CN105152535A - Fluorescent glass ceramic, preparation method of fluorescent glass ceramic and application of fluorescent glass ceramic in preparing laser light source - Google Patents

Fluorescent glass ceramic, preparation method of fluorescent glass ceramic and application of fluorescent glass ceramic in preparing laser light source Download PDF

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CN105152535A
CN105152535A CN201510599939.9A CN201510599939A CN105152535A CN 105152535 A CN105152535 A CN 105152535A CN 201510599939 A CN201510599939 A CN 201510599939A CN 105152535 A CN105152535 A CN 105152535A
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fluorescent glass
preparation
fluorescent
glass ceramic
glass powder
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王乐
罗东
潘桦滟
陈如标
吴拓
李旸晖
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China Jiliang University
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China Jiliang University
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Abstract

The invention discloses fluorescent glass ceramic, a preparation method of the fluorescent glass ceramic and application of the fluorescent glass ceramic in preparing a laser light source. The preparation method includes the steps that alpha-Si3N4, AlN, Al2O3 and Eu2O3 are subjected to heat preservation for 1-5 h at the temperature of 1500-2400 DEG C and the pressure intensity of 0.6-1.4 Mpa, the product is ground and sieved after being cooled, and Eu-doped Si-Al-O-N green fluorescent powder is obtained; the Eu-doped Si-Al-O-N green fluorescent powder and glass powder are subjected to heat preservation for 45-120 min at temperature of 450-700 DEG C after being mixed, and the fluorescent glass ceramic is obtained. The prepared green fluorescent powder is excellent in luminescence performance, the fluorescent glass ceramic prepared from the fluorescent glass ceramic compounded with the low-melting-point glass powder is excellent in heat stability, capable of being used for preparing the laser light source and resistant to blue light, the luminescence performance is not influenced, and the phenomenon of material deterioration or color changing will not occur in long-time high-temperature operation.

Description

Fluorescent glass pottery and preparation method thereof and the application in preparation LASER Light Source
Technical field
The present invention relates to the packaged material technical field of LASER Light Source, be specifically related to a kind of fluorescent glass pottery and preparation method thereof and the application in preparation LASER Light Source.
Background technology
Along with display and the improving constantly of light source technology, projection display technique is widely used in the fields such as amusement, education, medical treatment, and display industries is promptly risen, and becomes one of important electronics and information industry.Wherein, projection display technique refers to that the red, green, blue three primary colours utilizing light source to send carry out imaging, then after the amplification process of optical system, shows the technology of image in projection screen.Therefore, for improving projection quality, need to find suitable projection light source.The light source used at present is generally cathode tube, but also exists that luminous intensity is low, lack of homogeneity, volume large, the quality problem such as heavily.And laser is a kind of high directivity, the light source that brightness is high, can excitated fluorescent powder effectively, radiates the light of high brightness.Therefore, people propose to adopt laser illuminator light source to realize projection display technique.But LASER Light Source has the features such as high-power light emitting due to it, the heat that light source is produced at luminescence process is comparatively large, and then has influence on the working efficiency of whole indicating system.Therefore need to find suitable encapsulating structure and the good packaged material of thermal conductivity, and carry out corresponding optical design, thus effectively improve the luminous efficiency of LASER Light Source.
At present, common packaged material mainly epoxy resin.But the resistance toheat of this kind of organic packaging materials of epoxy resin itself is not high, and higher to the susceptibility of short-wave band light, and make under long hot operation, material there will be the phenomenon such as deterioration, variable color, greatly has influence on the luminous efficiency of lighting system.
