CN101885966A - A kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof - Google Patents
A kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof Download PDFInfo
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- CN101885966A CN101885966A CN2010102347691A CN201010234769A CN101885966A CN 101885966 A CN101885966 A CN 101885966A CN 2010102347691 A CN2010102347691 A CN 2010102347691A CN 201010234769 A CN201010234769 A CN 201010234769A CN 101885966 A CN101885966 A CN 101885966A
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Abstract
The present invention relates to a kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof.The chemical constitution of this composite phosphor is: (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05.The compound dissolution that accurately takes by weighing the compound of compound, aluminium of strontium and europium in proportion mixes with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made in deionized water or acid again with by tetraethoxy.Be adjusted to suitable pH value with acid, form colloidal sol; The colloidal sol oven dry is xerogel, forms reactive powder through calcining again, this powder is through wet-milling, and roasting at high temperature promptly gets the Sr-Al-Si series composite fluorescent powder of mixing europium.The present invention adopts a kind of chemical formulation and forms two kinds of different crystals simultaneously, by the visible light that to launch two to three kinds of different colours that excites to rare earth elements europium, can change two kinds of crystalline luminous intensities by adjusting chemical composition and maturing temperature, thereby adjust the luminescent properties of mixed light, can be used in the white light LED part.
Description
Technical field
The invention belongs to rare earth luminescent material manufacturing technology field, particularly a kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof.
Background technology
White light LEDs is a kind of solid-state semiconductor device that electric energy is converted into white light, have the efficient height, plurality of advantages such as volume is little, the life-span is long, safety, voltage are low, energy-saving and environmental protection, by people regard as after incandescent light, luminescent lamp, high-voltage gas discharging light the 4th generation lighting source, be used widely in fields such as backlight, demonstration, automobile, commerce and special lightings.
At present, realize that white light LEDs has multiple scheme.A kind of is how chip-shaped white light LEDs.This scheme needs the corresponding with it pilot circuit of many covers, causes cost to significantly improve; Because the rate of decay and the life-span of each chip have nothing in common with each other, cause the white light that forms in time photochromic and change, cause the white light LEDs life-span to have a greatly reduced quality.Another kind is a single-chip type white light LEDs.This method is to utilize the certain fluorescent material of coating on ultraviolet or the blue-light LED chip, by the conversion generation white light of fluorescent material.This scheme has been simplified the device of white light LEDs greatly, has saved cost.Wherein blue chip excites red, green emitting phosphor and ultraviolet or near ultraviolet chip to excite this dual mode of red, green, blue three primary colors fluorescent powder because color developing is good, has more vast potential for future development.Particularly ultraviolet or near ultraviolet chip excite this mode of red, green, blue three primary colors fluorescent powder owing to rich color, color developing are better, colour temperature can be prepared arbitrarily in 2500～10000K scope, and can break through the blockade of Japanese Patent, be present domestic and international research focus.
The rare earth doping fluorescent material is compared with corresponding non-rare-earth luminescent material, and its luminous efficiency and performance such as photochromic are all even better.And China is the resource and the big producing country of rare earth, has powerful resources advantage in the research of China's development rare-earth luminescent material.Fluorescent RE powder mainly is the development at monochromatic fluorescent material at present, and the mixing by each fluorescent material reaches the effect that emits white light again.The present invention adopts a kind of chemical formulation and forms two kinds of different crystals simultaneously, excite the visible light that to launch two to three kinds of different colours down by the rare earth elements europium doping in ultraviolet or near ultraviolet LED chip, can change two kinds of crystalline luminous intensities by adjusting chemical composition and maturing temperature, thereby adjust the luminescent properties of mixed light, can be used in the white light LED part.
