CN101643315B - Low-melting-point fluorescent glass for white light LED and preparation method thereof - Google Patents
Low-melting-point fluorescent glass for white light LED and preparation method thereof Download PDFInfo
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- CN101643315B CN101643315B CN2009100635282A CN200910063528A CN101643315B CN 101643315 B CN101643315 B CN 101643315B CN 2009100635282 A CN2009100635282 A CN 2009100635282A CN 200910063528 A CN200910063528 A CN 200910063528A CN 101643315 B CN101643315 B CN 101643315B
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Abstract
The invention relates to low-melting-point fluorescent glass for a white light LED and a preparation method thereof. The low-melting-point fluorescent glass for the white light LED is characterized by being prepared from raw materials containing the following components in percentage by weight: 1-20 percent of Na2O, 0-20 percent of ZnO, 20-40 percent of B2O3, 10-30 percent of SiO2, 1-25 percent of Al2O3, 0-10 percent of CaO, 0-4 percent of MgO, 0-1.5 percent of K2O and 5-30 percent of Ce-YAG. The preparation method comprises the following steps: firstly preparing low-melting-point glass by a fusion method, then mixing low-melting-point glass powder with fluorescent powder, and finally acquiring the low-melting-point fluorescent glass after sintering. The fluorescent glass acquired by the method has good luminescent performance of crystalline materials and excellent stability of glass materials, and can be used for white light LED devices for solving the problems of poor color stability and durability of the current white light LED.
Description
Technical field
The invention belongs to luminescent material, adulterated low-melting-point fluorescent glass of particularly a kind of fluorescent material and preparation method thereof.
Background technology
Total solids white light emitting diode (light emitting diode; LED) as the novel illumination light source; Having many-sided advantages such as energy-saving and environmental protection, long lifetime, designability are strong, is the lighting source of representative with replacing with incandescent light, luminescent lamp, causes a revolution on illumination circle.
The realization of white light LEDs is based upon on the basis that red-green-blue chip and all kinds of fluorescent material successfully researches and develops.LED realizes that the method for white light has at present: applying on the blue-light LED chip can be by the fluorescent material of blue-light excited emission gold-tinted, and two kinds of light mix the formation white light; Applying on the blue-light LED chip can be by the blue-light excited red-emitting and the fluorescent material of green glow, and three kinds of light mix the formation white light; Apply three primary colors fluorescent powder on purple light or the ultraviolet LED chip and obtain white light.
Some problems that white light LEDs exists.Wherein phosphor material powder is the important step of restriction white light LEDs performance.Present double-basis coloured light conversion of white light LED product, its light decay cause be unable to do without led chip, optical lens (being packaged material) and fluorescent material etc. equally.In addition, phosphor powder layer thickness inhomogeneous is prone to cause the tone drift of the white light that produces; Epoxy resin is prone to aging; The influence that fluorescent material receives temperature, make moist reduces the luminous efficiency of fluorescent material.
To the problem that LED exists, the investigator has made various effort both at home and abroad.Through improving the fluorescent material synthesis technique, the good fluorescent material of development luminescent properties; The doping and the kind thereof of the rare earth ion of adjustment fluorescent material, other rare earth sensitized ions of suitable interpolation makes it have high luminous efficiency; Improve the stability of fluorescent material through aftertreatment, carry out the surface of fluorescent material being modified after coating handles, can make fluorescent material have the better physical chemicalstability through chemical process; Improve fluorescent powder coating technique; Change fluorescent material matrix, as use glass, sytull, pottery or the like instead.Analyze from structure, fluorescent material doping low-melting-point fluorescent glass satisfies the fluorescent material of this requirement just.
Summary of the invention
The object of the invention provides a kind of low-melting-point fluorescent glass for white light LED and preparation method thereof, and this low-melting-point fluorescent glass can combine with blue-ray LED, realizes weather resistance, the stability of white light LEDs fluorescent material.
To achieve these goals, the technical scheme that the present invention adopted is: low-melting-point fluorescent glass for white light LED is characterized in that it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is:
Na
2O 1-20％，
ZnO 0-20％，
B
2O
3 20-40％，
SiO
2 10-30％，
Al
2O
3 1-25％，
CaO 0-10％，
MgO 0-4％，
K
2O 0-1.5％，
Ce-YAG 5-30％。
The shared mass percent the best of said ZnO is: 1-18%.
The shared mass percent the best of said CaO is: 1-8%.
The shared mass percent the best of said MgO is: 1-3%.
Said K
2The shared mass percent the best of O is: 0.5-1%.