Application publication number is that the Chinese invention patent application of CN104610967A (application number is 201510081434.3) discloses a kind of rear-earth-doped nitrogen oxide green fluorescent powder material, and the chemical general formula of this nitric oxide fluorescent powder is Ba 1-yln xal 2-x-zsi zo 4-zn z: yEu 2+, wherein, the rare earth ion Ln=Y of doping, La, Gd or Lu, the preparation method of this green emitting phosphor comprises: with Si, Al, Ba and Ln (Ln=Y, La, Gd or Lu) simple substance, oxide compound or corresponding salt and Si 3n 4for raw material, take corresponding raw material according to its chemical constitution and metering; Si will be removed 3n 4raw material add solubility promoter mixing after grinding evenly, the mixture high temperature roast after grinding; Product after above-mentioned roast is ground, then adds Si 3n 4after mixing, grinding evenly, the high-temperature calcination in reducing atmosphere of the mixture after grinding; Again through aftertreatment, namely obtain final product nitrogen oxygen oxide green emitting phosphor.This nitrogen oxygen oxide green emitting phosphor is added by the doping of rare earth ion and the selection of group solvent, improve the characteristics of luminescence of fluorescent material, but by it and epoxy resin is used for LASER Light Source jointly time, higher to the susceptibility of short-wave band light, make under long hot operation, material there will be the phenomenon such as deterioration, variable color.
Summary of the invention
For solving the technical problem of above-mentioned existence, realize high-brightness projection display, solve the problems such as power light source package cooling poor performance, the invention provides a kind of fluorescent glass pottery and preparation method thereof and the application in preparation LASER Light Source, by specific green emitting phosphor and glass powder compound, the fluorescent glass pottery Heat stability is good of preparation, can at high temperature long-play.
A preparation method for fluorescent glass pottery, comprises the following steps:
1) by α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3, under the environment being full of reducing gas, at temperature 1500 DEG C ~ 2400 DEG C and pressure 0.6Mpa ~ 1.4Mpa condition, be incubated 1h ~ 5h, after cooling, grind, sieve, obtain the green emitting phosphor of the silicon aluminum oxygen nitrogen of europium doping;
2) by step 1) after the green emitting phosphor of the silicon aluminum oxygen nitrogen of the europium prepared doping and glass powder mixing, at 450 DEG C to 700 DEG C insulation 45min ~ 120min, obtain fluorescent glass pottery;
Described glass powder is SiO 2-BaO-ZnO-B 2o 3-Al 2o 3system glass powder, Na 2o-Al 2o 3-B 2o 3system glass powder, V 2o 5-B 2o 3-TeO 2system glass powder, ZnO-B 2o 3-Ba 2o 3-Al 2o 3system glass powder or CaO-MgO-SiO 2system glass powder.
In the present invention, ad hoc approach is adopted to prepare the green emitting phosphor of the silicon aluminum oxygen nitrogen of europium doping, make it have excellent luminescent properties, and, prepare fluorescent glass pottery with specific glass powder with low melting point compound, make it have good thermostability, and do not affect luminescent properties, can blue light be resisted, under long hot operation, still can keep good thermostability, there will not be the phenomenon such as material degradation, variable color.
Following as the preferred technical solution of the present invention:
Step 1) in, at temperature 1800 DEG C ~ 2200 DEG C and pressure 0.8Mpa ~ 1.2Mpa condition, be incubated 1.5h ~ 4h.
Described reducing gas is nitrogen, argon gas or nitrogen and hydrogen mixture.
Before insulation, be warmed up to 1500 DEG C ~ 2400 DEG C with 15 ~ 30 DEG C/min (preferably 20 DEG C/min) temperature rise rate.
Described insulation is carried out in pyrocarbon pipe furnace.
The green emitting phosphor of the silicon aluminum oxygen nitrogen of described europium doping is β type green emitting phosphor, and its chemical formula is Si 6-zal zo zn 8-z: Eu 2+, wherein, the scope of z is 0 < z≤4.2.Further preferred, the chemical formula of the green emitting phosphor of the silicon aluminum oxygen nitrogen of described europium doping is Si 5.5al 0.5o 0.5n 7.5: Eu 2+.