Summary of the invention
The objective of the invention is to propose a kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof, its material composition characteristic is that its chemical constitution is (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05.Its preparation method concrete steps are as follows:
1) presses chemical constitution formula (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05 is a payment foundation, the compound dissolution that accurately takes by weighing the compound of compound, aluminium of a certain proportion of strontium and europium is in a certain amount of deionized water or acid, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, be adjusted to suitable pH value, heating also continues to stir formation colloidal sol.
2) place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain powder again.
3) with after the wet-milling of above-mentioned powder process, the oven dry,, after the cooling powder agglomates was pulverized 200 mesh sieves, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium at the high temperature kiln roasting.
The compound of said strontium is strontium nitrate, strontium chloride, strontium oxide or strontium hydroxide among the present invention, and the compound of aluminium is aluminum nitrate, aluminum chloride, aluminum oxide or aluminium hydroxide, and the compound of europium is europium nitrate, Europium trichloride, europium sesquioxide or europium hydroxide.
Adding the pH value that acid is adjusted to when forming colloidal sol among the present invention is 1～4.
Powder among the present invention is after wet-milling, oven dry, and the maturing temperature in High Temperature Furnaces Heating Apparatus is 1000～1500 ℃.
Mix in the Sr-Al-Si series composite fluorescent powder of europium at gained of the present invention, adopt a kind of chemical formulation and form two kinds of different crystals simultaneously, by the visible light that to launch two to three kinds of different colours that excites to rare earth elements europium, can change two kinds of crystalline luminous intensities by adjusting chemical composition and maturing temperature, thereby adjust the luminescent properties of mixed light, can be used in the white light LED part.
Description of drawings
Fig. 1 (64wt%) (Sr
0.99Eu
0.01Al
2Si
2O
8) (36wt%) (Sr
1.99Eu
0.01Al
2SiO
7) emmission spectrum of fluorescent material.
Fig. 2 (64wt%) (Sr
0.97Eu
0.03Al
2Si
2O
8) (36wt%) (Sr
1.97Eu
0.03Al
2SiO
7) emmission spectrum of fluorescent material.
Fig. 3 (36wt%) (Sr
0.97Eu
0.03Al
2Si
2O
8) (64wt%) (Sr
1.97Eu
0.03Al
2SiO
7) emmission spectrum of fluorescent material.
Embodiment
The present invention relates to a kind of Sr-Al-Si series composite fluorescent powder of mixing europium and preparation method thereof.The chemical constitution of this composite phosphor is: (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05.The compound dissolution that accurately takes by weighing the compound of compound, aluminium of strontium and europium in proportion mixes with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made in deionized water or acid again with by tetraethoxy.Be adjusted to suitable pH value with acid, form colloidal sol; The colloidal sol oven dry is xerogel, forms reactive powder through 550 ℃ of calcinings again, this powder is through wet-milling, and roasting at high temperature promptly gets the Sr-Al-Si series composite fluorescent powder of mixing europium.
The compound of above-mentioned said strontium is strontium nitrate, strontium chloride, strontium oxide or strontium hydroxide, and the compound of aluminium is aluminum nitrate, aluminum chloride, aluminum oxide or aluminium hydroxide, and the compound of europium is europium nitrate, Europium trichloride, europium sesquioxide or europium hydroxide; Adding the pH value that acid is adjusted to when forming colloidal sol is 1～4.With reactive powder through wet-milling, oven dry after, be 1000～1500 ℃ in the temperature of high temperature kiln roasting.
Below by embodiment, further illustrate outstanding feature of the present invention and marked improvement, only be the present invention is described and never limit the present invention.
Embodiment 1
With strontium nitrate, aluminum nitrate, tetraethoxy and europium nitrate is starting raw material, is (64wt%) (Sr by chemical constitution
0.99Eu
0.01Al
2Si
2O
8) (36wt%) (Sr
1.99Eu
0.01Al
2SiO
7), accurately take by weighing a certain proportion of strontium nitrate, aluminum nitrate and europium nitrate and be dissolved in a certain amount of deionized water, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 3, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1000 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder, and its emmission spectrum is seen Fig. 1.
