CN102040337A - Rare earth-doped yttrium aluminum garnet microcrystalline glass material and application thereof in white LED - Google Patents
Rare earth-doped yttrium aluminum garnet microcrystalline glass material and application thereof in white LED Download PDFInfo
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Abstract
The invention discloses a rare earth-doped yttrium aluminum garnet microcrystalline glass material and application thereof in a white light-emitting diode (LED). The rare earth-doped yttrium aluminum garnet microcrystalline glass material consists of the following components in percentage by mole: 0 to 20 percent of alkali metal oxide or alkaline earth metal oxide, 8 to 25 percent of Y2O3, 21 to 40 percent of Al2O3, 25 to 50 percent of SiO2 and 0.001 to 2 percent of oxide of rare-earth element Re. The microcrystalline glass material has the advantages of high excited emission efficiency, high uniformity, stable physical and chemical properties, long service life, high thermal conductivity and the like, is applied to the white LED, and can optimize the white LED package structure, reduce the cost and improve the luminous performance.
Description
Technical field
The present invention relates to rare-earth-dopping yttrium aluminum garnet (YAG) system glass ceramics and the application in white light LEDs thereof, belong to LED fluorescent material technical field.
Background technology
White light LEDs has, and volume is little, thermal value is low, current consumption is little, the life-span is long, speed of response is fast, but environmental protection planar package, easy exploiting become advantages such as frivolous small and exquisite product, be described as " the 4th generation lighting source " that will surmount incandescent light, luminescent lamp, application prospect is very wide.At present, the white light LEDs fluorescent material is mainly based on amorphous fluorescent material, and it is the development main flow that commercialization white light LEDs product forms white light with chip and phosphor combination.Current, as make high-level efficiency, high color rendering index (CRI), hang down colour temperature, large power white light LED to have become LED development active demand, and wherein the performance of fluorescent material (launching efficiency, luminous efficiency, homogeneity, materialization stability etc.) lifting is even more important.In order to address these problems, patent CN1836339A has narrated in white light LEDs lens surface plating fluorescent screen method, and CN101696085A discloses a kind of YAG fluorescent material and has been evenly distributed in the sodium borosilicate system glass and prepares blue-light excited fluorescent material.CN101314519 discloses a kind of white light LEDs and has mixed in borosilicate glass matrix it luminous under ultraviolet excitation altogether with rare earth Tb, Eu, Ce; CN101338879 openly utilizes the YAG crystalline ceramics to prepare the method for white light LEDs, and CN101643315 discloses low-melting-point fluorescent glass for white light LED, CN101749642A, a kind of blue-light excited white light LEDs fluorescent glass lens and preparation method thereof.
Summary of the invention
At the bottom of technical problem to be solved by this invention provides a kind of with short production cycle, cost, the rear-earth-doped YAG devitrified glass that is easy to produce in batches and preparation method thereof, this devitrified glass has outstanding advantages such as excitation-emission efficient height, high homogeneity, physical and chemical performance are stable, life-span length, thermal conductivity height, be applied to white light LEDs, can optimize white light packaged LED structure, reduce cost, improve luminescent properties.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
A kind of rare-earth-dopping yttrium aluminum garnet system glass ceramics material, the molar percentage of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material consists of: 0-20%, Y
2O
3: 8-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2%; The preparation of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material comprises the following steps:
(1) by the prescription of following molar percentage: alkalimetal oxide or alkaline earth metal oxide: 0-20%, Y
2O
3: 8-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2% weighing analytical pure raw material, pour in the crucible after raw material mixed and melt, glass melting temperature is 1600-1700 ℃, be incubated and after 2-5 hour glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gTemperature insulation 2-5 hour cools to 50 ℃ then with the furnace, closes the High Temperature Furnaces Heating Apparatus power supply and cools to room temperature automatically, takes out glass;
(2) glass that step (1) is made places the fine annealing stove at 1300-1500 ℃ of heat-treated 1-10 hour, cool to 50 ℃ then with the furnace, close fine annealing stove power supply, be cooled to room temperature automatically and obtain translucent rare-earth-dopping yttrium aluminum garnet system glass ceramics material.
In the step of the present invention (1), the oxide compound of rare earth elements RE is with REO
2Or RE
2O
3Add etc. form.
