CN102191055A - Core-shell structured silicate luminescent material and preparation method thereof - Google Patents
Core-shell structured silicate luminescent material and preparation method thereof Download PDFInfo
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- CN102191055A CN102191055A CN2010101225714A CN201010122571A CN102191055A CN 102191055 A CN102191055 A CN 102191055A CN 2010101225714 A CN2010101225714 A CN 2010101225714A CN 201010122571 A CN201010122571 A CN 201010122571A CN 102191055 A CN102191055 A CN 102191055A
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Abstract
The invention provides a core-shell structured silicate luminescent material, the structural formula of which is Ln2-xSiO5:Tbx@SiO2. Wherein, Ln stands for at least one rare earth element, @ represents cladding, and x is greater than 0 and smaller than or equal to 0.5. The invention also provides a preparation method for the luminescent material, comprising the steps of: mixing ethanol, deionized water and ammoniacal liquor, and adding the mixture into ethyl orthosilicate so as to obtain SiO2 nanospheres, adding a salting solution of Ln and a salting solution of Tb, then adding oxalic acid, washing, precipitating and drying the mixed solution so as to obtain a precursor, and finally cooling the precursor after a heat treatment and a reduction treatment, thus obtaining a finished product. The core-shell structured silicate luminescent material obtained in the invention is characterized by controllable size and morphology, excellent luminescent property, and good stability, while the method has the advantages of simple preparation technology, short cycle of reaction, good reproducibility, low cost as well as wide prospect of manufacturing and application.
Description
Technical field
The invention belongs to the luminescent material technical field, be specifically related to a kind of nucleocapsid structure silicate luminescent material and preparation method thereof.
Background technology
Present commercial luminescent material prepares with high temperature solid-state method mostly, pyroreaction big energy-consuming and size distribution inequality, and the powder pattern is different, need method with ball milling to obtain the fluorescent material of 2～8 micron grain sizes, and make the powder granule size inconsistent, pattern is imperfect, causes the coating inequality.People pass through to use sol-gel method, hydrothermal synthesis method, and methods such as complexing gel method prepare fluorescent material, and these methods can remedy the deficiency of high temperature solid phase synthesis, but the luminous intensity of the fluorescent material of these method gained is not as high temperature solid phase synthesis.Obtain size, pattern is controlled and the silicate material of good luminous performance is the target of researchist's effort always.
Summary of the invention
In view of this, the invention provides and a kind ofly can prepare size, pattern is controlled, luminescent properties is good nucleocapsid structure silicate luminescent material.
And, provide that a kind of preparation technology is simple, reaction time weak point, good reproducibility, nucleocapsid structure silicate luminescent material preparation method that cost is low.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
A kind of nucleocapsid structure silicate luminescent material, its structural formula are Ln
2-xSiO
5: Tb
x@SiO
2, wherein, Ln is a rare earth element, (@ coats, and x is 0＜x≤0.5.
And, a kind of nucleocapsid structure silicate luminescent material preparation method, it comprises the steps:
Ethanol, deionized water and ammoniacal liquor are mixed back adding tetraethoxy make SiO
2Nanometer ball; Again
Press structural formula Ln
2-xSiO
5: Tb
x@SiO
2Middle respective element stoichiometric ratio adds Ln salts solution and Tb salts solution, and wherein, Ln is a rare earth element, and @ coats, and x is 0＜x≤0.5;
Add oxalic acid in above-mentioned solution, washing precipitation and drying obtain presoma then;
Presoma heat-treated and reduce and handle postcooling and get described nucleocapsid structure silicate luminescent material finished product.
In above-mentioned nucleocapsid structure silicate luminescent material and preparation method thereof, the good stability of gained luminescent material; Simultaneously, in nucleocapsid structure silicate luminescent material preparation method, size, the pattern of nucleocapsid structure silicate luminescent material are controlled, and luminescent properties is good, and the reaction in this method is all finished in liquid phase.The preparation technology of this method is simple, reaction time weak point, good reproducibility, cost low, have wide production application prospect.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is that the luminescent material of the embodiment of the invention 3 preparation is the luminescent spectrum under the cathode-ray exciting under the 1.5KV and the comparison diagram of commercial powder at acceleration voltage, and wherein curve 1 is commercial powder Y
2SiO
5: the luminescent spectrum of Tb; Curve 2 is Y of embodiment 3 preparations
1.88SiO
5: Tb
0.12@SiO
2The luminescent spectrum of luminescent material.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Embodiment of the invention nucleocapsid structure silicate luminescent material, its structural formula is: Ln
2-xSiO
5: Tb
x@SiO
2, wherein, Ln is a rare earth element, at least a among preferred Y, Gd, Sc, Lu or the La; @ coats, and promptly is with spherical SiO
2Be nuclear, Ln
2-xSiO
5: Tb
xFluorescent material is shell; X is 0＜x≤0.5, is preferably 0.05≤x≤0.20.
