CN103756666A - Red phosphor for plasma and preparation method thereof - Google Patents
Red phosphor for plasma and preparation method thereof Download PDFInfo
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- CN103756666A CN103756666A CN201110459900.9A CN201110459900A CN103756666A CN 103756666 A CN103756666 A CN 103756666A CN 201110459900 A CN201110459900 A CN 201110459900A CN 103756666 A CN103756666 A CN 103756666A
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Abstract
The invention discloses a red phosphor for plasma and a preparation method thereof. The red phosphor comprises a red phosphor raw material and a film coated over the outer surface of the red phosphor raw material. According to the invention, since the film is coated over the outer surface of the red phosphor raw material, the red phosphor has greatly improved bombardment resistance, so the service life of the red phosphor is prolonged.
Description
Technical field
The present invention relates to the preparation field of gas discharge device, in particular to red fluorescence powder and preparation method thereof for a kind of plasma body.
Background technology
Plasma flat-plate technique of display (Plasma Display Panel) is a kind of under driving circuit is controlled, utilize the ultraviolet ray (mainly in 147 nanometers and 172 nanometers) of xenon (Xe) base rare gas, mixed gas plasma discharge generation to excite the luminous a kind of flat panel display of three primary colors fluorescent powder, visual angle is wide owing to having for PDP, the life-span is long, refresh rate is fast, light efficiency and many good characteristics become the at present important giant-screen such as brightness is high, easily make giant-screen, working range is wide, ultra-thin display mode it
In recent years, along with plasma flat-panel display part is towards high definition, the future development of 3-D display (3D), fluorescent material as key part is also had higher requirement, require fluorescent material brightness high, particle diameter is little of to meet high definition pixel request, and short persistence is to meet motion picture 3D display requirement, and the life-span is long, resistance to ion bombardment.Generally speaking, reach good 3D display effect, require 10% decay of fluorescent material can not be longer than 4 milliseconds time of persistence.Commercial PDP is long time of persistence with borate rouge and powder at present, and colour purity is not good enough, alum phosphoric acid salt rouge and powder low lightness, and the rare earth oxide rouge and powder life-span is poor, not resistance to bombardment.
Summary of the invention
The present invention aims to provide red fluorescence powder and preparation method thereof for a kind of plasma body, to solve poor technical problem of red fluorescence powder life-span for prior art applying plasma.
To achieve these goals, according to an aspect of the present invention, provide a kind of plasma body red fluorescence powder.This red fluorescence powder comprises red fluorescence powder raw material and is coated on the film of red fluorescence powder raw material outside surface.
Further, film contains MgF
2, MgO, Al
2o
3, or SiO
2in one or more.
Further, the chemical formula of red fluorescence powder raw material is (Y
1-x-y-zln
xr
yeu
z)
2o
3, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, R is basic metal or alkaline-earth metal.
According to another aspect of the present invention, provide the preparation method of a kind of plasma body with red fluorescence powder.This preparation method comprises the preparation of red fluorescence powder raw material and the processing of the coating of red fluorescence powder raw material, wherein, coating is processed and is comprised the following steps: red fluorescence powder raw material is placed in to polyglycol solution, adopt sol-gel method film former to be coated on phosphor surface, through stirring, filter, be dried to obtain plasma body red fluorescence powder.
Further, in the film of generation, contain MgF
2, MgO, Al
2o
3, or SiO
2in one or more particles
Further, the molecular weight of polyoxyethylene glycol is 10000-40000.
Further, stir as carrying out magnetic agitation in the temperature range at 50-150 ℃.
Further, the preparation of red fluorescence powder raw material comprises the following steps: 1) according to chemical formula (Y
1-x-y-zln
xr
yeu
z)
2o
3in the mol ratio of each element take Y
2o
3, Ln
2o
3, Eu
2o
3and containing R compound, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, is selected from one or more in rare earth oxide, alkaline carbonate, alkaline metal fluoride cpd containing R compound; 2) above-mentioned each feed composition taking being added to water mixes, drying, sieve after in 900-1400 ℃ of pre-burning 1～10 hour, products therefrom again in 900-1400 ℃ of sintering 1～10 hour, and then makes red fluorescence powder raw material through grinding, washing, filtration, baking step after grinding.