Further, the oxide compound of described rare earth elements RE is preferred following a kind of: CeO
2, Pr
2O
3, Sm
2O
3, Dy
2O
3, Er
2O
3, Nd
2O
3, EuO, Eu
2O
3, Cr
2O
3One of, more preferably following: CeO
2, Pr
2O
3, Sm
2O
3
Add alkalimetal oxide among the present invention (as Li
2O, Na
2O, K
2O etc.) or alkaline earth metal oxide (as SrO) mainly play fluxing action.
Further, the molar percentage of rare-earth-dopping yttrium aluminum garnet system glass ceramics material composition is preferably: alkalimetal oxide or alkaline earth metal oxide: 3-8%, Y
2O
3: 10-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2%.
Further, do not add solubility promoter alkalimetal oxide or alkaline earth metal oxide in the glass system, the molar percentage composition of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material is preferably: Y
2O
3: 10-25%, Al
2O
3: 25-40%, SiO
2: the oxide compound of 33-50%, rare earth elements RE: 0.001-2%.
Further, in the step (2), heat treatment time is preferably 5～10 hours.
Further, in the step (2), preferred 1400～1500 ℃ of thermal treatment temp.
Preferred corundum crucible of used crucible or platinum crucible in the step of the present invention (1).
The shape of the rear-earth-doped YAG devitrified glass that the present invention is prepared can be plane, concave surface, convex surface, and can cut, grind, polish.
Rare-earth-dopping yttrium aluminum garnet system glass ceramics material of the present invention can be applicable to prepare the fluorescent material in the white light LED part, can change the ray structure of white light LED part, simplifies packaging process, improves luminescent properties.
Compared with prior art, the present invention is with Y
2O
3-Al
2O
3-SiO
2Glass is as parent glass, add micro-RE, adopt preferred heat treating method to prepare pure phase YAG devitrified glass, the white light LEDs fluorescent glass-ceramics material that makes has outstanding advantages such as excitation-emission efficient height, high homogeneity, physical and chemical performance are stable, life-span length, thermal conductivity height, is applied to white light LEDs and can optimizes white light packaged LED structure, reduce cost, improve luminescent properties.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) figure of embodiment one different heat treatment temperature;
Fig. 2 is X-ray diffraction (XRD) figure of sample after the embodiment two enforcement micritization thermal treatments;
Fig. 3 is X-ray diffraction (XRD) figure of sample after the embodiment three enforcement micritization thermal treatments;
Fig. 4 is X-ray diffraction (XRD) figure of sample after the embodiment four enforcement micritization thermal treatments;
Fig. 5 is X-ray diffraction (XRD) figure of sample after the embodiment five enforcement micritization thermal treatments;
Fig. 6 is X-ray diffraction (XRD) figure of sample after the embodiment six enforcement micritization thermal treatments;
The emmission spectrum of the Ce:YAG devitrified glass that Fig. 7 excites for embodiment two to six usefulness 460nm wavelength.
Embodiment
Implement the present invention done below in conjunction with accompanying drawing and describe in further detail.
Glass under the different crystallization temperatures of embodiment one table 1
The first step, the prescription weighing 50 of pressing table 1 restrains the analytical pure raw materials, pours in the platinum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second the step, will make glass place the fine annealing stove respectively 980 ℃, 1080 ℃, 1240 ℃, 1340 ℃, 1400 ℃ thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
To the spectral quality test of the YAG devitrified glass of preparation, the XRD figure of the glass that obtains after micritization is handled as shown in Figure 1, its result is as follows: 980 ℃ do not have YAG to generate mutually, 1080 ℃ have a small amount of YAG with Y
2Si
2O
7Generate, 1240 ℃ have YAG and Y
2Si
2O
7Generate, 1340 ℃ have YAG and Y
2Si
2O
7Generation, 1400 ℃ of generation pure phase YAG, the material that obtains is that principal crystalline phase is the devitrified glass of YAG crystallization phase, does not have other impurity phase.
