CN109913216A - A kind of preparation method of fluorescent powder - Google Patents
A kind of preparation method of fluorescent powder Download PDFInfo
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- CN109913216A CN109913216A CN201910165523.4A CN201910165523A CN109913216A CN 109913216 A CN109913216 A CN 109913216A CN 201910165523 A CN201910165523 A CN 201910165523A CN 109913216 A CN109913216 A CN 109913216A
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- lanthanum
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- terbium
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Abstract
The present invention relates to phosphor technologies fields, and in particular to a kind of preparation method of fluorescent powder.The raw material for preparing fluorescent powder are isolated with crucible using plastic foil in the present invention, heating is carried out again fires fluorescent powder, it avoids fluorescent powder raw material from directly contacting with crucible to cause to bond, substantially increases and fire product yield (up to 97.5%, improving 10% or so more at present).And the speciality such as light efficiency, dispersibility and thermal stability of fluorescent powder can't reduce.
Description
Technical field
The present invention relates to phosphor technologies fields, and in particular to a kind of preparation method of fluorescent powder.
Background technique
The matrix of fluorescent powder is LaPO4, Ce3+As sensitization particle, Tb3+As Validation Counter, the chemical composition of fluorescent powder
General formula is (LaCeTb) PO4, lanthanum-cerium-terbium phosphate is a kind of orthophosphates mixture of rare earth.There are two kinds of structures of matter, a kind of
For monocline body structure, another is hexagonal structure.Wherein the lanthanum-cerium-terbium phosphate of monocline result can be under the excitation of ultraviolet light
Issue the phosphorescence of green.Its main emission peak is located at 545nm, is commonly called as green emitting phosphor.Since its luminous efficiency is high, chemical structure is steady
The features such as determining is widely used in rare-earth trichromatic energy saving lamp and LCD backlight in cold pole fluorescent lamp CCFL.
Application number 97119546.3 is disclosed in the prior art discloses small-sized lanthanum cerium terbium phosphate phosphors and its preparation
Method;Application number: 201110357490.7 disclose a kind of preparation method of lanthanum-cerium-terbium phosphate nano wire;Application number
201310268437.9 disclosing the preparation method of small size high brightness lanthanum-cerium-terbium phosphate green emitting phosphor;Due to extraneous factor and
The factor of luminescent material itself, powder is easy to stick is aoxidizing for the firing of prior art preparation obtained green emitting phosphor lanthanum-cerium-terbium phosphate
Inside aluminium crucible, powder yield is caused to be lower, to reduce income.
Summary of the invention
In view of this, it is necessary to for above-mentioned problem, provide a kind of preparation method of fluorescent powder.
To achieve the above object, the present invention takes technical solution below:
The preparation method of fluorescent powder of the invention, plastic foil is set between the raw material of fluorescent powder and crucible, then is carried out
Fluorescent powder is fired in heating.The raw material for preparing fluorescent powder are isolated with crucible using plastic foil, then carries out heating and fires fluorescent powder,
It avoids fluorescent powder raw material from directly contacting with crucible to cause to bond.
Before firing fluorescent powder, coating materials film can fix the shape of powder, but can be carried out with the crucible surface of installation every
From.
The plastic foil is a kind of material easily melted, and fusing point should be far below to prepare temperature achieved when fluorescent powder
Degree.During preparing fluorescent powder, plastic foil can be to melt volatilization at 600~800 DEG C of higher temperature, will not remain on fluorescence
In powder finished product.
Plastic foil be as polyethylene, polypropylene, polyester, nylon, polyvinyl chloride, vinyl acetate, polyethylene+vinyl acetate,
Film or polybag etc. that the materials such as the laminating polypropylene of polypropylene are formed, be also not limited to certainly the plastic material of the example above with
And forming shape, it can also be film or the bag etc. that other plastic materials are formed, fusing point, which meets to be far below, prepares fluorescent powder when institute
The temperature reached.