Embodiment 2
With strontium chloride, aluminum chloride, tetraethoxy and Europium trichloride is starting raw material, is (64wt%) (Sr by chemical constitution
0.97Eu
0.03Al
2Si
2O
8) (36wt%) (Sr
1.97Eu
0.03Al
2SiO
7), accurately take by weighing a certain proportion of strontium chloride, aluminum chloride and Europium trichloride and be dissolved in a certain amount of deionized water, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 2, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1200 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder, and its emmission spectrum is seen Fig. 2.
Embodiment 3
With strontium oxide, aluminum oxide, tetraethoxy and europium sesquioxide is starting raw material, is (36wt%) (Sr by chemical constitution
0.97Eu
0.03Al
2Si
2O
8) (64wt%) (Sr
1.97Eu
0.03Al
2SiO
7), accurately take by weighing a certain proportion of strontium oxide, aluminum oxide and europium sesquioxide and be dissolved in a certain amount of acid, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 1, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1400 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder, and its emmission spectrum is seen Fig. 3.
Embodiment 4
With strontium nitrate, aluminum chloride, tetraethoxy and europium nitrate is starting raw material, is (44wt%) (Sr by chemical constitution
0.96Eu
0.04Al
2Si
2O
8) (56wt%) (Sr
1.96Eu
0.04Al
2SiO
7), accurately take by weighing a certain proportion of strontium nitrate, aluminum chloride and europium nitrate and be dissolved in a certain amount of deionized water, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 4, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1100 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder.
Embodiment 5
With strontium hydroxide, aluminum oxide, tetraethoxy and europium nitrate is starting raw material, is (51wt%) (Sr by chemical constitution
0.95Eu
0.05Al
2Si
2O
8) (49wt%) (Sr
1.95Eu
0.05Al
2SiO
7), accurately take by weighing a certain proportion of strontium hydroxide, aluminum oxide and europium nitrate and be dissolved in a certain amount of acid, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 2, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1250 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder.
Embodiment 6
With strontium nitrate, aluminium hydroxide, tetraethoxy and europium hydroxide is starting raw material, is (42wt%) (Sr by chemical constitution
0.98Eu
0.02Al
2Si
2O
8) (58wt%) (Sr
1.98Eu
0.02Al
2SiO
7), accurately take by weighing a certain proportion of strontium nitrate, aluminium hydroxide and europium hydroxide and be dissolved in a certain amount of acid, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, adjust pH value to 2, heating also continues to stir formation colloidal sol; Place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain reactive powder again; Through after wet-milling, drying, 1350 ℃ of roastings in High Temperature Furnaces Heating Apparatus were pulverized 200 mesh sieves with powder agglomates after the cooling, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium with above-mentioned powder.
Claims (4)
1. preparation method who mixes the Sr-Al-Si series composite fluorescent powder of europium, its chemical constitution is (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05.It is characterized in that may further comprise the steps:.
1) presses chemical constitution formula (Xwt%) (Sr
1-yEu
yAl
2Si
2O
8) (100-Xwt%) (Sr
2-yEu
yAl
2SiO
7), X=30～70 wherein, y=0.01～0.05 is a payment foundation, the compound dissolution that accurately takes by weighing the compound of compound, aluminium of a certain proportion of strontium and europium is in a certain amount of deionized water or acid, form solution, mix with the solubilized stable liquid phase that a certain proportion of deionized water, dehydrated alcohol are made into again with by tetraethoxy; Add acid then, be adjusted to suitable pH value, heating also continues to stir formation colloidal sol.
2) place baking oven to dry gained colloidal sol, form xerogel; 550 ℃ of calcinings down, obtain powder again.
3) with after the wet-milling of above-mentioned powder process, the oven dry,, after the cooling powder agglomates was pulverized 200 mesh sieves, promptly got the Sr-Al-Si series composite fluorescent powder of mixing europium at the high temperature kiln roasting.