Step 2) in, the glass powder that the present invention selects is glass powder with low melting point.Further preferably, described glass powder is SiO 2-BaO-ZnO-B 2o 3-Al 2o 3system glass powder or CaO-MgO-SiO 2system glass powder.Described SiO 2-BaO-ZnO-B 2o 3-Al 2o 3the mol ratio of system glass powder is 0.4:0.3:0.2:0.05:0.05.Described CaO-MgO-SiO 2the mol ratio of system glass powder is 0.3:0.4:0.4.
The green emitting phosphor of the silicon aluminum oxygen nitrogen of described europium doping and glass powder are in total mass percentage ratio 100%, for mass percent 2% ~ 8% green emitting phosphor and mass percent 92% ~ 98% glass powder, more preferably mass percent 5% green emitting phosphor and mass percent 95% glass powder.When fluorescent material mass percent increases gradually in 0 ~ 8% scope, fluorescent glass Ceramic Luminescence intensity increases gradually.When fluorescent material mass percent is more than 8%, fluorescent glass Ceramic Luminescence intensity reduces gradually.
At 500 DEG C to 660 DEG C insulation 60min ~ 120min.
Fluorescent glass pottery prepared by the present invention, can be used for preparing LASER Light Source, especially for the LASER Light Source of Projection Display, described LASER Light Source, comprise blue laser chip and be encapsulated in the fluorescent glass pottery (also can claim devitrified glass) on described blue laser chip, this devitrified glass, under blue laser chip excites, can prepare green light source, or prepares white light source device in conjunction with other red light sources again.
Compared with prior art, tool of the present invention has the following advantages:
In the present invention, ad hoc approach is adopted to prepare the green emitting phosphor of the silicon aluminum oxygen nitrogen of europium doping, make it have excellent luminescent properties, and, prepare fluorescent glass pottery with specific glass powder with low melting point compound, make it have good thermostability, and do not affect luminescent properties, can blue light be resisted, under long hot operation, still can keep good thermostability, there will not be the phenomenon such as material degradation, variable color.
LASER Light Source of the present invention, adopts laser blue chip excitated fluorescent powder, utilizes the characteristics such as the monochromatic ray of laser, luminous high concentration, energy density are high, the green emitting phosphor of the silicon aluminum oxygen nitrogen that can effectively excite europium of the present invention to adulterate, improve luminous power.Devitrified glass formula encapsulates, and can improve the heat dispersion of laser chip, strengthens the stability of fluorescent material.Further, effectively can solve packaged material Yin Gaowen or short-wavelength light and the material degradation problem caused, improve the luminescent properties of device.
Accompanying drawing explanation
Fig. 1 is the utilizing emitted light spectrogram that 440nm ordinary light source excites fluorescent glass pottery obtained in embodiment 1;
Fluorescence spectrum figure measured by the fluorescent glass pottery that Fig. 2 excites embodiment 1 to prepare for 440nm LASER Light Source;
Fig. 3 is the SiO that embodiment 1 obtains 2-BaO-ZnO-B 2o 3-Al 2o 3scanning electronic microscope (SEM) figure of glass powder with low melting point;
Fig. 4 is the Si that fluorescent glass is ceramic and comparative example 1 is obtained that embodiment 1 obtains 5.5al 0.5o 0.5n 7.5: Eu 2+the comparison diagram of the thermostability of green emitting phosphor;
Fig. 5 is the Si of preparation in comparative example 1 5.5al 0.5o 0.5n 7.5: Eu 2+the SEM figure of green emitting phosphor;
Fig. 6 is the SEM figure of fluorescent glass pottery prepared by embodiment 1.
Embodiment
Embodiment 1
A fluorescent glass pottery, by the SiO of 95wt% 2-BaO-ZnO-B 2o 3-Al 2o 3the Si of glass powder with low melting point and 5wt% 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor forms.
