CN109516694B - Fluorescent glass, preparation method thereof and light-emitting device - Google Patents
Fluorescent glass, preparation method thereof and light-emitting device Download PDFInfo
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- CN109516694B CN109516694B CN201811320403.9A CN201811320403A CN109516694B CN 109516694 B CN109516694 B CN 109516694B CN 201811320403 A CN201811320403 A CN 201811320403A CN 109516694 B CN109516694 B CN 109516694B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21K—NON-ELECTRIC LIGHT SOURCES USING LUMINESCENCE; LIGHT SOURCES USING ELECTROCHEMILUMINESCENCE; LIGHT SOURCES USING CHARGES OF COMBUSTIBLE MATERIAL; LIGHT SOURCES USING SEMICONDUCTOR DEVICES AS LIGHT-GENERATING ELEMENTS; LIGHT SOURCES NOT OTHERWISE PROVIDED FOR
- F21K9/00—Light sources using semiconductor devices as light-generating elements, e.g. using light-emitting diodes [LED] or lasers
- F21K9/20—Light sources comprising attachment means
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/04—Particles; Flakes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
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- Optics & Photonics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- Glass Compositions (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses fluorescent glass and a preparation method thereof, wherein the fluorescent glass comprises a glass substrate and fluorescent powder, and the fluorescent powder is dispersed in the glass substrate; the components of the glass matrix include: alumina, silica, boron oxide and flux. Through the mode, the fluorescent glass has the characteristics of high temperature resistance, ageing resistance, uniform light emission, high light-emitting efficiency and long service life, and can be applied to manufacturing of light-emitting devices, so that the light-emitting devices containing the fluorescent glass have high light-emitting efficiency and long service life.
Description
Technical Field
The invention relates to the technical field of fluorescent materials, in particular to fluorescent glass, a preparation method thereof and a light-emitting device.
Background
At present, "green lighting" has become one of the important signs of the modernization degree of the human society, and is an important measure related to the sustainable development of the human society. Research and development of Light Emitting Diode (LED) lighting has been the most focused focus in recent years. White light LEDs (W-LEDs) have become the most promising light source in the 21 st century due to a series of advantages of energy saving, environmental protection, long service life, high luminous efficiency, etc., and will replace incandescent lamps and fluorescent lamps to become the third generation illumination light source.
For white LED packages, the phosphor powder functions to form white light by color recombination. The common fluorescent powder is used by mixing fluorescent powder with packaging adhesive (epoxy resin or silica gel) and then coating the mixture on an LED chip to form a fluorescent powder adhesive layer; because the fluorescent powder glue layer is prepared by epoxy resin or silica gel and fluorescent powder, the heat resistance and ageing resistance of the fluorescent powder glue layer are poor, and when the LED works for a long time under the drive of current, the temperature of a chip is increased, so that the packaging glue is easily carbonized and yellowed, and the luminous efficiency and the service life of an LED device are influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides fluorescent glass, a preparation method thereof and a light-emitting device.
The technical scheme adopted by the invention is as follows: the fluorescent glass comprises a glass matrix and fluorescent powder, wherein the fluorescent powder is dispersed in the glass matrix; the components of the glass matrix include: alumina (Na)2O), silicon oxide (SiO)2) Boron oxide (B)2O3) And a flux.
Preferably, the molar ratio of the alumina, the silicon oxide, the boron oxide and the fluxing agent is (0.1-0.3): (2-2.5): (0.2-0.6): (0.1 to 0.5); preferably, the molar mass ratio of the alumina, the silica, the boron oxide and the fluxing agent is 0.2: 2.2: 0.5: 0.3.
preferably, the flux comprises sodium oxide (Na)2O) and potassium oxide (K)2O). If the fluxing agent only adopts sodium oxide, the melting temperature in the manufacturing process is about 1500 ℃, and if the fluxing agent only adopts potassium oxide, the melting temperature in the manufacturing process is about 1300 ℃; if the fluxing agent adopts the combination of potassium oxide and potassium oxide, the melting temperature can be reduced to about 1000 ℃; therefore, the fluxing agent preferably adopts the combination of sodium oxide and potassium oxide to reduce the melting point of the glass matrix component during the production of the fluorescent glass product, namely the melting temperature in the manufacturing process.
Preferably, the components of the glass matrix further include magnesium oxide (MgO). The addition of the magnesium oxide can improve the mechanical strength of the fluorescent glass, strengthen the hardness of the fluorescent glass and improve the heat dissipation of the product.