A kind of preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor, comprising:
S1, the method using co-precipitation, mixed metal La3+、Ce3+、Tb3+Obtain lanthanum cerium terbium co-precipitation body;
Wherein, Tb is exciting agent, and Ce is sensitizer.
As some of which embodiment of the present invention, the invention also includes auxiliary agent, the auxiliary agent and lanthanum cerium terbium are co-precipitated
Bluk recombination forms mixed powder.
Preferably, the auxiliary agent is one of boric acid, lithium tetraborate, aluminium oxide or a variety of.
The ratio between the boric acid and lanthanum cerium terbium co-precipitation weight are added as 1:9~11;
The ratio between the lithium tetraborate and lanthanum cerium terbium co-precipitation weight are added as 1:30~38;
The ratio between the aluminium oxide and lanthanum cerium terbium co-precipitation weight are added as 1:50~60.
Further, the auxiliary agent is mixed with lanthanum cerium terbium co-precipitation body using blender, forms the mixed powder of white.Such as
It can be to be set as 200rpm by blender revolving speed, stir 10min, that is, obtain more uniform mixed powder.
Auxiliary agent added by the present invention, lithium tetraborate can reduce the firing temperature of powder, and boric acid can make the particle of fluorescent powder
It is rounded, aluminium oxide removes certain particular matters in fluorescent powder.
As the one such embodiment of the present invention, the auxiliary agent is boric acid, lithium tetraborate, aluminium oxide, described in addition
The ratio between boric acid and lanthanum cerium terbium co-precipitation weight are 1:9~11;Add the lithium tetraborate and lanthanum cerium terbium co-precipitation weight it
Than for 1:30~38;The ratio between the aluminium oxide and lanthanum cerium terbium co-precipitation weight are added as 1:50~60.
It is furthermore preferred that the auxiliary agent is boric acid, lithium tetraborate, aluminium oxide, boric acid: lanthanum cerium terbium is co-precipitated body=1:10;Four
Lithium borate: lanthanum cerium terbium is co-precipitated body=1:33;Aluminium oxide: lanthanum cerium terbium is co-precipitated body=1:50.
S2, lanthanum cerium terbium co-precipitation body is fired by being placed in crucible after plastic foil isolation;
The crucible can select the crucible as aoxidized aluminium material.
Plastic foil can be sheet;Also it can be made certain shapes, it is such as bag-shaped.
The addition of plastic foil or bag will not influence the progress of reaction, because just having melted in heating zone (600~800 DEG C)
Change, and this can be such that the powder shape in crucible solidifies, so as to separate powder periphery and crucible, to improve yield.
Further, it in sintering procedure described in S2, is passed through under 7~10% hydrogen and 93~90% nitrogen, the firing time is
6.5h~7.5h, temperature are 1300~1400 DEG C.
S3, the product after firing is post-processed up to lanthanum-cerium-terbium phosphate green emitting phosphor.
As some of embodiments of the invention, the last handling process include crushings, water sieve, slurried, PH adjust,
Sieving, dry, acquisition lanthanum-cerium-terbium phosphate green emitting phosphor.
Preferably, after PH adjustment, before sieving further include ball milling, make its particle size reduction and more uniform.Ball
The powder that mill terminates crosses 50~60 μm of sieve, obtains fine powder.
Further, it is described crushing be fluorescent powder, water, abrading-ball mass ratio be to be crushed under 1:2~3:1~2.
Above-mentioned crushing is that speed of agitator is 36~60rpm in magnetic bucket, and the time is 10~16h.
As some of embodiments of the invention, the water sieve is to remove thick ion by 830~860 μm of sieve.
As some of embodiments of the invention, the slurry is turned to adds deionized water submergence in powder, every 5
A water is changed within~10 minutes, is cleaned 3~5 times;
After slurried cleaning, its PH is adjusted to 5.0~6.0.Such as use mass percentage concentration for 20%~25% ammonium hydroxide
It slowly instills in slurry and adjusts its PH mono- until precipitating, the stirring of adjustment process side, slurry revolving speed are adjusted to 150~300rpm;
Preferably, above-mentioned slurry can also be stood washing after PH adjustment twice, make its PH further by washing
Up to 5.0~6.0.
