CN102373060A - Aluminate green fluorescent powder with core-shell structure and preparation method thereof - Google Patents

Aluminate green fluorescent powder with core-shell structure and preparation method thereof Download PDF

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CN102373060A
CN102373060A CN2011103183301A CN201110318330A CN102373060A CN 102373060 A CN102373060 A CN 102373060A CN 2011103183301 A CN2011103183301 A CN 2011103183301A CN 201110318330 A CN201110318330 A CN 201110318330A CN 102373060 A CN102373060 A CN 102373060A
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fluorescent powder
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green fluorescent
aluminate green
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CN102373060B (en
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陶颖
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Jiangmen Kanhoo Industry Co ltd
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Abstract

The invention discloses aluminate green fluorescent powder with a core-shell structure and a preparation method thereof. The fluorescent powder comprises an inner core and a shell, wherein the particle diameter of the inner core is 3-8 mum; the powder is low-Tb-content aluminate green fluorescent powder; and the outer shell consists of oxides of Ce and Tb. The formula of the powder is (CexTbM@CeyTbn)MgAl11O19, wherein (x+y) is more than or equal to 0.6 and is less than or equal to 0.8, (m+n) is more than or equal to 0 and is less than or equal to 0.4, and (m:n) is more than or equal to 1 and is less than or equal to 4. The preparation method comprises the following steps of: preparing the inner core of the aluminate green powder with low terbium content; precipitating cerium and terbium onto the inner core; and reacting in the reducing atmosphere to obtain the aluminate green fluorescent powder with the core-shell structure finally. In the invention, lattices of core and shell materials are highly matched, so that the surface defect of fluorescent powder particles is overcome, terbium elements serving as activating agents can be well distributed on the surface of the fluorescent powder, the utilization ratio of an expensive rare-earth activating agent is increased, the surface of the fluorescent powder is decorated, the fluorescence powder has more stable performance, and the fluorescent efficiency is greatly increased; and the preparation method is suitable for preparing high-performance aluminate green powder.