Preferably, the components of the glass matrix further include at least one of zinc oxide (ZnO), calcium oxide (CaO), lead oxide (PbO). By adding at least one component raw material of zinc oxide, calcium oxide and lead oxide, the refractive index of the fluorescent glass product can be improved, and the luminous brightness of the fluorescent glass can be enhanced. The refractive index is about 1.4 when lead oxide is not added, the refractive index is about 1.6 when lead oxide is added, and the components of the glass matrix preferably comprise zinc oxide, calcium oxide and lead oxide.
Preferably, the components of the glass matrix include: the flux is sodium oxide and potassium oxide.
Preferably, the molar ratio of the aluminum oxide, the silicon oxide, the boron oxide, the sodium oxide, the potassium oxide, the magnesium oxide, the zinc oxide, the calcium oxide and the lead oxide is (0.1-0.3): (2-2.5): (0.2-0.6): (0.1-0.3): (0.02-0.1): (0.01-0.05): (0.2-0.3): (0.2-0.3): (0.1-0.2). Through the mutual matching of the components and the fluorescent powder, the finished fluorescent glass has good glossiness, high luminous efficiency, good thermal stability and strong aging resistance. Further preferably, the molar ratio of the aluminum oxide, the silicon oxide, the boron oxide, the sodium oxide, the potassium oxide, the magnesium oxide, the zinc oxide, the calcium oxide and the lead oxide is 0.2: 2.2: 0.5: 0.3: 0.05: 0.03: 0.2: 0.3: 0.2.
preferably, the phosphor is selected from CaAlSiN3:Eu、K3SiF6:Mn4+、(CaSrBa)2SiO4、Y3Al5O12:Ce3+、Y3Al5O12:Ce3+(Ga)、Lu3Al5O12:Ce3+At least one of (1). The specific addition type, proportion and addition amount of the fluorescent powder can be added according to factors such as the display index of actual requirements and the like.
The invention also provides a preparation method of the more than one fluorescent glass, which comprises the following steps: the components of the glass matrix and the fluorescent powder are uniformly mixed and heated until the components of the glass matrix are melted, and then the mixture is cooled to be solidified. Specifically, mixing the components of the glass matrix and the fluorescent powder for about 48 hours until the raw materials are fully mixed; putting the glass into a clean crucible container, heating to 1000-1500 ℃ for melting, and melting all components of the glass matrix; and then cooled until solidified.
The fluorescent glass prepared by the method can be applied to the preparation of a light-emitting device. Therefore, the invention also provides a light-emitting device which comprises an excitation light source and any one of the above fluorescent glasses. The excitation light source can be a light-emitting diode, a laser diode or a combination thereof; the excitation light source is preferably an excitation light source emitting blue light. The light emitting device includes, but is not limited to, various lighting devices, laser projectors, laser televisions, and the like.
The beneficial technical effects of the invention are as follows: the invention provides fluorescent glass, a preparation method thereof and a light-emitting device, wherein the fluorescent glass has the advantages of high temperature resistance, good aging resistance, uniform light emission, high light-emitting efficiency and long service life, can be applied to the preparation of the light-emitting device, and can ensure that the light-emitting device containing the fluorescent glass has high light-emitting efficiency and long service life.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
The fluorescent glass comprises a glass substrate and fluorescent powder which is Lu3Al5O12:Ce3+And CaAlSiN3Eu; the components of the glass matrix include: alumina, silicon oxide, boron oxide, a fluxing agent, magnesium oxide, zinc oxide, calcium oxide and lead oxide, wherein the fluxing agent is specifically selected from sodium oxide and potassium oxide; and the molar ratio of aluminum oxide, silicon oxide, boron oxide, sodium oxide, potassium oxide, magnesium oxide, zinc oxide, calcium oxide and lead oxide is 0.2: 2.2: 0.5: 0.3: 0.05: 0.03: 0.2: 0.3: 0.2.
the preparation method comprises the following steps: taking the components of the glass matrix according to the molar ratio, and taking the glass matrix and the fluorescent powder Y3Al5O12:Ce3+And CaAlSiN3Eu, mixing the raw materials for 48 hours to fully mix the raw materials; then putting the glass into a clean crucible container, heating the glass to about 1000 ℃ for melting, so that all components of the glass matrix are melted and the fluorescent powder is not melted; and then cooling to solidify to obtain the fluorescent glass.
Comparative example 1: silica gel is used to replace the glass substrate in the embodiment 1 and is mixed with the fluorescent powder to prepare the fluorescent film adhesive.
