CN1085719C - Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp - Google Patents
Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp Download PDFInfo
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- CN1085719C CN1085719C CN97121937A CN97121937A CN1085719C CN 1085719 C CN1085719 C CN 1085719C CN 97121937 A CN97121937 A CN 97121937A CN 97121937 A CN97121937 A CN 97121937A CN 1085719 C CN1085719 C CN 1085719C
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- dysprosium
- fluorescent powder
- oxide
- ions
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Abstract
The present invention belongs to a preparation method for dysprosium and plumbum codoped fluorescent powder for high-voltage mercury lamps. Vanadium yttrium phosphate is used as a substrate material, and dysprosium ions are used as active ions by the present invention. The fluorescent powder is prepared by sintering the raw materials at high temperature in the air. The luminescence property of the fluorescent powder can be obviously improved by partially replacing positive yttrium ions in vanadium yttrium phosphate activated by dysprosium by plumbum ions, and the luminous intensity of the fluorescent powder is improved to a larger extent. Because europium oxide which has the disadvantages of small quantity and high price is replaced by dysprosium oxide which has the advantages of large quantity and low price in China, the production cost of the fluorescent powder of the present invention can be reduced, and the application approach of dysprosium resources is widened.
Description
The invention belongs to dysprosium, the plumbous preparation method who mixes the high-pressure mercury lamp phosphor altogether.
High voltage mercury lamp is a kind of lighting that is widely used at present, is mainly used in the illumination in road and other place.The principle of work of this kind light fixture is that the ultraviolet ray excited fluorescent material that is applied to the glass lamp housing inboard based on 365nm that utilizes the high-pressure mercury vapor discharge to be produced produces as seen luminous.Employed fluorescent RE powder mainly is europkium-activated vanadic acid yttrium and vanadium yttrium phosphate in high voltage mercury lamp at present.English Patent Brit.1,135,304 (C1.09k), General Electric Company discloses and has been entitled as " preparation that europium activates the vanadic acid yttrium "; It is that the feedstock production europium activates vanadic acid yttrium phosphor powder that this method has been reported with yttrium oxide, europium sesquioxide and Vanadium Pentoxide in FLAKES.United States Patent (USP) U.S.3,647,706 (C1.301-4p; C09k), people such as Lagos discloses and has been entitled as " preparation that europium activates vanadium yttrium phosphate fluorescent material "; It is that raw material prepares the method that europium activates lamp phosphor in 1200-1400 ℃ of calcination that this patent has been reported with yttrium oxide, europium sesquioxide, primary ammonium phosphate and ammonium vanadate.Though above-mentioned two kinds of fluorescent material all have preferable performance, owing to will use content rareness in rare-earth mineral, expensive europium sesquioxide and make the cost of this type of fluorescent material higher.The lamp phosphor that with the dysprosium is active ions also has report.United States Patent (USP) U.S.3 for example, 501,412 (C1.252-301.4; C 09 k), R.Ropp discloses the patent that is entitled as " activated by dysprosium rare-earth vanadate fluorescent material "; This method is a feedstock production geseous discharge lamp phosphor with rare earth oxide and Vanadium Pentoxide in FLAKES.Japanese Patent JP 02 28,283,[90 28,283] (C1.C09K11/83), K.Nakagawa discloses the patent that is entitled as " the white luminous fluorescent material of rare earth use for discharge lamp "; The described fluorescent material of this patent consist of Y
1-xDy
xV
1-yP
yO
4
The present invention finds by a large amount of experiment screening, partly replaces the luminescent properties that yttrium positively charged ion in the activated by dysprosium vanadium yttrium phosphate can significantly improve fluorescent material with lead ion, improves the luminous intensity of fluorescent material largely; Compare with not leaded ionic activated by dysprosium fluorescent material, the luminous intensity of plumbiferous corresponding fluorescent material can improve about 20%.Owing to used the europium sesquioxide that has replaced few amount and high price at the big inexpensive dysprosium oxide of China's amount,, also expanded new approach for the development and use of dysprosium oxide so the present invention can reduce the production cost of fluorescent material.
The objective of the invention is the mode of mixing altogether with dysprosium oxide, plumbous oxide, the high temperature sintering in air such as yttrium oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate that is equipped with respective numbers prepares the high-pressure mercury lamp phosphor.
The present invention at high temperature prepares the vanadium yttrium phosphate matrix compounds according to the principle of high temperature solid state reaction; The method that adopts positively charged ion to replace is introduced the case of ruthenium ion in the vanadium yttrium phosphate matrix by solid state reaction with dysprosium and lead ion under the condition of high temperature, thereby prepares dysprosium, lead is mixed fluorescent material altogether.The ultraviolet ray based on 365nm that high-pressure mercury vapor discharge is produced is at first absorbed by the anionic group in the material, and then the mode of intensity of activation by the non-radiative energy transmission is transported to the dysprosium ion that occupies the ruthenium ion case and makes it be in excited state and produce white luminous.
The present invention presses following mixed with yttrium oxide, dysprosium oxide, plumbous oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate:
Y
1-x-y(VO
4)
1-a(PO
4)
a∶Dy
x，Dy
x
Wherein: 0.005≤x≤0.02,0.005≤y≤0.02,0.10≤a≤0.80 mixture mixes the back in 400 ℃ of calcinations 4 hours in air through grinding, take out after the grinding again in 1200-1400 ℃ in air calcination 4-8 hour.Product is white powder fluorescent material after grinding, wash, drying.