Embodiment two tables 2 are glass formula and recrystallization temperature
Table 2
Concrete preparation process is as follows:
The first step, the prescription weighing 50 of pressing table 2 restrains the analytical pure raw materials, pours in the platinum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second step will make glass and place the fine annealing stove 1400 ℃ of thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
Spectral quality test to the YAG devitrified glass of preparation, the XRD figure of the glass that obtains after micritization is handled as shown in Figure 2, its result is as follows: the sample XRD diffraction peak that obtains through Overheating Treatment all conforms to the main diffraction peak of the standard map of YAG crystalline phase, the material crystalline phase that obtains is the devitrified glass of YAG phase, does not have other impurity phase; And the Ce:YAG devitrified glass emmission spectrum that is excited by the 460nm wavelength is shown in Fig. 7 a, and it is similar to Ce:YAG crystalline fluorescence Spectra, and fluorescence intensity is in the 537nm maximum.
Embodiment three tables 3 are glass formula and recrystallization temperature
Table 3
Concrete preparation process is as follows:
The first step, the prescription weighing 50 of pressing table 3 restrains the analytical pure raw materials, pours in the platinum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second step will make glass and place the fine annealing stove 1440 ℃ of thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
Spectral quality test to the YAG devitrified glass of preparation, the XRD figure of the glass that obtains after micritization is handled as shown in Figure 3, its result is as follows: the sample XRD diffraction peak that obtains through Overheating Treatment all conforms to the main diffraction peak of the standard map of YAG crystalline phase, therefore the material that obtains is the devitrified glass of pure YAG crystallization phase, does not have other impurity phase; Because of Ce
3+Ionic radius for being slightly larger than Y
3+So, Ce during micritization thermal treatment
3+Can substitute Y
3+Enter into YAG lattice position.And the Ce:YAG devitrified glass emmission spectrum that is excited by the 460nm wavelength is shown in Fig. 7 b, and it is similar to Ce:YAG crystalline fluorescence Spectra, and fluorescence intensity is in the 537nm maximum.
Embodiment four table 4 glass formula and recrystallization temperatures
Table 4
Concrete preparation process is as follows:
The first step, the prescription weighing 50 of pressing table 4 restrains the analytical pure raw materials, pours in the platinum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second step will make glass and place the fine annealing stove 1400 ℃ of thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
Spectral quality test to the YAG devitrified glass of preparation, the glass that obtains XRD such as Fig. 4 after micritization is handled, its result is as follows: the sample XRD diffraction peak that obtains through Overheating Treatment all conforms to the main diffraction peak of the standard map of YAG crystalline phase, therefore the material that obtains is the devitrified glass of pure YAG crystallization phase, does not have other impurity phase; Because of Ce
3+Ionic radius for being slightly larger than Y
3+So, Ce during micritization thermal treatment
3+Can substitute Y
3+Enter into YAG lattice position.And the Ce:YAG devitrified glass emmission spectrum such as Fig. 7 c that are excited by the 460nm wavelength, it is similar to Ce:YAG crystalline fluorescence Spectra, and fluorescence intensity is in the 531nm maximum.
Embodiment five table 5 glass formula and recrystallization temperatures
Table 5
Concrete preparation process is as follows:
The first step, the prescription weighing 50 of pressing table 5 restrains the analytical pure raw materials, pours in the corundum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second step will make glass and place the fine annealing stove 1400 ℃ of thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
Spectral quality test to the YAG devitrified glass of preparation, the XRD figure of the glass that obtains after micritization is handled as shown in Figure 5, its result is as follows: the sample XRD diffraction peak that obtains through Overheating Treatment all conforms to the main diffraction peak of the standard map of YAG crystalline phase, the material that obtains is the devitrified glass of pure YAG crystallization phase, does not have other dephasign to generate; Ce
3+Substitute Y
3+Enter into YAG lattice position.The Ce:YAG devitrified glass emmission spectrum that excites at the 460nm wavelength is shown in Fig. 7 d, and it is similar to Ce:YAG crystalline fluorescence Spectra, and fluorescence intensity is in the 531nm maximum.
Embodiment six table 6 glass formula and recrystallization temperatures
Table 6
Concrete preparation process is as follows:
The first step, the prescription weighing 50 of pressing table 6 restrains the analytical pure raw materials, pours in the corundum crucible after raw material is mixed and melts, 1650 ℃ of glass melting temperatures, be incubated and after 2 hours glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gThe temperature insulation cools to 50 ℃ with the furnace after 2 hours then, closes the High Temperature Furnaces Heating Apparatus power supply and will ask room temperature automatically, takes out glass; Second step will make glass and place the fine annealing stove 1400 ℃ of thermal treatments 9 hours, cool to 50 ℃ then with the furnace.Close fine annealing stove power supply and be cooled to room temperature automatically, obtain the translucent cerium YAG devitrified glass sample of mixing.