Above-mentioned nucleocapsid structure silicate luminescent material good stability, and this luminescent material has spherical morphology, and size, pattern are controlled, and spherical morphology has higher tap density, is convenient to be coated with screen technology and improves display effect.
The preparation method of embodiment of the invention nucleocapsid structure silicate luminescent material, it comprises the steps:
Adopt
Method coated Si O
2Nanometer ball is about to add tetraethoxy after ethanol, deionized water and ammoniacal liquor mix and makes SiO
2Nanometer ball; Again
Press structural formula Ln
2-xSiO
5: Tb
x@SiO
2Middle respective element stoichiometric ratio adds the salts solution of Ln and Tb, mix the back and drip oxalic acid solution, generate white precipitate, with ammoniacal liquor reaction system is regulated the pH value to weakly alkaline again, follow being carried out to, filtration successively, precipitate with deionized water and absolute ethanol washing, final drying obtains presoma;
Placing retort furnace to heat-treat and reduce presoma handles postcooling and gets described silicate luminescent material finished product.
Above-mentioned employing
Method coated Si O
2The nanometer ball method be according to
The sol-gel method that at first proposes Deng the people is prepared SiO
2Nanometer ball, promptly according to
Method is mixed back adding tetraethoxy with ethanol, deionized water and ammoniacal liquor and is prepared SiO
2Nanometer ball.Should
Method can be regulated and control this ratio of ethanol, deionized water, ammoniacal liquor, tetraethoxy, and prepares the SiO of different-grain diameter
2Ball.
In the above-mentioned preparation presoma step, the salts solution preferably nitrate solution of Ln and Tb is or/and chloride salt solution, and its addition is that Ln and Tb element mole sum and whole preparation method use the Si element molar ratio in the reactant to be less than or equal to 2.The consumption of oxalic acid should capacity, calculates according to amount, and excessive 25% is advisable, promptly guaranteed sedimentary fully.This step can generate white precipitate after adding oxalic acid, regulates the pH value to weakly alkaline with ammoniacal liquor then, stirs successively, ageing, filtration again, uses deionized water and absolute ethanol washing then, and oven dry at last obtains presoma.The invention described above embodiment utilizes ball
The SiO of method preparation
2Ball is that raw material adopts coprecipitation method to prepare Ln
2SiO
5, therefore, Ln salt is deposited in SiO
2The ball surface.
In the above-mentioned preparation finished product step, thermal treatment preferably is placed on presoma in the retort furnace and handles 1～12h down in 900 ℃～1600 ℃.Reduction is handled preferably and is placed reducing environment at 1000 ℃～1600 ℃ reduction 1～8h presoma after heat treatment, and this reducing environment is N
2And H
2The mixed gas reducing atmosphere, carbon reducing agent atmosphere, CO reducing atmosphere or the pure H that form
2Reducing atmosphere.In the invention described above nucleocapsid structure silicate luminescent material preparation method, adopt earlier
Method prepares SiO
2Nanometer ball, can obtain size, the powder that pattern is controlled, the thickness of the granular size by regulating silicon dioxide microsphere and the beds of precipitation of formation can realize controlling the granular size of fluorescent material, and because nuclear (silicon dioxide microsphere) is spheric, therefore serve as the main spheric just of granule-morphology of examining the fluorescent material that obtains with it, therefore say that pattern can accomplish even and single, the spheric particle can obtain bigger tap density simultaneously, the light that self is sent is also the strongest in the emission effect of all directions, thereby can reduce the scattering of light of fluorescent material, form core-shell material by coating then, can improve the internal quantum efficiency of luminescent material greatly, it is good further to obtain luminous intensity by the high temperature solid-state step again, stay-in-grade fluorescent material.Meanwhile, the reaction in this method is all finished in liquid phase, and preparation technology is simple, reaction time is short, good reproducibility, cost are low, has wide production application prospect.
Below illustrate the nucleocapsid structure silicate luminescent material by a plurality of embodiment difference form and preparation method thereof, with and aspect such as performance.
Embodiment 1
Coprecipitation method prepares Sc
1.95SiO
5: Tb
0.05@SiO
2:
Get the 30mL dehydrated alcohol in Erlenmeyer flask, add 8mL deionized water and 10mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 1.2mL while stirring, behind the reaction 6h, add 7.8mL 1mol/LScCl
3With 4mL 0.05mol/L TbCl
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1600 ℃ of thermal treatment 1h of retort furnace, again in tube furnace at 95%N
2+ 5%H
2The following 1000 ℃ of sintering 8h reduction of reducing atmosphere is cooled to room temperature, can obtain Sc
1.95SiO
5: Tb
0.05@SiO
2Luminescent material.