2. a kind of preparation method who mixes the Sr-Al-Si series composite fluorescent powder of europium according to claim 1, it is characterized in that: the compound of said strontium is strontium nitrate, strontium chloride, strontium oxide or strontium hydroxide, the compound of aluminium is aluminum nitrate, aluminum chloride, aluminum oxide or aluminium hydroxide, and the compound of europium is europium nitrate, Europium trichloride, europium sesquioxide or europium hydroxide.
3. a kind of preparation method who mixes the Sr-Al-Si series composite fluorescent powder of europium according to claim 1 is characterized in that: adding the pH value that acid is adjusted to when forming colloidal sol is 1～4.
4. a kind of preparation method who mixes the Sr-Al-Si series composite fluorescent powder of europium according to claim 1 is characterized in that: powder is after wet-milling, oven dry, and the maturing temperature in High Temperature Furnaces Heating Apparatus is 1000～1500 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061166A (en) * | 2011-01-07 | 2011-05-18 | 华东师范大学 | Method for synthesizing superfine ceramic fluorescent powder |
| CN107916104A (en) * | 2017-11-16 | 2018-04-17 | 华南理工大学 | The near-infrared luminous temperature sensing nano material of tetravalence chromium doping and its preparation and application |
| JP2018095783A (en) * | 2016-12-15 | 2018-06-21 | 国立研究開発法人物質・材料研究機構 | Phosphor and light emitting device |
| CN108949172A (en) * | 2018-07-25 | 2018-12-07 | 河南大学 | A kind of fluorescent powder and preparation method thereof of tunable radiation emitting color |
| CN109825286A (en) * | 2019-03-08 | 2019-05-31 | 武汉工程大学 | A kind of aluminosilicate fluorescent powder material and preparation method thereof |
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| CN1995276A (en) * | 2006-12-18 | 2007-07-11 | 天津理工大学 | Rare-earth alumo silicate matrix fluorescent material, and preparation method |
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2010
- 2010-07-22 CN CN2010102347691A patent/CN101885966A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1995276A (en) * | 2006-12-18 | 2007-07-11 | 天津理工大学 | Rare-earth alumo silicate matrix fluorescent material, and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| WANG YINHAI ET AL.: "Synthesis of Long Afterglow Phosphor CaAl2SiO8:Eu2+,Dy3+ via Sol-Gel Techique and Its Optical Properties", 《JOURNAL OF RARE EARTHS》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061166A (en) * | 2011-01-07 | 2011-05-18 | 华东师范大学 | Method for synthesizing superfine ceramic fluorescent powder |
| CN102061166B (en) * | 2011-01-07 | 2013-08-07 | 华东师范大学 | Method for synthesizing superfine ceramic fluorescent powder |
| JP2018095783A (en) * | 2016-12-15 | 2018-06-21 | 国立研究開発法人物質・材料研究機構 | Phosphor and light emitting device |
| CN107916104A (en) * | 2017-11-16 | 2018-04-17 | 华南理工大学 | The near-infrared luminous temperature sensing nano material of tetravalence chromium doping and its preparation and application |
| CN107916104B (en) * | 2017-11-16 | 2020-08-18 | 华南理工大学 | Tetravalent chromium doped near-infrared luminescent temperature detection nano material and preparation and application thereof |
| CN108949172A (en) * | 2018-07-25 | 2018-12-07 | 河南大学 | A kind of fluorescent powder and preparation method thereof of tunable radiation emitting color |
| CN108949172B (en) * | 2018-07-25 | 2021-04-06 | 河南大学 | Fluorescent powder with adjustable luminous color and preparation method thereof |
| CN109825286A (en) * | 2019-03-08 | 2019-05-31 | 武汉工程大学 | A kind of aluminosilicate fluorescent powder material and preparation method thereof |
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Application publication date: 20101117 |