Embodiment provided by the invention is as follows:
1. with 55.32 gram yttrium oxide, 22.74 gram Vanadium Pentoxide in FLAKESs, 28.76 gram primary ammonium phosphates, 0.93 gram dysprosium oxide and 1.12 gram plumbous oxide mixings, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1300 ℃ of calcinations 8 hours; The product porphyrize after washing, oven dry promptly get and consist of Y
0.98(VO
4)
0.10(PO
4)
0.10: Dy
0.01, Pb
0.01White fluorescent powder.Coated the inside and outside town of 250W high voltage mercury lamp with this fluorescent material, luminous efficiency is respectively 19.171m/w and 48.80 1m/w.
2. with 1.117 gram yttrium oxide, 0.728 gram Vanadium Pentoxide in FLAKES, 0.230 gram primary ammonium phosphate, 0.009 gram dysprosium oxide and 0.011 gram plumbous oxide mixing, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1200 ℃ of calcinations 6 hours; The product porphyrize after washing, oven dry promptly get and consist of Y
0.59(VO
4)
0.80(PO
4)
0.20: Dy
0.005, Pb
0.005White fluorescent powder.This fluorescent material all produces strong white luminous under the exciting of 365nm and 254nm mercury line.
3. with 1.095 gram yttrium oxide, 0.181 gram Vanadium Pentoxide in FLAKES, 0.923 gram primary ammonium phosphate, 0.028 gram dysprosium oxide and 0.034 gram plumbous oxide mixing, porphyrize; Mixture was in 400 ℃ of calcinations 4 hours; Take out behind the porphyrize again in 1400 ℃ of calcinations 4 hours; The product porphyrize after washing, oven dry promptly get and consist of Y
0.97(VO
4)
0.20(PO
4)
0.80: Dy
0.015, Pb
0.015White fluorescent powder.This fluorescent material all produces strong white luminous under the exciting of 365nm and 254nm mercury line.
Claims (1)
1. a dysprosium, the plumbous preparation method who mixes the high-pressure mercury lamp phosphor altogether is characterized in that yttrium oxide, dysprosium oxide, plumbous oxide, Vanadium Pentoxide in FLAKES and primary ammonium phosphate by following mixed:
Y
1-x-y(VO
4)
1-a(PO
4)
a∶Dy
x，Pb
y
Wherein: 0.005≤x≤0.02,0.005≤y≤0.02,0.10≤a≤0.80 mixture mixes the back in 400 ℃ of calcinations 4 hours in air through grinding, take out after the grinding again in 1200-1400 ℃ in air calcination 4-8 hour.Product is white powder fluorescent material after grinding, wash, drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121937A CN1085719C (en) | 1997-11-21 | 1997-11-21 | Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121937A CN1085719C (en) | 1997-11-21 | 1997-11-21 | Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1218084A CN1218084A (en) | 1999-06-02 |
| CN1085719C true CN1085719C (en) | 2002-05-29 |
Family
ID=5176556
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121937A Expired - Fee Related CN1085719C (en) | 1997-11-21 | 1997-11-21 | Preparation of fluorescent powder for dysprosium and lead dosed high voltage mercury lamp |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1085719C (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100655894B1 (en) | 2004-05-06 | 2006-12-08 | 서울옵토디바이스주식회사 | Light Emitting Device |
| KR100658700B1 (en) | 2004-05-13 | 2006-12-15 | 서울옵토디바이스주식회사 | Light emitting device with RGB diodes and phosphor converter |
| KR100665299B1 (en) | 2004-06-10 | 2007-01-04 | 서울반도체 주식회사 | Luminescent material |
| KR100665298B1 (en) | 2004-06-10 | 2007-01-04 | 서울반도체 주식회사 | Light emitting device |
| US8308980B2 (en) | 2004-06-10 | 2012-11-13 | Seoul Semiconductor Co., Ltd. | Light emitting device |
| KR101258397B1 (en) | 2005-11-11 | 2013-04-30 | 서울반도체 주식회사 | Copper-Alkaline-Earth-Silicate mixed crystal phosphors |
| KR101055772B1 (en) | 2005-12-15 | 2011-08-11 | 서울반도체 주식회사 | Light emitting device |
| KR100875443B1 (en) | 2006-03-31 | 2008-12-23 | 서울반도체 주식회사 | Light emitting device |
| RU2467051C2 (en) | 2007-08-22 | 2012-11-20 | Сеул Семикондактор Ко., Лтд. | Luminophores based on nonstoichiometric tetragonal silicates of copper and alkali-earth metal and method for production thereof |
| KR101055769B1 (en) | 2007-08-28 | 2011-08-11 | 서울반도체 주식회사 | Light-emitting device adopting non-stoichiometric tetra-alkaline earth silicate phosphor |
| DE102009030205A1 (en) | 2009-06-24 | 2010-12-30 | Litec-Lp Gmbh | Luminescent substance with europium-doped silicate luminophore, useful in LED, comprises alkaline-, rare-earth metal orthosilicate, and solid solution in form of mixed phases arranged between alkaline- and rare-earth metal oxyorthosilicate |
| KR101055762B1 (en) | 2009-09-01 | 2011-08-11 | 서울반도체 주식회사 | Light-emitting device employing a light-emitting material having an oxyosilicate light emitter |
| CN104861977A (en) * | 2015-05-25 | 2015-08-26 | 湖南爱德光电新材料有限公司 | White vanadium phosphate phosphor and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146478A (en) * | 1995-06-28 | 1997-04-02 | 罗纳·布朗克化学公司 | Compound based rare-earth phosphate used as luminous material in plasma system |
-
1997
- 1997-11-21 CN CN97121937A patent/CN1085719C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146478A (en) * | 1995-06-28 | 1997-04-02 | 罗纳·布朗克化学公司 | Compound based rare-earth phosphate used as luminous material in plasma system |
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| Publication number | Publication date |
|---|---|
| CN1218084A (en) | 1999-06-02 |
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