CN103571489A - Method for synthesizing small-granularity narrow-distribution green fluorescent precursor - Google Patents
Method for synthesizing small-granularity narrow-distribution green fluorescent precursor Download PDFInfo
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- CN103571489A CN103571489A CN201310550094.5A CN201310550094A CN103571489A CN 103571489 A CN103571489 A CN 103571489A CN 201310550094 A CN201310550094 A CN 201310550094A CN 103571489 A CN103571489 A CN 103571489A
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Abstract
The invention discloses a method for synthesizing small-granularity narrow-distribution green fluorescent precursor. The method comprises the following steps: mixing the following raw materials in parts by mass: 1 part of lanthanum cerium terbium mixed rare earth oxide, 1.05-1.2 parts of diammonium hydrogen phosphate, 0-0.15 parts of boric acid, 0.01-0.1 parts of lithium tetraborate and 0.01-0.2 parts of aluminum oxide and then feeding the mixture into a firing furnace; introducing hydrogen and nitrogen; controlling the hydrogen content to be 2-10 percent, the oxygen content to be less than 30 PPM, the maximum temperature to be 1,050-1,250 DEG C and the time to be 30-120 minutes; sintering to obtain the small-granularity narrow-distribution LAP (Lanthanum Phosphate) green fluorescent powder precursor. According to the method, the rare earth oxide is used as the raw material, so that the production cost is reduced; by adjusting the proportion of lanthanum oxide, cerium oxide and terbium oxide in the raw material, LAP green fluorescent powders of different compositions are synthesized; by controlling the granularity and distribution of the rare earth raw material, the granularity and distribution of the green fluorescent powder are controlled; by adding a fluxing agent, the quality of the LAP green fluorescent powder is improved.
Description
Technical field
The present invention relates to the synthetic method of the narrow distribution lanthanum-cerium-terbium phosphate green emitting phosphor of a kind of small grain size, be specifically related to the synthetic method of lanthanum-cerium-terbium phosphate green emitting phosphor for a kind of electricity-saving lamp.
Background technology
Lanthanum-cerium-terbium phosphate green emitting phosphor for electricity-saving lamp (being called for short LAP green emitting phosphor), it is manufactured process Zhong Shicong raw material manufacturer place and buys lanthanum-cerium-terbium phosphate presoma powder, solubility promoter mixing different in interpolation shake up, sintering at suitable temperature, pass through again treatment process, be prepared into lanthanum-cerium-terbium phosphate green emitting phosphor.Electricity-saving lamp lamp manufacturing process, in order to reduce fluorescent material usage quantity, requires LAP green emitting phosphor to have less medium particle diameter, the distribution of narrower particle diameter at present.In fluorescent material preparation process, although can pass through sintering, the particle diameter of the technology controlling and process LAP green emitting phosphors such as ball-milling processing.But because the composition of lanthanum-cerium-terbium phosphate presoma and the distribution of medium particle diameter and particle diameter are determined, by processes such as sintering, ball-milling processing, to the distribution of the composition of LAP green emitting phosphor, medium particle diameter scope, granularity, adjust limited.
Summary of the invention
The object of the present invention is to provide the method for the narrow distribution green emitting phosphor of a kind of synthetic small grain size presoma, it uses monomer rare earth oxide as starting material, by regulating the ratio of lanthanum trioxide, cerium oxide, terbium sesquioxide in starting material, the synthetic LAP green emitting phosphors with different compositions; By the control to rare earth oxide starting material granularity and distribution, control lanthanum-cerium-terbium phosphate green emitting phosphor granularity and distribution; By the fusing assistant adding is improved, improve the quality of LAP green emitting phosphor.
In order to reach above-mentioned purpose, the technical solution used in the present invention is:
First starting material are mixed by the mass ratio of following material: lanthanum cerium terbium mixed rare-earth oxide 1, lanthanum trioxide, cerium oxide, terbium sesquioxide mix according to certain ratio, ratio can be adjusted as required, Secondary ammonium phosphate 1.05～1.2, boric acid 0～0.15, lithium tetraborate 0.01～0.1, aluminum oxide 0.01～0.2; Mix laggard firing furnace sintering, logical hydrogen and nitrogen mixture body in firing furnace, the hydrogen richness in control firing furnace is between 2%～10%, and oxygen level is less than 30PPM, control the highest sintering temperature of firing furnace between 1050 ℃～1250 ℃, top temperature sintering time is 30～120 minutes; Sintering fluorescent material is out the narrow distribution LAP of small grain size green emitting phosphor presoma.
Adopt after such scheme, the present invention adopts monomer rare earth oxide as starting material, according to the finished product, requires to adjust flexibly raw-material proportioning, synthesizes and has the different LAP green emitting phosphors that form.By controlling raw-material medium particle diameter and the size-grade distribution such as lanthanum trioxide, cerium oxide, terbium sesquioxide, control particle diameter and the distribution of LAP green emitting phosphor.Fluorescent material forms and granularity control is also more prone to.The sintering process of the precursor synthesis process of LAP green emitting phosphor and fluorescent material is combined to a step to be processed, saved the process of synthetic lanthanum-cerium-terbium phosphate presoma, saved great amount of cost, and by adding different fusing assistants, with the control to firing process, product is improved, improve on the whole LAP green emitting phosphor quality.
