CN103351864A - Preparation method of small size and high brightness lanthanum phosphate activated by cerium and terbium, green phosphor - Google Patents
Preparation method of small size and high brightness lanthanum phosphate activated by cerium and terbium, green phosphor Download PDFInfo
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- CN103351864A CN103351864A CN2013102684379A CN201310268437A CN103351864A CN 103351864 A CN103351864 A CN 103351864A CN 2013102684379 A CN2013102684379 A CN 2013102684379A CN 201310268437 A CN201310268437 A CN 201310268437A CN 103351864 A CN103351864 A CN 103351864A
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Abstract
A preparation method of small size and high brightness lanthanum phosphate activated by cerium and terbium, green phosphor comprises following steps: rare earth soluble salt containing crystal water, and chloride or nitrate, are mixed with alkali metal or phosphatic of ammonium and then the mixture is grinded or ball milled at the room temperature, the precursor of lanthanum phosphate activated by cerium and terbium is obtained after a drying process, then the precursor is sintered for 1 to 24 hours in the presence of auxiliary agent Li2(CO3)3 in a reduction atmosphere at the temperature of 950 to 1250 DEG C, and finally the phosphor product is produced after a washing post-treatment. The substrate of the phosphor is LaPO4, Ce3+ is the sensitization particle, and Tb3+ is the activating center. The chemical formula of the phosphor is La<x>Ce<y>Tb<1-x-y>PO4. The phosphor can give off strong green light with a wavelength around 545 nm under the activation of ultraviolet. The phosphor has the advantages that the particles of the synthesis phosphor are small, the diameters of the median particles are smaller than 1 micrometer, and the light intensity of the phosphor is higher than that of aluminate green phosphor in the present market.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, be specifically related to the method that wet solid phase mechanochemical reaction prepares small size, high brightness lanthanum-cerium-terbium phosphate green emitting phosphor.
Background technology
LaPO
4: Ce, Tb(LAP) be the very important efficient green luminescent material of a class in the three primary colors fluorescent powder.At present, its route of synthesis mainly contains following two kinds: the one, and dry method is synthetic or claim the high temperature solid-state chemical reaction method synthetic, is at high temperature calcination (LaCeTb)
xO
y(NH
4)
2HPO
4Mixture, generate (LaCeTb) PO
4The 2nd, wet method is synthetic or claim the presoma high-temperature calcination synthetic, is that muriate or the nitrate solution of La, Ce, Tb are directly used H
3PO
4Or (NH
4)
2HPO
4Precipitation obtains (LaCeTb) PO
4Presoma, more at a certain temperature reduction calcining after washing drying or the calcining; First method is easy to operate, and output is large, but synthesis temperature is higher, and energy consumption is large, and high to equipment, ingredient requirement, product particle is large, and is essential through ball milling.And ball milling can cause the decline of product fluorescence property, therefore, is difficult to solve the problems such as dephasign generation and globule size control difficulty; Second method seems that simply synthesis temperature also has substantial degradation, and cost is low, but in fact because the deposit seeds that forms is little, filtration is difficult, washing chlorine root is not thorough, and water consumption is very large.And when calcining easily reunite, make the large and skewness of product granularity, quality product is stable not; Therefore, exploring a kind of simple and effective, with low cost, eco-friendly lanthanum-cerium-terbium phosphate preparation method tool is of great significance.
The present invention developed a kind of under normal temperature condition, utilize mechanical external force be used for impelling chemical reaction between the phosphoric acid salt of rare earth chloride, rare earth nitrate and basic metal or ammonium, form lanthanum-cerium-terbium phosphate, calcine to prepare LAP through the reduction under the comparatively high temps again.We have studied the impact that reaction conditions forms LAP, and have inquired into the relation that affects granular size and fluorescence property.Determined to use the top condition that the method is prepared the green emitting phosphor of superior performance.The LAP that synthesizes with high temperature solid-state chemical reaction method and wet method synthetic method compares, and the method need not solvent, the product particle size is less and even, the more important thing is by present commercial aluminate green powder (CAT) height of the LAP luminance factor of the method preparation.Therefore, the present invention can prepare high quality LAP green emitting phosphor under gentle, easy, eco-friendly condition, thereby provides experimental basis for large-scale commercial production.