1) proportionally precise α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3raw material, puts into crucible after mixing, and moves to and is full of in the pyrocarbon pipe furnace of nitrogen reducing gas, and in stove, pressure is 1.0Mpa.After being warming up to 2000 DEG C, soaking time is set to 3h, is cooled to after room temperature 25 DEG C, is ground by taking-up sample, sieve, obtain high purity Si until in-furnace temperature 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor.
2) according to mol ratio precise 40%SiO 2, 30%BaO, 20%ZnO, 5%B 2o 3, 5%Al 2o 3be placed in after agate mortar mixes, move in crucible, be placed on and be full of in the pyrocarbon pipe furnace of nitrogen reducing gas, be warming up to 1300 DEG C, fully react 1h, treat that reaction in furnace terminates, take out sample and grind, obtain SiO 2-BaO-ZnO-B 2o 3-Al 2o 3glass powder with low melting point.
3) by the Si of 5wt% 5.5al 0.5o 0.5n 7.5: Eu 2+the SiO of green emitting phosphor and 95wt% 2-BaO-ZnO-B 2o 3-Al 2o 3glass powder is put into agate mortar and is mixed in proportion, and is pressed into disc-shaped, is placed in retort furnace, reheats to 630 DEG C, insulation 60min, thus obtains fluorescent glass pottery.
Fig. 1 is the utilizing emitted light spectrogram that 440nm ordinary light source excites fluorescent glass pottery obtained in embodiment 1, as shown in Figure 1, mixes the Si of 5wt% 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor, effectively can improve the luminous intensity of fluorescent glass pottery.
Fluorescence spectrum figure measured by the fluorescent glass pottery that Fig. 2 excites embodiment 1 to prepare for 440nm LASER Light Source.Show in figure: blue laser light source can excite devitrified glass effectively, and the green intensity sent is high, can be applied in laser projection display field.
Fig. 3 is the SiO that embodiment 1 obtains 2-BaO-ZnO-B 2o 3-Al 2o 3the SEM figure of glass powder with low melting point.As can be seen from the figure, particle size is in 1-5 μm, and this shows SiO 2-BaO-ZnO-B 2o 3-Al 2o 3glass powder with low melting point has less lattice imperfection, has good stability.
Embodiment 2
A fluorescent glass pottery, by the CaO-MgO-SiO of 95wt% 2the Si of glass powder and 5wt% 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor forms.
1) proportionally precise α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3raw material, puts into crucible after mixing, and moves to and is full of in the pyrocarbon pipe furnace of nitrogen reducing gas, and in stove, pressure is 1.0Mpa.After being warming up to 2000 DEG C, soaking time is set to 3h, is cooled to after room temperature 25 DEG C, is ground by taking-up sample, sieve, obtain high purity Si until in-furnace temperature 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor.
2) according to mol ratio precise 30%CaO, 30%MgO, 40%SiO 2be placed in after agate mortar mixes, move in crucible, be placed on and be full of in the pyrocarbon pipe furnace of nitrogen reducing gas, be warming up to 1300 DEG C, fully react 1h, treat that reaction in furnace terminates, take out sample and grind, obtain CaO-MgO-SiO 2glass powder with low melting point.
3) by the Si of 5wt% 5.5al 0.5o 0.5n 7.5: Eu 2+the CaO-MgO-SiO of green emitting phosphor and 95wt% 2glass powder with low melting point is mixed in proportion in agate mortar, and is pressed into disc-shaped, is placed in retort furnace, reheats to 630 DEG C, insulation 60min, thus obtains the fluorescent glass pottery for laser projection.
Comparative example 1
A kind of Si 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor, by α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3make.
Proportionally precise α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3raw material, puts into crucible after mixing, and moves to and is full of in the pyrocarbon pipe furnace of nitrogen reducing gas, and in stove, pressure is 1.0Mpa.After being warming up to 2000 DEG C, soaking time is set to 3h, is cooled to after room temperature 25 DEG C, is ground by taking-up sample, sieve, obtain high purity Si until in-furnace temperature 5.5al 0.5o 0.5n 7.5: Eu 2+green emitting phosphor.