The preparation method of above-mentioned low-melting-point fluorescent glass for white light LED is characterized in that it comprises the steps:
1) by the shared mass percent of each component is: Na
2O:1-20%, ZnO:0-20%, B
2O
3: 20-40%, SiO
2: 10-30%, Al
2O
3: 1-25%, CaO:0-10%, MgO:0-4%, K
2O:0-1.5%, Ce-YAG:5-30%; Take by weighing Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO, K
2CO
3With the Ce-YAG raw material, subsequent use;
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO and K
2CO
3Melt after raw materials mix is even, 900 ℃-1300 ℃ of temperature of fusion are incubated 1-3 hour, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, at N
2Sintering under the protective atmosphere, 400 ℃-600 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 0.5-3h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
The transition temperature Tg of resulting low-melting-point fluorescent glass for white light LED is 400-700 ℃.
The invention has the beneficial effects as follows (comparing): be doped to fluorescent material (Ce-YAG) in the suitable glass matrix with existing fluorescent material for white light LED; Through sintering processes to glass; Fluorescent material is coated by glass matrix, thereby obtain to have concurrently the fluorescent material of good luminous property of crystalline material and excellent stability of glass material.Low-melting-point fluorescent glass for white light LED of the present invention is fit to nearly blue-ray LED and excites, and can be used for white light LED part, and this low-melting-point fluorescent glass can combine with blue-ray LED, realizes weather resistance, the stability of white light LEDs fluorescent material.The invention solves the weather resistance of the fluorescent material that current white light LEDs causes because of sweating and/ or heating with fluorescent material and the problem of color stability difference.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with instance, but the present invention not only is confined to following embodiment.
Embodiment 1:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 1.
Table 1
Concrete preparation process is following: 1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 1
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3With the Ce-YAG raw material);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3Melt after raw materials mix is even, 900 ℃ of temperature of fusion are incubated 2 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 540 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 1h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Low-melting-point fluorescent glass to preparation carries out XRD and spectral quality test, and the result who obtains is following: XRD diffraction peak and yttrium aluminum garnet crystalline phase (YAG) through glass after the sintering processes are consistent, so the crystalline phase that contains in the glass is the yttrium aluminum garnet crystalline phase.Sample is mainly launched gold-tinted down the blue-light excited of 470nm, can be combined into white light with the blue light that blue-light LED chip sends.
Organic materials epoxy resin receives aging yellowing after the rayed, and aging back just influences the quality that it sends light, promptly photochromic stability naturally.Adopt low-melting-point fluorescent glass for white light LED of the present invention, be difficult for agingly, therefore the invention solves the weather resistance of the fluorescent material that current white light LEDs causes because of sweating and/ or heating with fluorescent material and the problem of color stability difference.
Embodiment 2:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 2.
Table 2
Concrete preparation process is following: 1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 2
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3With the Ce-YAG raw material);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3Melt after raw materials mix is even, 910 ℃ of temperature of fusion are incubated 2 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 550 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 1h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Low-melting-point fluorescent glass to preparation carries out XRD and spectral quality test, and the result who obtains is following: XRD diffraction peak and yttrium aluminum garnet crystalline phase (YAG) through glass after the sintering processes are consistent, so the crystalline phase that contains in the glass is the yttrium aluminum garnet crystalline phase.Sample is mainly launched gold-tinted down the blue-light excited of 470nm, can be combined into white light with the blue light that blue-light LED chip sends.
Embodiment 3:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, the feedstock production of CaO and Ce-YAG component forms; The shared mass percent of each component is seen table 3.
Table 3
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 3
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3With the Ce-YAG raw material);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3Melt after raw materials mix is even, 920 ℃ of temperature of fusion are incubated 2 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 560 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 1.5h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 4;
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, the feedstock production of CaO and Ce-YAG component forms; The shared mass percent of each component is seen table 4.
Table 4
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 4
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3With the Ce-YAG raw material);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3Melt after raw materials mix is even, 930 ℃ of temperature of fusion are incubated 2 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 570 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 1.5h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 5:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 5.
Table 5
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 5
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3With the Ce-YAG raw material);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3Melt after raw materials mix is even, 940 ℃ of temperature of fusion are incubated 2 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 580 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 2h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 6:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, B
2O
3, SiO
2, Al
2O
3, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 6.
Table 6
| Component | Na 2O | B 2O 3 | SiO 2 | Al 2O 3 | Ce-YAG |
| Component concentration (wt%) | 20 | 20 | 30 | 1 | 29 |
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 6
2CO
3, H
3BO
3, SiO
2, Al
2O
3With the Ce-YAG raw material);
2) with Na
2CO
3, H
3BO
3, SiO
2, Al
2O
3Melt after raw materials mix is even, 900 ℃ of temperature of fusion are incubated 1 hour, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 400 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 0.5h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 7:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, B
2O
3, SiO
2, Al
2O
3, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 7.