Summary of the invention
The less energy-consumption synthetic method that the purpose of this invention is to provide the lanthanum-cerium-terbium phosphate green emitting phosphor (LAP) that a kind of synthetic epigranular is tiny, brightness is high, to replace wet method coprecipitation method and high temperature solid-state chemical reaction method commonly used at present, reach energy-saving and cost-reducing, pollution-free and low-cost target.
The objective of the invention is to be achieved through the following technical solutions:
Adopting rare earth chloride or nitrate is raw material, by synthesizing the lanthanum-cerium-terbium phosphate presoma with the phosphatic mechanico-chemical reaction of basic metal or ammonium at normal temperatures and pressures.This presoma can without washing dry can with the Li as the charge compensation agent
2CO
3And some other fusing assistant or dispersant, furnace cooling after the calcining obtains the fluorescent material stock in reducing atmosphere, passes through follow-up washing, dispersion and drying again, obtains required fluorescent material product.The chemical constitution general formula of synthetizing phosphor powder is La
xCe
yTb
1-x-yPO
4, the span of x and y is: X between 0.4 and 0.6, x+y＞0.8, optimum value is x=0.58, y=0.3.Stable RE phosphate (LaPO wherein
4) be matrix, Ce
3+As sensitization particle, Tb
3+As activation center.
Preparation method's step of small size high brightness lanthanum-cerium-terbium phosphate green emitting phosphor of the present invention is as follows:
(1) the pure above LaCl of Analysis on Selecting
36H
2O, CeCl
3.6H
2O, TbCl
3.6H
2O is raw material, according to following chemical constitution formula La
xCe
yTb
1-x-yPO
4The mol ratio that requires accurately takes by weighing corresponding raw material;
The chemical constitution general formula is La
xCe
yTb
1-x-yPO
4, the span of x and y is: X between 0.4 and 0.6, x+y＞0.8, optimum value is x=0.58, y=0.3.Wherein stable RE phosphate is LaPO
4Be matrix, Ce
3+As sensitization particle, Tb
3+As activation center;
(2) pure (NH of Analysis on Selecting
4)
2HPO
4, according to phosphoric acid salt: rare earth=1.05:1 takes by weighing Secondary ammonium phosphate;
(3) above-mentioned raw materials is mixed after, in agate grinds, grind or on ball mill ball milling, grind or ball milling all is to carry out at normal temperatures, milling time is between 40 minutes to 2 hours; Ball-milling Time is between 10 minutes to 40 minutes; The product that obtains behind grinding or the ball milling does not need washing;
(4) will grind or product drying in baking oven that ball milling obtains obtains precursor;
(5) add 1%～20% auxiliary agent in precursor, adjuvant used can be Li
2CO
3, one or more combinations in aluminum oxide, lithium tetraborate, the lithium fluoride.Compound is placed corundum crucible, under reducing atmosphere, calcine, can obtain the sintered compact of this green emitting phosphor;
(6) sintered compact with gained mixes making beating with water, and filtration washing is removed water miscible inorganic salt, 100-160 ℃ of scope oven dry, disperses again, obtains needed fluorescent material.
Beneficial effect of the present invention:
(1) green emitting phosphor that the present invention synthesized adopts stable RE phosphate (LaPO
4) as matrix, Ce
3+As sensitization particle, Tb
3+As activation center, the chemical constitution general formula of synthetizing phosphor powder is La
xCe
yTb
1-x-yPO
4, the span of x and y is: x between 0.4 and 0.6, x+y＞0.8, optimum value is x=0.58, y=0.3 has maximum excitation about 280nm, emission maximum is about 544nm.
(2) green emitting phosphor illumination effect of the present invention is good, and its fluorescent brightness is better than at present commercial aluminate green fluorescent powder CAT, and powder granularity is evenly and less than 1 μ m.
(3) green fluorescence powder, preparation method thereof of the present invention is simple, and easy handling need not to use solvent in the preparation process, energy conservation and consumption reduction effects is arranged, and is typical green synthesis techniques, and therefore good application prospect is arranged.