La in co-precipitation body of the invention3+、Ce3+、Tb3+It is preferred that proportionally (10~12): (5~7): (1~5), to obtain
Obtain preferable fluorescent effect.
The invention has the benefit that
1, compared with prior art, the present invention is easy to stick inside alumina crucible for current fluorescent powder firing powder,
It causes powder yield greatly to reduce, in order to solve this problem, introduces a kind of plastic film, substantially increase firing product
Yield (up to 97.5%, improves 10% or so) more at present.And the speciality such as light efficiency, dispersibility and thermal stability of fluorescent powder are simultaneously
It will not reduce.Wherein, when plastic foil is as crucible volume, yield is maximum;When polybag volume is more than or less than crucible,
Yield is decreased slightly as.When plastics film thickness is in 0.088~0.176mm, the firing of fluorescent powder will not influence.
2, lanthanum-cerium-terbium phosphate green emitting phosphor prepared by the present invention has steady chemical structure, and luminous efficiency is high, easily burns
At, feature at low cost.Simultaneously because LAP has and the comparable density of red fluorescence powder, therefore using fluorescent lamp made from LAP
Pipe end color difference is seldom generated, and for aluminate green powder, the available relatively fine particle of LAP, it is possible to reduce glimmering
Consumption of the light powder in fluorescent lamp, to save valuable rare earth resources.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution work further clearly and completely describes.It should be noted that described embodiment is only the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
It is as follows to prepare lanthanum-cerium-terbium phosphate green emitting phosphor process of the invention:
1, by La3+、Ce3+、Tb3+Lanthanum cerium terbium proportionally, which is mixed to get, for 11:6:3 is co-precipitated body;
2,569g is co-precipitated body, 56.9g boric acid, 17.24g lithium tetraborate, 11.38g aluminium oxide to be put into blender, is turned
Speed is 200rpm, and time 10min, powder color is white;
3,600g powder finely dispersed in 2 is fitted into polybag, is then charged into alumina crucible;
4, product in 3 is put into firing furnace, firing time 7h, temperature is 1300 DEG C, and is passed through 7% hydrogen and 93%
Nitrogen;
5, it crushes: powder 600g, water 1500g, abrading-ball 900g after firing being fitted into magnetic bucket and stir 12h, revolving speed is
36rpm;
6, thick ion water sieve: is removed by the sieve of 850um;
7, slurried: powder and the total volume of deionized water are 2000ml, a water are changed every 5 minutes, cleaning is twice;
8, PH is adjusted: slowly being instilled in slurry using 25% ammonium hydroxide, is made its PH=5.0~6.0, one until precipitating, is added
When slurry revolving speed 300rpm;
9, it washes: upper step slurry being stood into washing twice, makes its PH up to 5.0~6.0;
10, KB disperses: according to powder: water: small abrading-ball: big abrading-ball=1:3:1:1.8 carries out ball milling 14h to powder, makes it
Particle size reduction is simultaneously more uniform;
11, water sieve: the sieve for the powder 850um that ball milling terminates removes thick ion;
12, it is dehydrated, is dried to obtain lanthanum-cerium-terbium phosphate green emitting phosphor.