Table 7
| Component | Na 2O | B 2O 3 | SiO 2 | Al 2O 3 | Ce-YAG |
| Component concentration (wt%) | 15 | 20 | 10 | 25 | 30 |
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 7
2CO
3, H
3BO
3, SiO
2, Al
2O
3With the Ce-YAG raw material);
2) with Na
2CO
3, H
3BO
3, SiO
2, Al
2O
3Melt after raw materials mix is even, 1300 ℃ of temperature of fusion are incubated 3 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, place sintering oven, at N
2Sintering under the protective atmosphere, 600 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 3h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 8:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 8;
Table 8
| Component | Na 2O | ZnO | B 2O 3 | SiO 2 | Al 2O 3 | ?CaO | MgO | K 2O | Ce-YAG |
| Component concentration (wt%) | 1 | 1 | 20 | 20 | 25 | ?1 | 1 | 1 | 30 |
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 8
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO, K
2CO
3And Ce-YAG);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO and K
2CO
3Melt after raw materials mix is even, 900 ℃ ℃ of temperature of fusion are incubated 3 hours, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, sintering under protective atmosphere, 400 ℃ ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 3h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 9:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 9;
Table 9
| Component | Na 2O | ZnO | B 2O 3 | SiO 2 | Al 2O 3 | CaO | MgO | K 2O | Ce-YAG |
| Component concentration (wt%) | 1 | 18 | 20 | 10 | 9.5 | 8 | 3 | 0.5 | 30 |
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 9
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO, K
2CO
3And Ce-YAG);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO and K
2CO
3Melt after raw materials mix is even, 1300 ℃ of temperature of fusion are incubated 1 hour, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, sintering under protective atmosphere, 600 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 0.5h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Embodiment 10:
Low-melting-point fluorescent glass for white light LED, it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is seen table 10;
Table 10
| Component | Na 2O | ZnO | B 2O 3 | SiO 2 | Al 2O 3 | ?CaO | MgO | K 2O | Ce-YAG |
| Component concentration (wt%) | 1 | 20 | 20 | 10 | 13.5 | ?10 | 4 | 1.5 | 20 |
Concrete preparation process is following:
1) at first according to the prescription weighing certainweight analytical pure raw material (Na in the table 10
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO, K
2CO
3And Ce-YAG);
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO and K
2CO
3Melt after raw materials mix is even, 1300 ℃ of temperature of fusion are incubated 1 hour, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, sintering under protective atmosphere, 600 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 0.5h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
Each raw material that the present invention is cited and the bound value of each raw material, and the bound value of each processing parameter can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (2)
1. low-melting-point fluorescent glass for white light LED is characterized in that it is by comprising Na
2O, ZnO, B
2O
3, SiO
2, Al
2O
3, CaO, MgO, K
2The feedstock production of O and Ce-YAG component forms; The shared mass percent of each component is:
Na
2O 1-20％，
ZnO 1-18％，
B
2O
3 20-40％，
SiO
2 10-30％，
Al
2O
3 1-25％，
CaO 1-8％，
MgO 1-3％，
K
2O 0.5-1％，
Ce-YAG 5-30％。
2. the preparation method of low-melting-point fluorescent glass for white light LED as claimed in claim 1 is characterized in that it comprises the steps:
1) by the shared mass percent of each component is: Na
2O:1-20%, ZnO:1-18%, B
2O
3: 20-40%, SiO
2: 10-30%, Al
2O
3: 1-25%, CaO:1-8%, MgO:1-3%, K
2O:0.5-1%, Ce-YAG:5-30%; Take by weighing Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO, K
2CO
3With the Ce-YAG raw material, subsequent use;
2) with Na
2CO
3, ZnO, H
3BO
3, SiO
2, Al
2O
3, CaCO
3, MgO and K
2CO
3Melt after raw materials mix is even, 900 ℃-1300 ℃ of temperature of fusion are incubated 1-3 hour, obtain glass metal;
3) glass metal is poured in the cold water, carried out the shrend cooling, obtain residuite glass;
4) glass is worn into powder and Ce-YAG uniform mixing, at N
2Sintering under the atmosphere, 400 ℃-600 ℃ of sintering temperatures, 4 ℃/min of temperature rise rate, sintering time 0.5-3h, the cooling of annealing then promptly gets low-melting-point fluorescent glass for white light LED.
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