Description of drawings
Fig. 1 is the products of embodiment 1,2,3,4 preparations, the excitation spectrum that records product take 545nm as the monitoring wavelength with and with the excitation spectrum correlative value of the aluminate green fluorescent powder (CAT) of commercialization.Its strongest excitation peak is positioned at the 279nm place as known in the figure, and the prolongation along with milling time, the fluorescence intensity of product also improves constantly, after milling time reaches 90min, reach best fluorescence, the product that wherein ground 60 minutes and ground 90 minutes is better than commercial aluminate green fluorescent powder (CAT) through fluorescence intensity after calcining;
Fig. 2 is the La of the embodiment of the invention 3 preparations
0.58Ce
0.3Tb
0.12PO
4Through the fluorescence intensity contrast after the differing temps calcining, as seen from the figure, product has best fluorescence intensity after 1100 ℃ of calcinings;
Fig. 3 is the La of the embodiment of the invention 2 preparations
0.58Ce
0.3Tb
0.12PO
4Through washing calcining or the resulting product emmission spectrum of dinectly bruning, as seen from the figure, no matter whether wash the green emitting phosphor that can both obtain high brightness, the effect of even not washing dinectly bruning is better;
Fig. 4 is the La of embodiment 1,2,3,4 preparations
0.58Ce
0.3Tb
0.12PO
4The XRD figure spectrum of precursor, as seen from the figure, along with the prolongation of milling time, the degree of crystallization of product improves, and can form the crystallization RE phosphate in the ball-milling reaction process;
Fig. 5 is the La of embodiment 3,5,6,7 preparations
0.58Ce
0.3Tb
0.12PO
4XRD figure, as seen from the figure, the product phase of differing temps calcining is without obvious difference, and just degree of crystallinity is slightly different;
Fig. 6 is the scanning electron microscope (SEM) photograph of embodiment 3 preparation samples; As seen from the figure, the synthetic product of the method has uniform granularity, and size calcine the front pattern that washs product and have no significant effect, but the product after the washing has adhesion less than 1 μ m.
Table 1 is the fluorescence intensity contrast of the samples of embodiment 3,8,9,10,11 preparations, shows the consumption of solubility promoter as can be known to the impact of product fluorescence intensity, a small amount of Li by this
2CO
3Can improve the luminosity of fluorescent material, but increase rate is very little, adds relatively large Li
2CO
3Then brightness slightly descends.Under this experiment condition, Li
+Incorporation should not be too large, should be controlled at 2 %-4 %.
Fig. 7 is the fluorescence intensity contrast of embodiment 12,13,14,15 products therefroms, as known in the figure, adopt ball milling method also can obtain the green emitting phosphor of high brightness, and Ball-milling Time is influential to the fluorescence of product, prolongation along with the time, the fluorescence intensity rear decline of rising first, 30 minutes best results of ball milling.
Fig. 8 is the XRD of embodiment 16,17,18 products obtained therefroms, as known in the figure, changes the rare earth source or changes the phase that source of phosphoric acid does not affect product.
Fig. 9 is the utilizing emitted light spectrogram of embodiment 17,18 products obtained therefroms, this figure is arranged as can be known, changes the fluorescence intensity that phosphoric acid salt can affect product, and the effect of ammonium phosphate salt is better than sodium phosphate salt.
Figure 10 is the utilizing emitted light spectrogram of embodiment 16 products therefroms, as known in the figure, changes the fluorescence intensity that the rare earth source also can affect product, and the effect of rare earth chloride is better than rare earth nitrate.
Embodiment
Embodiment 1: the pure above LaCl of Analysis on Selecting
36H
2O, CeCl
3.6H
2O, TbCl
3.6H
2O is raw material, according to chemical constitution formula La
xCe
yTb
1-x-yPO
4The mol ratio that requires accurately takes by weighing corresponding raw material; (the NH that Analysis on Selecting is pure
4)
2HPO
4, according to phosphoric acid salt: rare earth=1.05:1 takes by weighing Secondary ammonium phosphate; After they are mixed, ground 40 minutes in agate grinds, the product that then ball milling is obtained drying in baking oven obtains precursor, adds 2% solubility promoter Li in precursor again
2CO
3, at last precursor is placed 1100 ℃ of calcinings of reduction furnace 3h, namely obtain product.Its exciting light spectrogram is seen Fig. 1, and XRD figure is seen Fig. 4.