Spectral quality test to the YAG devitrified glass of preparation, the glass that obtains XRD such as Fig. 6 after micritization is handled, the result is as follows: the sample XRD diffraction peak that obtains through Overheating Treatment all conforms to the main diffraction peak of the standard map of YAG crystalline phase, the material that obtains is the devitrified glass of pure YAG crystallization phase, does not have other dephasign to generate; Ce
3+Substitute Y
3+Enter into YAG lattice position.At Ce:YAG devitrified glass emmission spectrum such as Fig. 7 e that the 460nm wavelength excites, it is similar to Ce:YAG crystalline fluorescence Spectra, and fluorescence intensity is in the 531nm maximum.
Claims (9)
1. rare-earth-dopping yttrium aluminum garnet system glass ceramics material, it is characterized in that: the molar percentage of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material consists of: alkalimetal oxide or alkaline earth metal oxide: 0-20%, Y
2O
3: 8-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2%; The preparation of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material comprises the following steps:
(1) by the prescription of following molar percentage: alkalimetal oxide or alkaline earth metal oxide: 0-20%, Y
2O
3: 8-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2% weighing analytical pure raw material, pour in the crucible after raw material mixed and melt, glass melting temperature 1600-1700 ℃, be incubated and after 2-5 hour glass melt poured on the pig mold, place High Temperature Furnaces Heating Apparatus to anneal then, in glass transformation temperature T
gTemperature insulation 2-5 hour cools to 50 ℃ then with the furnace, closes the High Temperature Furnaces Heating Apparatus power supply and cools to room temperature automatically, takes out glass;
(2) glass that step (1) is made places the fine annealing stove 1300-1500 ℃ of heat-treated 1～10 hour, cool to 50 ℃ then with the furnace, close fine annealing stove power supply, be cooled to room temperature automatically and obtain translucent rare-earth-dopping yttrium aluminum garnet system glass ceramics material.
2. rare-earth-dopping yttrium aluminum garnet system glass ceramics material according to claim 1 is characterized in that: the oxide compound of described rare earth elements RE is selected from one of following: CeO
2, Pr
2O
3, Sm
2O
3, Dy
2O
3, Er
2O
3, Nd
2O
3, EuO, Eu
2O
3, Cr
2O
3
3. rare-earth-dopping yttrium aluminum garnet system glass ceramics material according to claim 1, it is characterized in that: the oxide compound of described rare earth elements RE is selected from following a kind of: CeO
2, Pr
2O
3, Sm
2O
3
4. according to the described rare-earth-dopping yttrium aluminum garnet system glass ceramics of one of claim 1～3 material, it is characterized in that: the molar percentage of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material consists of: alkalimetal oxide or alkaline earth metal oxide: 3-8%, Y
2O
3: 10-25%, Al
2O
3: 21-40%, SiO
2: the oxide compound of 25-50%, rare earth elements RE: 0.001-2%.
5. according to the described rare-earth-dopping yttrium aluminum garnet system glass ceramics of one of claim 1～3 material, it is characterized in that: the molar percentage of described rare-earth-dopping yttrium aluminum garnet system glass ceramics material consists of: Y
2O
3: 10-25%, Al
2O
3: 25-40%, SiO
2: the oxide compound of 33-50%, rare earth elements RE: 0.001-2%.
6. according to the described rare-earth-dopping yttrium aluminum garnet system glass ceramics of one of claim 1～3 material, it is characterized in that: in the step (2), heat treatment time is 5～10 hours.
7. according to the described rare-earth-dopping yttrium aluminum garnet system glass ceramics of one of claim 1～3 material, it is characterized in that: in the step (2), thermal treatment temp is 1400～1500 ℃.
8. according to the described rare-earth-dopping yttrium aluminum garnet system glass ceramics of one of claim 1～3 material, it is characterized in that: used crucible is corundum crucible or platinum crucible in the step (1).
9. rare-earth-dopping yttrium aluminum garnet system glass ceramics material according to claim 1 in the preparation white light LED part as the application of fluorescent material.
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