Embodiment 2
Coprecipitation method prepares Gd
1.80SiO
5: Tb
0.20@SiO
2:
Get the 20mL dehydrated alcohol in Erlenmeyer flask, add 6mL deionized water and 3mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 1.5mL while stirring, behind the reaction 6h, add 3.6mL 2mol/LGd (NO
3)
3With 4mL 0.20mol/L Tb (NO
3)
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 900 ℃ of thermal treatment 12h of retort furnace, and 1400 ℃ of sintering 4h reduction under carbon reducing agent atmosphere in retort furnace again are cooled to room temperature, can obtain Gd
1.80SiO
5: Tb
0.20@SiO
2Luminescent material.
Embodiment 3
Coprecipitation method prepares Y
1.88SiO
5: Tb
0.12@SiO
2:
Get the 25mL dehydrated alcohol in Erlenmeyer flask, add 10mL deionized water and 6mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 1.0mL while stirring, behind the reaction 6h, add 7.52mL 1mol/LY (NO
3)
3With 9.6mL 0.05mol/L Tb (NO
3)
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1200 ℃ of thermal treatment 2h of retort furnace, again in tube furnace at 95%N
2+ 5%H
2The following 1200 ℃ of sintering 2h reduction of reducing atmosphere is cooled to room temperature, can obtain Y
1.88SiO
5: Tb
0.12@SiO
2Luminescent material.Be the green emitting phosphor (Y of existing commercial distribution as shown in Figure 1
2SiO
5: Tb) with the cathodoluminescence spectrum comparison diagram of the nucleocapsid structure silicate luminescent material of present embodiment preparation, the green emitting phosphor (Y of existing commercial distribution wherein
2SiO
5: Tb) being is the Y of dopant ion with Tb
2SiO
5Green emitting phosphor, as can be seen from the figure the luminescent material of present embodiment has stronger emission peak at the 544nm place, and luminous intensity is than the green emitting phosphor (Y of commercial distribution
2SiO
5: luminous intensity Tb) is strong by 40%, and the luminescent material of present embodiment has the higher characteristics of good stability, high color purity and luminous efficiency.
Embodiment 4
Coprecipitation method prepares Lu
1.92SiO
5: Tb
0.08@SiO
2:
Get the 15mL dehydrated alcohol in Erlenmeyer flask, add 10mL deionized water and 4mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 1.8mL while stirring, behind the reaction 6h, add 7.6mL 1mol/LLuCl
3With 6.4mL 0.05mol/L TbCl
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1500 ℃ of thermal treatment 3h of retort furnace, and 1600 ℃ of sintering 1h reduction under the CO reducing atmosphere in tube furnace again are cooled to room temperature, can obtain Lu
1.92SiO
5: Tb
0.08@SiO
2Luminescent material.
Embodiment 5
Coprecipitation method prepares La
1.85SiO
5: Tb
0.15@SiO
2:
Get the 20mL dehydrated alcohol in Erlenmeyer flask, add 6mL deionized water and 2mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 2.0mL while stirring, behind the reaction 6h, add 3.7mL 2mol/LY (NO
3)
3With 6mL 0.1mol/L Tb Cl
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1400 ℃ of thermal treatment 6h of retort furnace, again in tube furnace at H
2The following 1300 ℃ of sintering 3h reduction of reducing atmosphere is cooled to room temperature, can obtain La
1.85SiO
5: Tb
0.15@SiO
2Luminescent material.
Embodiment 6
Coprecipitation method prepares Y
1.50SiO
5: Tb
0.50@SiO
2:
Get the 35mL dehydrated alcohol in Erlenmeyer flask, add 10mL deionized water and 8mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 2.0mL while stirring, behind the reaction 6h, add 6mL 1mol/LY (NO
3)
3With 5mL 0.4mol/L Tb (NO
3)
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1500 ℃ of thermal treatment 2h of retort furnace, again in tube furnace at 95%N
2+ 5%H
2The following 1300 ℃ of sintering 4h reduction of reducing atmosphere is cooled to room temperature, can obtain Y
1.50SiO
5: Tb
0.50@SiO
2Luminescent material.