Fig. 4 is the Si that fluorescent glass is ceramic and comparative example 1 is obtained that embodiment 1 obtains 5.5al 0.5o 0.5n 7.5: Eu 2+the thermostability comparison diagram of green emitting phosphor.Shown by figure: adopt the mode of fluorescent glass pottery not reduce the thermostability of fluorescent material, embody fluorescent glass ceramic packing formula method and effectively can retain the good thermostability of fluorescent material.
Fig. 5 is the Si of preparation in comparative example 1 5.5al 0.5o 0.5n 7.5: Eu 2+the SEM figure of green emitting phosphor.Shown by figure, the fluorescent powder grain distribution of preparation is comparatively even, can be applied to encapsulation preferably.
Fig. 6 is the SEM figure of fluorescent glass pottery prepared by embodiment 1.Have figure to find out, fluorescent material and glass powder merge closely, form fine and close microtexture, effectively by laser excitation, can produce brightness, the saturate light source of light.

Claims (10)

1. a preparation method for fluorescent glass pottery, is characterized in that, comprises the following steps:
1) by α-Si 3n 4, AlN, Al 2o 3and Eu 2o 3, under the environment being full of reducing gas, at temperature 1500 DEG C ~ 2400 DEG C and pressure 0.6Mpa ~ 1.4Mpa condition, be incubated 1h ~ 5h, after cooling, grind, sieve, obtain the green emitting phosphor of the silicon aluminum oxygen nitrogen of europium doping;
2) by step 1) after the green emitting phosphor of the silicon aluminum oxygen nitrogen of the europium prepared doping and glass powder mixing, at 450 DEG C to 700 DEG C insulation 45min ~ 120min, obtain fluorescent glass pottery;
Described glass powder is SiO 2-BaO-ZnO-B 2o 3-Al 2o 3system glass powder, Na 2o-Al 2o 3-B 2o 3system glass powder, V 2o 5-B 2o 3-TeO 2system glass powder, ZnO-B 2o 3-Ba 2o 3-Al 2o 3system glass powder or CaO-MgO-SiO 2system glass powder.
2. the preparation method of fluorescent glass pottery according to claim 1, is characterized in that, step 1) in, at temperature 1800 DEG C ~ 2200 DEG C and pressure 0.8Mpa ~ 1.2Mpa condition, be incubated 1.5h ~ 4h.
3. the preparation method of fluorescent glass pottery according to claim 1, is characterized in that, step 1) in, described reducing gas is nitrogen, argon gas or nitrogen and hydrogen mixture.
4. the preparation method of fluorescent glass pottery according to claim 1, is characterized in that, step 1) in, before insulation, be warmed up to 1500 DEG C ~ 2400 DEG C with 15 ~ 30 DEG C/min temperature rise rate.
5. the preparation method of fluorescent glass pottery according to claim 1, is characterized in that, step 1) in, the chemical formula of the green emitting phosphor of the silicon aluminum oxygen nitrogen of described europium doping is Si 6-zal zo zn 8-z: Eu 2+, wherein, the scope of z is 0 < z≤4.2.
6. the preparation method of fluorescent glass pottery according to claim 1, it is characterized in that, step 2) in, the green emitting phosphor of the silicon aluminum oxygen nitrogen of described europium doping and glass powder, in total mass percentage ratio 100%, are mass percent 2% ~ 8% green emitting phosphor and mass percent 92% ~ 98% glass powder.
7. the preparation method of fluorescent glass pottery according to claim 1, is characterized in that, step 2) in, at 500 DEG C to 660 DEG C insulation 60min ~ 120min.
8. fluorescent glass pottery prepared by the preparation method according to any one of claim 1 ~ 7.