Embodiment 2: the pure above LaCl of Analysis on Selecting
36H
2O, CeCl
3.6H
2O, TbCl
3.6H
2O is raw material, according to chemical constitution formula La
xCe
yTb
1-x-yPO
4The mol ratio that requires accurately takes by weighing corresponding raw material; (the NH that Analysis on Selecting is pure
4)
2HPO
4, according to phosphoric acid salt: rare earth=1.05:1 takes by weighing Secondary ammonium phosphate; After they are mixed, ground 60 minutes in agate grinds, the product that then ball milling is obtained drying in baking oven obtains precursor, adds 2% auxiliary agent Li in precursor again
2CO
3, at last precursor is placed 1100 ℃ of calcinings of reduction furnace 3h, namely obtain product.Its exciting light spectrogram is seen Fig. 1, and XRD figure is seen Fig. 4.
Embodiment 3: adopt the identical method of embodiment 1, milling time is extended to 90 minutes, its exciting light spectrogram is seen Fig. 1, and XRD figure is seen Fig. 4, and emmission spectrum is seen Fig. 2, and scanning electron microscope (SEM) photograph is seen Fig. 6.
Embodiment 4: adopt the identical method of embodiment 1, milling time is extended to 120 minutes, its exciting light spectrogram is seen Fig. 1, and XRD figure is seen Fig. 4.
Embodiment 5: adopt the method for embodiment 3, change calcining temperature into 950 °, its emmission spectrum is seen Fig. 3, and XRD sees Fig. 5.
Embodiment 6: adopt the method for embodiment 3, calcining temperature is changed into: 1000 °, its emmission spectrum is seen Fig. 3, and XRD sees Fig. 5.
Embodiment 7: adopt the method for embodiment 3, calcining temperature is changed into: 1250 °, its emmission spectrum is seen Fig. 3, and XRD sees Fig. 5.
Embodiment 8: adopt the method for embodiment 3, with auxiliary agent Li
2CO
3Consumption change 4% into, emissive porwer sees Table 1.
Embodiment 9: adopt the method for embodiment 3, with auxiliary agent Li
2CO
3Consumption change 6% into, emissive porwer sees Table 1.
Embodiment 10: adopt the method for embodiment 3, with auxiliary agent Li
2CO
3Consumption change 8% into, emissive porwer sees Table 1.
Embodiment 11: adopt the method for embodiment 3, do not add auxiliary agent, emissive porwer sees Table 1
Embodiment 12: the pure above LaCl of Analysis on Selecting
36H
2O, CeCl
3.6H
2O, TbCl
3.6H
2O is raw material, according to chemical constitution formula La
xCe
yTb
1-x-yPO
4The mol ratio that requires accurately takes by weighing corresponding raw material; (the NH that Analysis on Selecting is pure
4)
2HPO
4, be phosphoric acid salt according to the ratio of amount of substance: rare earth=1.05:1 takes by weighing Secondary ammonium phosphate; After they are mixed, ball milling certain hour on ball mill (30 minutes), the product that then ball milling is obtained drying in baking oven obtains precursor, adds 2% auxiliary agent Li in precursor again
2CO
3, at last precursor is placed 1100 ℃ of calcinings of reduction furnace 3h, namely obtain product.Its fluorescence intensity the results are shown in Figure 7.
Embodiment 13: according to the method for embodiment 12, changing Ball-milling Time is 10 minutes, and its fluorescence intensity the results are shown in Figure 7.
Embodiment 14: according to the method for embodiment 12, changing Ball-milling Time is 20 minutes, and its fluorescence intensity the results are shown in Figure 7.
Embodiment 15: according to the method for embodiment 12, changing Ball-milling Time is 40 minutes, and its fluorescence intensity the results are shown in Figure 7.
Embodiment 16: the method according to embodiment 12, change Secondary ammonium phosphate into ammonium phosphate, and its XRD the results are shown in Figure 8, and its emmission spectrum is seen Fig. 9.
Embodiment 17: the method according to embodiment 12, change Secondary ammonium phosphate into sodium phosphate, and its XRD the results are shown in Figure 8, and its emmission spectrum is seen Fig. 9.