Embodiment 7
Coprecipitation method prepares Y
1.0Sc
0.50SiO
5: Tb
0.50@SiO
2:
Get the 25mL dehydrated alcohol in Erlenmeyer flask, add 8mL deionized water and 5mL ammoniacal liquor then, after stirring, add the positive tetraethyl orthosilicate of 1.5mL while stirring, behind the reaction 6h, add 4mL 1mol/LY (NO
3)
3, 2mL 1mol/L Sc (NO
3)
3With 5mL 0.4mol/L Tb (NO
3)
3Solution, after stirring, drip the oxalic acid solution of 15mL 1mol/L again, generate white precipitate, then regulate pH value to 8～9, stir 3h, ageing, filtration then successively with ammoniacal liquor, use deionized water and absolute ethanol washing 3 times at last, oven dry obtains presoma.Presoma is placed 1400 ℃ of thermal treatment 6h of retort furnace, again in tube furnace at H
2The following 1300 ℃ of sintering 4h reduction of reducing atmosphere is cooled to room temperature, can obtain Y
1.0Sc
0.50SiO
5: Tb
0.50@SiO
2Luminescent material.
Claims (10)
1. nucleocapsid structure silicate luminescent material, its structural formula is Ln
2-xSiO
5: Tb
x@SiO
2, wherein, Ln is a rare earth element, and @ coats, and x is 0＜x≤0.5.
2. nucleocapsid structure silicate luminescent material as claimed in claim 1 is characterized in that: described Ln is at least a among Y, Gd, Sc, Lu or the La.
3. nucleocapsid structure silicate luminescent material as claimed in claim 1 is characterized in that: described coating is a spherical SiO
2Be nuclear, fluorescent material Ln
2-xSiO
5: Tb
xBe shell.
4. nucleocapsid structure silicate luminescent material as claimed in claim 1 is characterized in that: described x is 0.05≤x≤0.20.
5. nucleocapsid structure silicate luminescent material preparation method, it comprises the steps:
Ethanol, deionized water and ammoniacal liquor are mixed back adding tetraethoxy make SiO
2Nanometer ball; Again
Press structural formula Ln
2-xSiO
5: Tb
x@SiO
2Middle respective element stoichiometric ratio adds Ln salts solution and Tb salts solution, and wherein, Ln is a rare earth element, and @ coats, and x is 0＜x≤0.5;
Add oxalic acid in above-mentioned solution, washing precipitation and drying obtain presoma then;
Presoma heat-treated and reduce and handle postcooling and get described nucleocapsid structure silicate luminescent material finished product.
6. the preparation method of nucleocapsid structure silicate luminescent material as claimed in claim 5 is characterized in that:
Described Ln salts solution and Tb salts solution consumption satisfy Ln and Tb element mole sum and whole preparation method and use the Si element molar ratio in the reactant to be less than or equal to 2.
7. the preparation method of nucleocapsid structure silicate luminescent material as claimed in claim 6 is characterized in that: the salts solution of described Ln and Tb is that nitrate solution is or/and chloride soln.
8. the preparation method of nucleocapsid structure silicate luminescent material as claimed in claim 5 is characterized in that: described thermal treatment is to handle 1～12h down at 900 ℃～1600 ℃.
9. the preparation method of nucleocapsid structure silicate luminescent material as claimed in claim 5 is characterized in that: it is to build a reducing environment around presoma that described reduction is handled, 1000 ℃～1600 ℃ of its envrionment temperatures, reduction treatment time 1～8h.
10. the preparation method of nucleocapsid structure silicate luminescent material as claimed in claim 9 is characterized in that: described reducing environment is meant and contains N
2And H
2, carbon dust, CO or pure H
2Reducing atmosphere.
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| CN106590620A (en) * | 2016-11-22 | 2017-04-26 | 青岛海信电器股份有限公司 | Fluorescent powder, preparation method thereof, fluorescent powder film sheet, and fluorescent powder module structure |
| CN113088277A (en) * | 2021-03-18 | 2021-07-09 | 山东师范大学 | CeF3Base up-conversion luminescent material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013166665A1 (en) * | 2012-05-08 | 2013-11-14 | 海洋王照明科技股份有限公司 | Core-shell structured silicate luminescent material and preparation method therefor |
| CN104271706A (en) * | 2012-05-08 | 2015-01-07 | 海洋王照明科技股份有限公司 | Core-shell structured silicate luminescent material and preparation method therefor |
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| CN103881713A (en) * | 2012-12-20 | 2014-06-25 | 海洋王照明科技股份有限公司 | Core-shell structured calcium silicate luminescent material and preparation method thereof |
| CN103881713B (en) * | 2012-12-20 | 2015-07-08 | 海洋王照明科技股份有限公司 | Core-shell structured calcium silicate luminescent material and preparation method thereof |
| CN106590620A (en) * | 2016-11-22 | 2017-04-26 | 青岛海信电器股份有限公司 | Fluorescent powder, preparation method thereof, fluorescent powder film sheet, and fluorescent powder module structure |
| CN113088277A (en) * | 2021-03-18 | 2021-07-09 | 山东师范大学 | CeF3Base up-conversion luminescent material and preparation method and application thereof |
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