The fluorescent glass of example 1 and the fluorescent film adhesive of comparative example 1 were subjected to aging test tests, respectively, and the results are shown in table 1 below.
TABLE 1 data statistics of aging test results for example 1 fluorescent glass and comparative example 1 fluorescent film adhesive
As can be seen from table 1 above, the luminous flux of the fluorescent glass in example 1 is greater than that of the fluorescent film adhesive in comparative example 1. In addition, the fluorescent glass in the embodiment 1 is subjected to an aging test at a high temperature of 100 ℃, and the luminous flux of the fluorescent glass gradually increases and then gradually decreases along with the increase of aging time; the maintenance rate is gradually increased and then slowly reduced along with the increase of the aging time; this is because the energy of the phosphor in the fluorescent glass of example 1 is continuously excited under high temperature conditions, and the luminous flux and the maintenance rate of the fluorescent glass initially increase gradually with the aging time. The fluorescent film adhesive in the comparative example 1 is subjected to aging test at a high temperature of 85 ℃, and the luminous flux and the maintenance rate of the fluorescent film adhesive are continuously reduced along with the increase of the aging time, because the fluorescent film adhesive is in a high-temperature environment for a long time, the efficiency of the fluorescent film adhesive is gradually reduced along with the increase of the high-temperature time, and the aging and yellowing of the fluorescent film adhesive are accelerated at a higher temperature. As can be seen from the above, the fluorescent glass in example 1 has high thermal stability, high temperature resistance, aging resistance, high luminous efficiency, and long service life.
Example 2
The present embodiment differs from embodiment 1 in that: the phosphor is Y3Al5O12:Ce3+And K3SiF6:Mn4+A combination of (1); the components of the glass matrix are as follows: aluminum oxide, silicon oxide, boron oxide, sodium oxide, potassium oxide, magnesium oxide, zinc oxide, calcium oxide, and lead oxide in a molar ratio of 0.1: 2.5: 0.6: 0.2: 0.02: 0.01: 0.25: 0.23: 0.1; the specific preparation method is the same as that of example 1.
Example 3
The present embodiment differs from embodiment 1 in that: the fluorescent powder is (CaSrBa)2SiO4(ii) a The components of the glass matrix are as follows: aluminum oxide, silicon oxide, boron oxide, sodium oxide, potassium oxide, magnesium oxide, zinc oxide, calcium oxide, and lead oxide in a molar ratio of 0.3: 2: 0.2: 0.1: 0.07: 0.05:0.3: 0.2: 0.15; the specific preparation method is the same as that of example 1.
Example 4
The present embodiment differs from embodiment 1 in that: the phosphor is Y3Al5O12:Ce3+And CaAlSiN3Eu; the components of the glass matrix include: alumina, silicon oxide, boron oxide, a fluxing agent, magnesium oxide and lead oxide, wherein the fluxing agent is specifically selected from sodium oxide and potassium oxide; and the molar ratio of alumina, silica, boron oxide, sodium oxide, potassium oxide, magnesium oxide and lead oxide is 0.18: 2.4: 0.4: 0.15: 0.1: 0.02: 0.2; the specific preparation method is the same as that of example 1.
Example 5
The present embodiment differs from embodiment 1 in that: the fluorescent powder is Lu3Al5O12:Ce3+And Y3Al5O12:Ce3+(ii) a The components of the glass matrix include: alumina, silicon oxide, boron oxide and a fluxing agent, wherein the fluxing agent is specifically selected from sodium oxide and potassium oxide; and the mol ratio of alumina, silicon oxide, boron oxide, sodium oxide and potassium oxide is 0.2: 2.2: 0.5: 0.2: 0.1; the specific preparation method is the same as that of example 1.
Example 6
The present embodiment differs from embodiment 1 in that: the fluorescent powder is Lu3Al5O12:Ce3+(ii) a The components of the glass matrix include: alumina, silicon oxide, boron oxide, a fluxing agent and magnesium oxide, wherein the fluxing agent is sodium oxide; and the molar ratio of alumina, silica, boron oxide, sodium oxide and magnesium oxide is 0.15: 2.3: 0.3: 0.3: 0.04; the preparation method is similar to that of the embodiment 1, and the melting temperature is controlled to be about 1300 ℃ in the embodiment.