9. the application of fluorescent glass pottery according to claim 8 in preparation LASER Light Source.
10. application according to claim 9, is characterized in that, described LASER Light Source, comprises blue laser chip and is encapsulated in the fluorescent glass pottery on described blue laser chip.
CN201510599939.9A 2015-09-18 2015-09-18 Fluorescent glass ceramic, preparation method of fluorescent glass ceramic and application of fluorescent glass ceramic in preparing laser light source Pending CN105152535A (en)

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CN106830690A (en) * 2017-03-03 2017-06-13 中南大学 Silicon nitride/the aluminium nitride of a kind of self-reinforcing toughness reinforcing/lanthanum barium Aluminous Silicate Glass-Ceramics trielement composite material and preparation method thereof
CN106833611A (en) * 2017-01-25 2017-06-13 东华大学 A kind of Nitride phosphor/glass powder with low melting point composite fluorescence lamella and preparation method thereof
CN108249772A (en) * 2018-01-19 2018-07-06 南昌大学 Preparation method based on the nanocrystalline luminescent microcrystal glass of rare earth ion doped Yttrium Orthovanadate
CN110156326A (en) * 2018-02-11 2019-08-23 天津理工大学 Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof
CN110483069A (en) * 2019-09-12 2019-11-22 周立军 Inorganic ceramic energy-storing self-luminescent material and its preparation method and application, self-luminescent ceramic particle and self-luminescent ceramic brick
CN115180835A (en) * 2022-07-14 2022-10-14 江西理工大学 Sapphire-based fluorescent glass ceramic and preparation method thereof

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CN109721250B (en) * 2016-12-01 2021-11-26 天津理工大学 Method for preparing luminescent glass ceramic by using low-melting-point glass powder
CN106587641A (en) * 2016-12-01 2017-04-26 天津理工大学 Low-melting-point glass powder and laser-illumination glass ceramic made from low-melting-point glass powder
CN109721250A (en) * 2016-12-01 2019-05-07 天津理工大学 The method for preparing luminescent glass ceramic with glass powder with low melting point
CN106587641B (en) * 2016-12-01 2019-05-07 天津理工大学 Glass powder with low melting point and its laser lighting glass ceramics of manufacture
CN106833611A (en) * 2017-01-25 2017-06-13 东华大学 A kind of Nitride phosphor/glass powder with low melting point composite fluorescence lamella and preparation method thereof
CN106830690A (en) * 2017-03-03 2017-06-13 中南大学 Silicon nitride/the aluminium nitride of a kind of self-reinforcing toughness reinforcing/lanthanum barium Aluminous Silicate Glass-Ceramics trielement composite material and preparation method thereof
CN106830690B (en) * 2017-03-03 2019-02-19 中南大学 A kind of silicon nitride/aluminium nitride of self-reinforcing toughening/lanthanum barium Aluminous Silicate Glass-Ceramics trielement composite material and preparation method thereof
CN108249772A (en) * 2018-01-19 2018-07-06 南昌大学 Preparation method based on the nanocrystalline luminescent microcrystal glass of rare earth ion doped Yttrium Orthovanadate
CN110156326B (en) * 2018-02-11 2021-11-26 天津理工大学 Fluorescent glass ceramic based on low-melting-point glass powder and preparation method thereof
CN110156326A (en) * 2018-02-11 2019-08-23 天津理工大学 Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof
CN110483069A (en) * 2019-09-12 2019-11-22 周立军 Inorganic ceramic energy-storing self-luminescent material and its preparation method and application, self-luminescent ceramic particle and self-luminescent ceramic brick
CN115180835A (en) * 2022-07-14 2022-10-14 江西理工大学 Sapphire-based fluorescent glass ceramic and preparation method thereof
CN115180835B (en) * 2022-07-14 2023-10-24 江西理工大学 Sapphire-based fluorescent glass ceramic and preparation method thereof

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Application publication date: 20151216