Description

Aluminate green fluorescent powder of a kind of nucleocapsid structure and preparation method thereof
Technical field
The present invention relates to a kind of power saving fluorescent lamp and use the three primary colours green emitting phosphor, particularly a kind of aluminate green fluorescent powder of nucleocapsid structure.
Background technology
With cerium, the coactivated rare earth aluminate (Ce of terbium 0.67Tb 0.33) MgAl 11O 19(being called for short CAT) is a kind of material that extensively applies to the green light in the luminescent lamp.At CeMgAl 11O 19: among the Tb, taken place from Ce 3+→ Tb 3+The high efficiency energy transmission, thereby obtain this green-emitting phosphor of CAT, be a kind of cerium, the coactivated fluorescent material of terbium.In the industrial production, the aluminate green powder is mainly synthetic through high temperature solid-state method, and the Tb element is distributed in the whole fluorescent material, and the Tb element of powder surface enrichment is less, and utilization ratio is lower.At present, fluorescent material has great specific surface area, makes that its surface reconstruction and surface imperfection are serious; Thereby caused the luminous efficiency of fluorescent material low; And the rare earth material price rises sharply, and the heavy rare earths price occupies high, and wherein terbium element price is high; Improve the terbium utilization ratio, it is particularly important to prepare high performance aluminate fluorescent powder.
Patent EP0766285B1, US5879586 have introduced several kinds of aluminate fluorescent powders that the high temperature solid-state method synthetic is not fluorine-containing, terbium activated (Ce wherein 0.67Tb 0.33) MgAl 11O 19(CAT), its synthesis temperature is very high, and high temperature causes the crystalline structure of green powder relatively poor, and luminescent properties is influenced.At present, part document and patent report the have been arranged advantage of nucleocapsid structure material, there be limited evidence currently of has the preparation and the property research thereof of the aluminate green powder of the nucleocapsid structure of reporting for work.
CN101701153A has reported a kind of preparation method of aluminate green phosphor with low content of terbium, and the preparation earlier of this method does not contain the powder of terbium, redeposition terbium element, and then powder pyroreaction under reducing atmosphere obtained aluminate green fluorescent powder, activation process is by interior Ce 3+→ outer Tb 3+Realize transmission ofenergy, use the aluminate green powder terbium content of this method preparation to reduce by 10～40%, but the luminescent properties of fluorescent material reduces by 1～5%.
With regard to the market requirement, the product of high-performance and low-cost has more the market competitiveness.This experiment is through improving formula for a product, and the adjustment production technique prepares high performance fluorescent material.
Summary of the invention
The object of the present invention is to provide aluminate green fluorescent powder of a kind of nucleocapsid structure and preparation method thereof.
The technical scheme that the present invention taked is:
A kind of aluminate green fluorescent powder of nucleocapsid structure comprises kernel and shell, and the particle diameter of kernel is the low Tb content aluminate green fluorescent powder of 3 ~ 8 μ m, and shell is the oxide compound of Ce and Tb, and its composition formula is (Ce xTb mCe yTb n) MgAl 11O 19, wherein, 0.6≤x+y≤0.8,0≤m+n≤0.4,1≤m:n≤4.
The preparation method of the aluminate green fluorescent powder of above-mentioned nucleocapsid structure comprises the steps:
1) use high temperature solid-state method to prepare core A;
2) will contain Tb, Ce water-soluble salt and core A mixing in the aqueous solution, and obtain mixed solution, the pH that uses basic soln adjusting mixed solution makes Tb, Ce ion precipitation on the surface of core A to alkalescence, washing, and drying obtains powder B;
3) powder B is placed crucible, calcination in the reducing atmosphere after the cooling, is ground and is promptly obtained fluorescent material.
Preferably, contain Tb, Ce water-soluble salt and be its nitrate salt, villaumite.
Preferably, calcination temperature is 1200～1300 ℃.
Preferably, calcination time is 3～5h.
Preferably, use basic soln to regulate pH to 8～9 of mixed solution.
Preferably, basic soln is at least a in ammoniacal liquor, sal volatile, ammonium bicarbonate soln, the urea soln.
Preferably, high temperature solid-state method prepares core A and comprises the steps: the chemical constitution according to core A, takes by weighing raw material, adds fusing assistant, 1450～1550 ℃ of sintering, fragmentation.
Preferably, fusing assistant is BaF 2, BaCl 2, MgCl 2, MgF 2, H 3BO 3In at least a.
Preferably, the agglomerating time is 3～5h.
The invention has the beneficial effects as follows:
The present invention is through preparing the kernel of low terbium content earlier, and particle diameter is 3 ~ 8 μ m, coats cerium, terbium element again; Form nucleocapsid structure,, improved the surface imperfection of fluorescent powder grain owing to the matched of core-shell material lattice; Not only make activator terbium element be distributed in phosphor surface preferably, improved rare-earth activated dose expensive rate of utilization, also play the effect of modifying phosphor surface; Make that the fluorescent material performance is more stable; Transmission ofenergy neither be from inside to outside single, and luminous efficiency improves greatly, is suitable for preparing high-performance aluminate green powder.The inventive method technology is simple, and mild condition is applicable to large-scale industrialization production.
Description of drawings
Fig. 1 is the xps figure of Comparative Examples 1 green emitting phosphor;
Fig. 2 is the xps figure of embodiment 2 green emitting phosphors.
Embodiment
Further specify the present invention below in conjunction with embodiment.
The structure of following examples green emitting phosphor all is expressed as: kernel is formed shell and is formed.
Embodiment 1
（Ce 0.223Tb 0.11Ce 0.447Tb 0.22）MgAl 11O 19
Cerium oxide 1.919g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 1.028g, boric acid 0.07g, Sellaite 0.1 g are ground in mortar in the corundum crucible of packing into behind the 1.5h at 1450 ℃ of following calcination 3h; Naturally cool to room temperature; Grind 15min, both got core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 73.3 mL and 0.2mol/L Ce (NO 3) 3 . 6H 2O solution 111.5mL stirs and to add 20% urea behind the 15min and regulate pH to 8.0, stirs 30min, leaves standstill 1h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1280 ℃ of reaction 4h, cool to room temperature grinds 15min and gets green emitting phosphor.