Example 7
The present embodiment differs from embodiment 1 in that: the phosphor is K3SiF6:Mn4+And (CaSrBa)2SiO4(ii) a The components of the glass matrix include: alumina, silicon oxide, boron oxide, a fluxing agent, zinc oxide and calcium oxide, wherein the fluxing agent is potassium oxide; and alumina, oxidationThe mol ratio of silicon to boron oxide to potassium oxide to zinc oxide to calcium oxide is 0.25: 2.1: 0.4: 0.08: 0.25: 0.2; the preparation method is similar to that of the embodiment 1, and the melting temperature is controlled to be about 1500 ℃ in the embodiment.
The fluorescent glass prepared in the above examples 1 to 7 has high temperature resistance, good aging resistance, high luminous efficiency and long service life, and can be applied to various light-emitting devices, such as various lighting devices, laser projectors, laser televisions and the like. Such light emitting devices typically include an excitation light source, which may be a light emitting diode, a laser diode, or a combination thereof, and any of the above fluorescent glasses, and the laser light source is typically selected to emit blue light. And the appropriate fluorescent glass can be selected according to specific needs, so that the light can be converted into the required light by the cooperation of the excitation light source and the fluorescent glass.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The fluorescent glass is characterized in that raw materials comprise a glass matrix and fluorescent powder, and the fluorescent powder is dispersed in the glass matrix; the components of the glass matrix comprise aluminum oxide, silicon oxide, boron oxide, fluxing agent, magnesium oxide, zinc oxide, calcium oxide and lead oxide, wherein the fluxing agent is sodium oxide and potassium oxide;
the molar ratio of the aluminum oxide to the silicon oxide to the boron oxide to the sodium oxide to the potassium oxide to the magnesium oxide to the zinc oxide to the calcium oxide to the lead oxide is (0.1-0.3): (2-2.5): (0.2-0.6): (0.1-0.3): (0.02-0.1): (0.01-0.05): (0.2-0.3): (0.2-0.3): (0.1-0.2).
2. The fluorescent glass of claim 1, wherein the phosphor is selected from CaAlSiN3:Eu、K3SiF6:Mn4+、Y3Al5O12:Ce3+、Lu3Al5O12:Ce3+At least one of (1).
3. The method for producing a fluorescent glass according to claim 1 or 2, characterized by comprising the steps of: the components of the glass matrix and the fluorescent powder are uniformly mixed and heated until the components of the glass matrix are melted, and then the mixture is cooled to be solidified.
4. A light-emitting device comprising an excitation light source and the fluorescent glass according to claim 1 or 2.
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| CN113620600B (en) * | 2021-07-21 | 2023-11-03 | 温州大学 | Preparation method and application of composite glass material |
| CN115386374B (en) * | 2022-09-07 | 2023-08-15 | 包头稀土研究院 | Rare earth doped fluorescent material and preparation method and application thereof |
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| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| CN105121375A (en) * | 2013-07-25 | 2015-12-02 | 中央硝子株式会社 | Phosphor-dispersed glass |
| CN105198224A (en) * | 2015-09-09 | 2015-12-30 | 温州大学 | Ce:YAG glass ceramic as well as preparation method and application thereof |
| CN105637659A (en) * | 2013-12-17 | 2016-06-01 | 日本电气硝子株式会社 | Wavelength-conversion member and light-emitting device |
| CN105849921A (en) * | 2014-04-01 | 2016-08-10 | 日本电气硝子株式会社 | Wavelength conversion member and light emitting device using same |
| JP2018043912A (en) * | 2016-09-14 | 2018-03-22 | 旭硝子株式会社 | Photoconversion member, illumination light source and method for producing photoconversion member |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2016063930A1 (en) * | 2014-10-24 | 2017-08-03 | デンカ株式会社 | Wavelength converter, light emitting device using the same, and method of manufacturing wavelength converter |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| CN105121375A (en) * | 2013-07-25 | 2015-12-02 | 中央硝子株式会社 | Phosphor-dispersed glass |
| CN105637659A (en) * | 2013-12-17 | 2016-06-01 | 日本电气硝子株式会社 | Wavelength-conversion member and light-emitting device |
| CN105849921A (en) * | 2014-04-01 | 2016-08-10 | 日本电气硝子株式会社 | Wavelength conversion member and light emitting device using same |
| CN105198224A (en) * | 2015-09-09 | 2015-12-30 | 温州大学 | Ce:YAG glass ceramic as well as preparation method and application thereof |
| JP2018043912A (en) * | 2016-09-14 | 2018-03-22 | 旭硝子株式会社 | Photoconversion member, illumination light source and method for producing photoconversion member |
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