Embodiment
Embodiment 1: by D50, be first 2.0-4.5 μ m lanthanum trioxide, cerium oxide, the mixed oxide of terbium sesquioxide, primary ammonium phosphate, lithium tetraborate, aluminum oxide was by the mass ratio of material 1: 1.05: 0.04: 0.05 mixes, put into firing furnace, controlling firing furnace top temperature is 1200 ℃, under nitrogen protection atmosphere condition, hydrogen content is 7.5%, oxygen level is less than 30PPM, highest temperature soaking time is 80 minutes, sintering sintered compact D50 is out 3.5-6.5 μ m, after treatment, the D50 of final LAP green emitting phosphor is 3.0-5.5 μ m, 1 μ m～10 μ m containing ratio is 95%.
Embodiment 2: by D50, be first 2.0-4.5 μ m lanthanum trioxide, cerium oxide, the mixed oxide of terbium sesquioxide, primary ammonium phosphate, boric acid, lithium tetraborate, aluminum oxide was by the mass ratio of material 1: 1.1: 0.05: mix at 0.06: 0.08, put into firing furnace, controlling firing furnace top temperature is 1160 ℃, under nitrogen protection atmosphere condition, hydrogen content is 7.5%, oxygen level is less than 30PPM, highest temperature soaking time is 80 minutes, sintering sintered compact D50 is out that D50 is 3.0-4.5 μ m, after treatment, the 2.5-4.5 μ m of final LAP green emitting phosphor, 1 μ m～8 μ m containing ratio is 95%.
Embodiment 3: by D50, be first 2.0-3.5 μ m lanthanum trioxide, cerium oxide, the mixed oxide of terbium sesquioxide, primary ammonium phosphate, boric acid, lithium tetraborate, aluminum oxide was by the mass ratio of material 1: 1.15: 0.1: mix at 0.06: 0.15, put into firing furnace, controlling firing furnace top temperature is 1100 ℃, under nitrogen protection atmosphere condition, hydrogen content is 7.5%, oxygen level is less than 30PPM, highest temperature soaking time is 60 minutes, sintering sintered compact D50 is out that D50 is 2.5-4.0 μ m, after treatment, the 2.0-3.5 μ m of final LAP green emitting phosphor, 1 μ m～8 μ m containing ratio is 95%.
Embodiment 4: by D50, be first 2.0-3.5 μ m lanthanum trioxide, cerium oxide, the mixed oxide of terbium sesquioxide, primary ammonium phosphate, boric acid, lithium tetraborate, aluminum oxide was by the mass ratio of material 1: 1.2: 0.15: mix at 0.06: 0.2, put into firing furnace, controlling firing furnace top temperature is 1100 ℃, under nitrogen protection atmosphere condition, hydrogen content is 7.5%, oxygen level is less than 30PPM, highest temperature soaking time is 60 minutes, sintering sintered compact D50 is out that D50 is 2.0-4.0 μ m, after treatment, the 1.5-3.0 μ m of final LAP green emitting phosphor, 1 μ m～8 μ m containing ratio is 95%.
Claims (1)
1. the method for the narrow distribution green emitting phosphor of a synthetic small grain size presoma, it is characterized in that: first starting material are mixed by the mass ratio of following material: lanthanum cerium terbium mixed rare-earth oxide 1, lanthanum trioxide, cerium oxide, terbium sesquioxide mix according to certain ratio, Secondary ammonium phosphate 1.05～1.2, boric acid 0～0.15, lithium tetraborate 0.01～0.1, aluminum oxide 0.01～0.2; Mix laggard firing furnace sintering, logical hydrogen and nitrogen mixture body in firing furnace, the hydrogen richness in control firing furnace is between 2%～10%, and oxygen level is less than 30PPM, control the highest sintering temperature of firing furnace between 1050 ℃～1250 ℃, top temperature sintering time is 30～120 minutes; Sintering fluorescent material is out the narrow distribution LAP of small grain size green emitting phosphor presoma.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178164A (en) * | 2014-07-15 | 2014-12-03 | 宜兴新威利成稀土有限公司 | Method for preparing small-granularity cerium terbium lanthanum phosphate rare earth product with high luminous efficiency |
| CN106381141A (en) * | 2016-08-31 | 2017-02-08 | 广州珠江光电新材料有限公司 | Boron-containing aluminosilicate long afterglow phosphor and preparation method thereof |
| CN109913216A (en) * | 2019-03-05 | 2019-06-21 | 广州珠江光电新材料有限公司 | A kind of preparation method of fluorescent powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351864A (en) * | 2013-07-01 | 2013-10-16 | 南昌大学 | Preparation method of small size and high brightness lanthanum phosphate activated by cerium and terbium, green phosphor |
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2013
- 2013-11-08 CN CN201310550094.5A patent/CN103571489A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351864A (en) * | 2013-07-01 | 2013-10-16 | 南昌大学 | Preparation method of small size and high brightness lanthanum phosphate activated by cerium and terbium, green phosphor |
Non-Patent Citations (1)
| Title |
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| 王旻: "钨酸钙_磷酸镧铈铽_硅酸锌锰的微波热效应法合成及其光致发光性能研究", 《中山大学研究生学刊自然科学版》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178164A (en) * | 2014-07-15 | 2014-12-03 | 宜兴新威利成稀土有限公司 | Method for preparing small-granularity cerium terbium lanthanum phosphate rare earth product with high luminous efficiency |
| CN106381141A (en) * | 2016-08-31 | 2017-02-08 | 广州珠江光电新材料有限公司 | Boron-containing aluminosilicate long afterglow phosphor and preparation method thereof |
| CN109913216A (en) * | 2019-03-05 | 2019-06-21 | 广州珠江光电新材料有限公司 | A kind of preparation method of fluorescent powder |
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Application publication date: 20140212 |