Embodiment 2
（Ce 0.168Tb 0.0825Ce 0.502Tb 0.248）MgAl 11O 19
Cerium oxide 1.446g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 0.771g, boric acid 0.06g, bariumchloride 0.1g are ground in mortar in the corundum crucible of packing into behind the 1.5h at 1520 ℃ of following calcination 3h; Naturally cool to room temperature; Grind 15min, both got core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 82.5 mL and 0.2 mol/L Ce (NO 3) 3 . 6H 2O solution 126.0 mL stir and to add 30% ammoniacal liquor behind the 15min and regulate pH to 8.5, stir 30min, leave standstill 1h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1300 ℃ of reaction 3h, cool to room temperature grinds 15min and gets green emitting phosphor.
Embodiment 3
（Ce 0.134Tb 0.066Ce 0.536Tb 0.264）MgAl 11O 19
Cerium oxide 1.153g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 0.617g, boric acid 0.16g are ground in mortar in the corundum crucible of packing into behind the 1.5h at 1480 ℃ of following calcination 5h, naturally cool to room temperature, grind 15min, both core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 88.0 mL and 0.2mol/L Ce (NO 3) 3 . 6H 2O solution 134m.0 mL stirs and to add 30% ammoniacal liquor behind the 15min and regulate pH to 8.2, stirs 30min, leaves standstill 2h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1250 ℃ of reaction 3h, cool to room temperature grinds 15min and gets green emitting phosphor.
Embodiment 4
（Ce 0.447Tb 0.22Ce 0.223Tb 0.11）MgAl 11O 19
With cerium oxide 3.847g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 2.056g, boric acid 0.08g, magnesium chloride 0.1 g; In mortar, grind in the corundum crucible of packing into behind the 1.5h at 1480 ℃ of following calcination 5h; Naturally cool to room temperature, grind 15min, both got core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 36.6 mL and 0.2mol/L Ce (NO 3) 3 . 6H 2O solution 55.9mL stirs and to add 20% bicarbonate of ammonia behind the 15min and regulate pH to 9.0, stirs 30min, leaves standstill 3h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1230 ℃ of reaction 3h, cool to room temperature grinds 15min and gets green emitting phosphor.
Embodiment 5
（Ce 0.503Tb 0.248Ce 0.167Tb 0.0824）MgAl 11O 19
Cerium oxide 4.329g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 2.318g, boric acid 0.18g barium fluoride 0.18g are ground in mortar in the corundum crucible of packing into behind the 1.5h at 1550 ℃ of following calcination 3h; Naturally cool to room temperature; Grind 15min, both got core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 27.6 mL and 0.2mol/L Ce (NO 3) 3 . 6H 2O solution 41.9mL stirs and to add 30% ammoniacal liquor behind the 15min and regulate pH to 8.5, stirs 30min, leaves standstill 1h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1300 ℃ of reaction 3h, cool to room temperature grinds 15min and gets green emitting phosphor.
Embodiment 6
（Ce 0.536Tb 0.264Ce 0.134Tb 0.066）MgAl 11O 19
Grind with cerium oxide 4.612g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 2.467g, boric acid 0.07g, in mortar in the corundum crucible of packing into behind the 1.5h at 1500 ℃ of following calcination 3h, naturally cool to room temperature, grind 15min, both core A.
A is scattered in (quality of A and the volume ratio of pure water are 2:1) in the pure water, under agitation condition, adds 0.15 mol/L TbCl 3Solution (being dissolved in nitric acid) 22.1mL and 0.2mol/L Ce (NO 3) 3 . 6H 2O solution 33.5mL stirs and to add 25% volatile salt behind the 15min and regulate pH to 8.6, stirs 30min, leaves standstill 1h, pure water wash to pH for neutral, suction filtration, 150 ℃ of oven dry, the powder after the oven dry is crossed 80 eye mesh screens, obtains powder B.
Powder B is packed in the crucible, at N 295%+H 2Under 10% reducing atmosphere, 1200 ℃ of reaction 5h, cool to room temperature grinds 15min and gets green emitting phosphor.
Confirming of above reaction parameter all is the optimum experimental conditions under the same recipe that condition optimizing obtains.Its luminescent properties of nucleocapsid structure aluminate green powder by preferred reaction parameter preparation is the optimum of this prescription.
Comparative Examples 1
（Ce 0.67）MgAl 11O 19?：Tb 0.33
Cerium oxide 5.766g, Natural manganese dioxide 2.015g, aluminum oxide 28.039g, terbium sesquioxide 3.084g, boric acid 0.194g are ground in mortar in the corundum crucible of packing into behind the 1.5h at 1550 ℃ of following calcination 6h; Naturally cool to room temperature; Green powder work in-process are ground 15min; Then powder is packed in the corundum crucible, at N 295%+H 21400 ℃ of reaction 6h take out after naturally cooling to room temperature in 5% the reducing atmosphere, the green powder of gained is ground 15min promptly get green emitting phosphor.
The difference of above-mentioned each embodiment nucleocapsid terbium constituent content ratio is to fluorescent material Effect on Performance such as table 1.
Figure 2011103183301100002DEST_PATH_IMAGE001
Can know that by above data analysis the aluminate green powder brightness of nucleocapsid structure generally improves among the present invention.Under the close situation of terbium content,, can obtain better luminous intensity through regulating the ratio of nucleocapsid Ce and Tb.When kernel terbium content hanged down with the shell terbium, fluorescent material brightness improved the situation that is higher than shell greater than kernel terbium content; When terbium content is examined: brightness improved 11% when shell was 1:3.The green powder brightness of this patent synthetic has improved 17% and 15.5% than the aluminate green powder of the non-nucleocapsid structure of CN101701153A report under equal experiment condition, and the green powder of the luminous performance of preparation can satisfy the demand of high light efficiency power saving fluorescent lamp.
Adopt photoelectron spectrograph (xps) that embodiment 2 is analyzed with Comparative Examples 1 green emitting phosphor particulate top layer constituent content.Fig. 1 is the xps figure of Comparative Examples 1 green emitting phosphor, and Fig. 2 is the xps figure of embodiment 2 green emitting phosphors.Can be known that by figure the Tb of Fig. 2, Ce constituent content are than the height of Fig. 1, activator can well be enriched in the shell structure in the visible fluorescent powder with core-shell structure of the present invention, has improved rare-earth activated dose expensive rate of utilization.