Embodiment 2
It is as follows to prepare lanthanum-cerium-terbium phosphate green emitting phosphor of the invention:
1, by La3+、Ce3+、Tb3+Lanthanum cerium terbium proportionally, which is mixed to get, for 12:5:1 is co-precipitated body;
2,569g body, 56.9g boric acid, 17.24g lithium tetraborate, 11.38g aluminium oxide will be co-precipitated to be put into blender,
Revolving speed is 200rpm, and time 10min, powder color is white;
3,600g powder finely dispersed in 2 is fitted into polybag, is then charged into alumina crucible;
4, it is put into firing furnace, firing time 7h, temperature is 1300 DEG C, and is passed through 7% hydrogen and 93% nitrogen;
5, it crushes: powder 600g, water 1500g, abrading-ball 900g after firing being fitted into magnetic bucket and stir 12h, revolving speed is
36rpm;
6, thick ion water sieve: is removed by the sieve of 850um;
7, slurried: powder and the total volume of deionized water are 2000ml, a water are changed every 5 minutes, cleaning is twice;
8, PH is adjusted: slowly being instilled in slurry using 25% ammonium hydroxide, is made its PH=5.0~6.0, one until precipitating, is added
When slurry revolving speed 300rpm;
9, it washes: upper step slurry being stood into washing twice, makes its PH up to 5.0~6.0;
10, KB disperses: according to powder: water: small abrading-ball: big abrading-ball=1:3:1:1.8 carries out ball milling 14h to powder, makes it
Particle size reduction is simultaneously more uniform;
11, water sieve: the sieve for the powder 850um that ball milling terminates removes thick ion;
12, it is dehydrated, is dried to obtain lanthanum-cerium-terbium phosphate green emitting phosphor.
Further to verify technical effect of the invention, the following experiment test of progress:
One, influence of the use of plastic foil to product yield
The yield of the product being prepared of above-described embodiment 1 and 2 is tested in this experiment, wherein chromaticity coordinates (x, y),
Horizontal axis is x, longitudinal axis y;Br represents relative luminance (relative brightness), and test result is as shown in Table 1 below:
Table 1
Content | x | y | Br | Yield |
Embodiment 1 does not add polybag | 0.3612 | 0.5740 | 103.5 | 91.5% |
Polybag is added in embodiment 1 | 0.3609 | 0.5741 | 103.6 | 97.5% |
Embodiment 2 does not add polybag | 0.3611 | 0.5740 | 103.6 | 92% |
Polybag is added in embodiment 2 | 0.3610 | 0.5740 | 103.5 | 98% |
Conclusion: according to embodiment 1 and example 2, polybag is not added and polybag is added for fluorescent powder chromaticity coordinates and opposite
Brightness does not influence substantially, but addition polybag can greatly promote yield.
Two, influence of the auxiliary agent to experimental result
On the basis of this test result is according to the operation of embodiment 1, makees following be adaptively adjusted and tested, in which: control
Experimental group 1 is no added auxiliary agent group;Control experiment group 2 is that added auxiliary agent replaces with all addition lithium tetraborates;To according to the facts
It tests group 3 and replaces with addition lithium tetraborate and mebor for added auxiliary agent, the proportion of the mixture is lithium tetraborate: boron
Acid=3:10;Control experiment group 4 is that added auxiliary agent replaces with all addition aluminium oxide;Control experiment group 5 is added
Auxiliary agent replaces with addition lithium tetraborate and alumina mixture, and the proportion of the mixture is lithium tetraborate: aluminium oxide=3:2;It is right
It is that added auxiliary agent replaces with addition aluminium oxide and mebor according to experimental group 6, the proportion of the mixture is aluminium oxide: boron
Acid=1:5.Wherein D50Central particle diameter distribution is represented, experimental result is shown in Table shown in 2:
Table 2
Content | x | y | Br | D50 |
Control experiment group 1 | 0.3599 | 0.5740 | 88.1 | 3.0 |
Control experiment group 2 | 0.3610 | 0.5740 | 90.2 | 3.2 |
Control experiment group 3 | 0.3611 | 0.5738 | 94.0 | 7.5 |
Control experiment group 4 | 0.3610 | 0.5739 | 92.6 | 3.5 |
Control experiment group 5 | 0.3610 | 0.5740 | 98.3 | 4.5 |
Control experiment group 6 | 0.3610 | 0.5741 | 93.5 | 6.0 |
Embodiment 1 | 0.3610 | 0.574 | 103.6 | 4.0 |
Conclusion: according to control experiment group 1~6, it is known that there is no variations substantially for chromaticity coordinates (x, y), therefore add difference and help
Agent does not influence the chromaticity coordinates of fluorescent powder substantially, and has a great impact to brightness.It wherein, can according to control experiment 1 and 2
Know, lithium tetraborate, which is added, can be improved brightness and increase partial size;Partial size can be made to become it is found that boric acid is added according to control experiment 2 and 3
Greatly, it is more harder than 2 silty of control experiment to make fluorescent powder;According to control experiment 1,4 and 5 it is found that aluminium oxide, which is added, can increase partial size
And keep partial size more uniform, to improve brightness;According to control experiment 3,5,6 and embodiment 1 it is found that three kinds of auxiliary agent timeliness are added
Fruit is best.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of fluorescent powder, which is characterized in that plastic foil is set between the raw material of fluorescent powder and crucible, then
It carries out heating and fires fluorescent powder;The raw material for preparing fluorescent powder are isolated with crucible using plastic foil, then carry out heating fire it is glimmering
Light powder avoids fluorescent powder raw material from directly contacting with crucible and causes to bond.
