclic binary or multicomponent complex that described a metal-organic complex is selected from Eu, Sm, Tb, Dy, Pt, Ir, Ru, Os, Al, Zn, Cu or Ni.
6. the manufacture method of fluorescent glass according to claim 1 is characterized in that solvent is selected from ethanol, methyl alcohol, chloroform, acetone, ether, normal hexane, hexanaphthene, tetrahydrofuran (THF) or benzene in the described organic fluorescence materials solution.
7. the manufacture method of fluorescent glass according to claim 1 is characterized in that described sintered glass pore size is 4～100nm, and the volume in hole accounts for 25～40% of described fluorescent glass cumulative volume.
8. as the manufacture method of fluorescent glass as described in the claim 7, it is characterized in that described sintered glass contains 94.0%～98wt%SiO
2, 1.0～3.0wt%B
2O
3, 1.0～3.0wt%Al
2O
3, 0～1%Na
2O, 0～1%ZrO
2
9. one kind is passed through the fluorescent glass that each described manufacture method of claim 1～8 prepares.
10. one kind is used to cooperate the semiconductor light-emitting-diode in 200nm～550nm scope to make light-emitting device as fluorescent glass as described in the claim 9.
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|---|---|---|---|
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| CN101928111B CN101928111B (en) | 2012-04-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271735A (en) * | 2015-10-29 | 2016-01-27 | 严梅霞 | High-silica glass capable of emitting red light and preparation method thereof |
| CN105271729A (en) * | 2015-10-29 | 2016-01-27 | 严梅霞 | Red light emitting glass and manufacturing method for red light emitting glass |
| CN111003937A (en) * | 2019-12-17 | 2020-04-14 | 上海应用技术大学 | Noctilucent glass bracelet and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190082A (en) * | 1997-02-01 | 1998-08-12 | 中国科学院长春光学精密机械研究所 | Preparation of ultrafast response non-linear optical glass |
| EP1566367B1 (en) * | 2002-11-29 | 2015-01-07 | Japan Science and Technology Agency | Luminescent glass |
| CN100484896C (en) * | 2005-07-15 | 2009-05-06 | 中国科学院上海光学精密机械研究所 | Method for producing green-emitting high-silica glass |
| CN1944297A (en) * | 2006-10-24 | 2007-04-11 | 中国科学院上海光学精密机械研究所 | Method for manufacturing neodymium-ytterbium co-doped high silica laser glass |
| CN101154036A (en) * | 2007-09-06 | 2008-04-02 | 北京科技大学 | Method for controlling glass etching depth with optical-controlling method |
| CN101215093B (en) * | 2007-12-26 | 2010-06-09 | 中国科学院上海光学精密机械研究所 | Method for manufacturing integrated color luminous high silica glass |
-
2009
- 2009-06-26 CN CN200910108140XA patent/CN101928111B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271735A (en) * | 2015-10-29 | 2016-01-27 | 严梅霞 | High-silica glass capable of emitting red light and preparation method thereof |
| CN105271729A (en) * | 2015-10-29 | 2016-01-27 | 严梅霞 | Red light emitting glass and manufacturing method for red light emitting glass |
| CN105271729B (en) * | 2015-10-29 | 2017-12-26 | 严梅霞 | A kind of red light emitting glass and its manufacture method |
| CN105271735B (en) * | 2015-10-29 | 2017-12-26 | 严梅霞 | A kind of high silica red light emitting glass and its manufacture method |
| CN111003937A (en) * | 2019-12-17 | 2020-04-14 | 上海应用技术大学 | Noctilucent glass bracelet and preparation method thereof |
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|---|---|
| CN101928111B (en) | 2012-04-25 |
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