Claims (10)

1. the aluminate green fluorescent powder of a nucleocapsid structure comprises kernel and shell, and the particle diameter of kernel is the low Tb content aluminate green fluorescent powder of 3 ~ 8 μ m, and shell is the oxide compound of Ce and Tb, and its composition formula is (Ce xTb mCe yTb n) MgAl 11O 19, wherein, 0.6≤x+y≤0.8,0≤m+n≤0.4,1≤m:n≤4.
2. the preparation method of the aluminate green fluorescent powder of the described nucleocapsid structure of claim 1 comprises the steps:
1) use high temperature solid-state method to prepare core A;
2) will contain Tb, Ce water-soluble salt and core A mixing in the aqueous solution, and obtain mixed solution, the pH that uses basic soln adjusting mixed solution makes Tb, Ce ion precipitation on the surface of core A to alkalescence, washing, and drying obtains powder B;
3) powder B is placed crucible, calcination in the reducing atmosphere after the cooling, is ground and is promptly obtained fluorescent material.
3. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 2 is characterized in that: contain Tb, the Ce water-soluble salt is its nitrate salt, villaumite.
4. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 2, it is characterized in that: calcination temperature is 1200～1300 ℃.
5. according to the aluminate green fluorescent powder preparation method of claim 2 or 4 described nucleocapsid structures, it is characterized in that: calcination time is 3～5h.
6. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 2 is characterized in that: use basic soln to regulate pH to 8～9 of mixed solution.
7. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 2 is characterized in that: basic soln is at least a in ammoniacal liquor, sal volatile, ammonium bicarbonate soln, the urea soln.
8. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 2; It is characterized in that: high temperature solid-state method prepares core A and comprises the steps: the chemical constitution according to core A, takes by weighing raw material, adds fusing assistant; 1450～1550 ℃ of sintering, fragmentation.
9. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 8, it is characterized in that: fusing assistant is BaF 2, BaCl 2, MgCl 2, MgF 2, H 3BO 3In at least a.
10. the aluminate green fluorescent powder preparation method of nucleocapsid structure according to claim 8, it is characterized in that: the agglomerating time is 3～5h.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102888224A (en) * 2012-09-07 2013-01-23 彩虹集团电子股份有限公司 Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor
CN106800410A (en) * 2017-01-13 2017-06-06 中国计量大学 A kind of yttria-base laser ceramics of Yb sensitizations and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0674688B1 (en) * 1992-12-18 1999-03-31 E.I. Du Pont De Nemours And Company Luminescent materials prepared by coating luminescent compositions onto substrate particles
CN101701153A (en) * 2009-11-17 2010-05-05 江门市科恒实业股份有限公司 Method for preparing aluminate green phosphor with low content of terbium
CN102051171A (en) * 2010-11-19 2011-05-11 江门市科恒实业股份有限公司 Method for preparing low-europium red fluorescent powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0674688B1 (en) * 1992-12-18 1999-03-31 E.I. Du Pont De Nemours And Company Luminescent materials prepared by coating luminescent compositions onto substrate particles
CN101701153A (en) * 2009-11-17 2010-05-05 江门市科恒实业股份有限公司 Method for preparing aluminate green phosphor with low content of terbium
CN102051171A (en) * 2010-11-19 2011-05-11 江门市科恒实业股份有限公司 Method for preparing low-europium red fluorescent powder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102888224A (en) * 2012-09-07 2013-01-23 彩虹集团电子股份有限公司 Method for preparing ultraviolet excited or vacuum ultraviolet excited green emitting phosphor
CN106800410A (en) * 2017-01-13 2017-06-06 中国计量大学 A kind of yttria-base laser ceramics of Yb sensitizations and preparation method thereof
CN106800410B (en) * 2017-01-13 2020-01-24 中国计量大学 Yb-sensitized yttrium oxide-based laser ceramic and preparation method thereof

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