2. the preparation method of fluorescent powder according to claim 1, which is characterized in that during preparing fluorescent powder, plastics
Film can be to melt volatilization at 600~800 DEG C of higher temperature, will not remain in fluorescent powder finished product.
3. a kind of preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor characterized by comprising
S1, the method using co-precipitation, mixed metal La3+、Ce3+、Tb3+Obtain lanthanum cerium terbium co-precipitation body;
S2, lanthanum cerium terbium co-precipitation body is fired by being placed in crucible after plastic foil isolation;
S3, the product after firing is post-processed up to lanthanum-cerium-terbium phosphate green emitting phosphor.
4. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 3, which is characterized in that further include helping
Agent, the auxiliary agent and the co-precipitation bluk recombination of lanthanum cerium terbium form mixed powder;The auxiliary agent is boric acid, in lithium tetraborate, aluminium oxide
It is one or more.
5. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 4, which is characterized in that
The ratio between the boric acid and lanthanum cerium terbium co-precipitation weight are added as 1:9~11;
The ratio between the lithium tetraborate and lanthanum cerium terbium co-precipitation weight are added as 1:30~38;
The ratio between the aluminium oxide and lanthanum cerium terbium co-precipitation weight are added as 1:50~60.
6. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 1, which is characterized in that fired described in S2
In the process, it is passed through under 7~10% hydrogen and 93~90% nitrogen, the firing time is 6.5h~7.5h, and temperature is 1300~1400
℃。
7. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 1, which is characterized in that the post-processing
Process includes crushing, water sieve, slurried, PH adjustment, sieving, dry, acquisition lanthanum-cerium-terbium phosphate green emitting phosphor.
8. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 7, which is characterized in that adjust it in PH
Afterwards, further include ball milling before sieving, make its particle size reduction and more uniform.
9. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 7, which is characterized in that the crushing is
Fluorescent powder, water, abrading-ball mass ratio be 1:2~3:1~2 under crushed.
10. the preparation method of lanthanum-cerium-terbium phosphate green emitting phosphor according to claim 7, which is characterized in that the slurry
It turns to and adds deionized water submergence in powder, a water was changed every 5~10 minutes, clean 3~5 times.
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Cited By (1)
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CN112410023A (en) * | 2020-11-23 | 2021-02-26 | 广州珠江光电新材料有限公司 | Europium-excited strontium borate ultraviolet fluorescent powder and preparation method thereof |
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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 |
CN106367067A (en) * | 2016-08-30 | 2017-02-01 | 内蒙古科技大学 | Aluminate blue fluorescent powder and preparation method thereof |
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2019
- 2019-03-05 CN CN201910165523.4A patent/CN109913216A/en active Pending
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Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN106367067A (en) * | 2016-08-30 | 2017-02-01 | 内蒙古科技大学 | Aluminate blue fluorescent powder and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112410023A (en) * | 2020-11-23 | 2021-02-26 | 广州珠江光电新材料有限公司 | Europium-excited strontium borate ultraviolet fluorescent powder and preparation method thereof |
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