Embodiment 18: the method according to embodiment 12, change rare earth chloride into rare earth nitrate, and its XRD the results are shown in Figure 8, and its emmission spectrum is seen Figure 10.
Following table is that the consumption of embodiment 3,8,9,10,11 solubility promoters is on the impact of product fluorescence intensity
| Li +Content (g/g) | Relative brightness |
| 0% | 1.00 |
| 2% | 1.14 |
| 4% | 1.07 |
| 6% | 0.952 |
| 8% | 0.560 |
Claims (1)
1. the preparation method of small size high brightness lanthanum-cerium-terbium phosphate green emitting phosphor is characterized in that:
(1) the pure above LaCl of Analysis on Selecting
36H
2O, CeCl
3.6H
2O, TbCl
3.6H
2O is raw material, according to following chemical constitution formula La
xCe
yTb
1-x-yPO
4The mol ratio that requires accurately takes by weighing corresponding raw material;
The chemical constitution general formula is La
xCe
yTb
1-x-yPO
4, the span of x and y is: X between 0.4 and 0.6, x+y＞0.8, optimum value is x=0.58, y=0.3;
Wherein stable RE phosphate is LaPO
4Be matrix, Ce
3+As sensitization particle, Tb
3+As activation center;
(2) pure (NH of Analysis on Selecting
4)
2HPO
4, according to phosphoric acid salt: rare earth=1.05:1 takes by weighing Secondary ammonium phosphate;
(3) above-mentioned raw materials is mixed after, in agate grinds, grind or on ball mill ball milling, grind or ball milling all is to carry out at normal temperatures, milling time is between 40 minutes to 2 hours; Ball-milling Time is between 10 minutes to 40 minutes; The product that obtains behind grinding or the ball milling does not need washing;
(4) will grind or product drying in baking oven that ball milling obtains obtains precursor;
(5) add 1%～20% auxiliary agent in precursor, adjuvant used can be Li
2CO
3, one or more combinations in aluminum oxide, lithium tetraborate, the lithium fluoride; Compound is placed corundum crucible, under reducing atmosphere, calcine, can obtain the sintered compact of this green emitting phosphor;
(6) sintered compact with gained mixes making beating with water, and filtration washing is removed water miscible inorganic salt, 100-160 ℃ of scope oven dry, disperses again, obtains needed fluorescent material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571489A (en) * | 2013-11-08 | 2014-02-12 | 广州珠江光电新材料有限公司 | Method for synthesizing small-granularity narrow-distribution green fluorescent precursor |
| 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 |
| CN110563339A (en) * | 2019-10-17 | 2019-12-13 | 维沃泰克仪器(扬州)有限公司 | Preparation method of anhydrous lithium borate fluxing agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070474A (en) * | 2007-06-14 | 2007-11-14 | 中南大学 | Shell-grade green illuminating material for lamp and preparing method |
| WO2011012508A1 (en) * | 2009-07-29 | 2011-02-03 | Rhodia Operations | Composition comprising a cerium and/or terbium phosphate and sodium, of core/shell type, phosphor resulting from this composition and methods for preparing same |
-
2013
- 2013-07-01 CN CN2013102684379A patent/CN103351864A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070474A (en) * | 2007-06-14 | 2007-11-14 | 中南大学 | Shell-grade green illuminating material for lamp and preparing method |
| WO2011012508A1 (en) * | 2009-07-29 | 2011-02-03 | Rhodia Operations | Composition comprising a cerium and/or terbium phosphate and sodium, of core/shell type, phosphor resulting from this composition and methods for preparing same |
Non-Patent Citations (1)
| Title |
|---|
| MIAN-ZENG SU等: "Reaction mechanism for the solid state synthesis of LaPO4:Ce,Tb phosphor", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103571489A (en) * | 2013-11-08 | 2014-02-12 | 广州珠江光电新材料有限公司 | Method for synthesizing small-granularity narrow-distribution green fluorescent precursor |
| 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 |
| CN110563339A (en) * | 2019-10-17 | 2019-12-13 | 维沃泰克仪器(扬州)有限公司 | Preparation method of anhydrous lithium borate fluxing agent |
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Application publication date: 20131016 |