Plasma body red fluorescence powder of the present invention, due to red fluorescence powder raw material outside surface be also coated with film, improved greatly the resistance to bombardment performance of red fluorescence powder, thereby extended its work-ing life; Particularly in film, contain MgF
2, MgO, Al
2o
3, or SiO
2in one or more time, the improvement of its performance is particularly remarkable.
Embodiment
It should be noted that, in the situation that not conflicting, embodiment and the feature in embodiment in the present invention can combine mutually.Below in conjunction with embodiment, describe the present invention in detail.
According to a kind of typical embodiment of the present invention, this plasma body comprises red fluorescence powder raw material with red fluorescence powder and is coated on the film of red fluorescence powder raw material outside surface.Plasma body red fluorescence powder of the present invention, the also coated film due to red fluorescence powder raw material outside surface, has improved greatly the resistance to bombardment performance of red fluorescence powder, thereby has extended its work-ing life; Particularly in film, contain MgF
2, MgO, Al
2o
3, or SiO
2in one or more time, the improvement of its performance is particularly remarkable.
Preferably, the chemical formula of red fluorescence powder raw material is (Y
1-x-y-zln
xr
yeu
z)
2o
3, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, R is basic metal or alkaline-earth metal.There is the fluorescent material of this kind of component to have stronger absorption at 147nm and 172nm place (especially 172nm), and under 147nm and 172nm optical excitation, have the stronger red light transmitting that is positioned at 618nm left and right, meet the requirement of PDP application.
According to a kind of typical embodiment of the present invention, this plasma body comprises the preparation of red fluorescence powder raw material and the processing of the coating of red fluorescence powder raw material by the preparation method of red fluorescence powder, wherein, coating is processed and is comprised the following steps: red fluorescence powder raw material is placed in to polyglycol solution, with sol-gel method film former, be coated on phosphor surface, through stirring, filter, be dried to obtain plasma body red fluorescence powder.
Preferably, in the film of generation, contain MgF
2, MgO, Al
2o
3, or SiO
2in one or more particles.Preferably, the molecular weight of polyoxyethylene glycol is 10000-40000.It is large that polyoxyethylene glycol in this molecular weight ranges has molecular weight, and density is high, and the characteristic to the good dispersity of fluorescent material, for disperseing fluorescent material, is beneficial to and forms its MgF
2, MgO, A1
2o
3, SiO
2deng particle film, be coated on phosphor surface, can improve significantly its resistance to bombardment performance.Stir as to carry out magnetic agitation in the temperature range of 50-150 ℃, be beneficial to the carrying out of coating reaction.
According to a kind of typical embodiment of the present invention, the preparation of red fluorescence powder raw material comprises the following steps: 1) according to chemical formula (Y
1-x-y-zln
xr
yeu
z)
2o
3in the mol ratio of each element take Y
2o
3, Ln
2o
3, Eu
2o
3and containing R compound, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, is selected from one or more in rare earth oxide, alkaline carbonate, alkaline metal fluoride cpd containing R compound; 2) above-mentioned each feed composition taking being added to water mixes, drying, sieve after in 900-1400 ℃ of pre-burning 1～10 hour, products therefrom again in 900-1400 ℃ of sintering 1～10 hour, and then makes red fluorescence powder raw material through grinding, washing, filtration, baking step after grinding.The red fluorescence powder raw material standby according to this legal system not only has stronger absorption at 147nm and 172nm place (especially 172nm), and the sunset glow time reach 3-4ms, its manufacture craft is simple, easy handling, advantages of nontoxic raw materials, environmental protection.
Below in conjunction with embodiment, further illustrate beneficial effect of the present invention.
Embodiment 1
First by mole% by 70% yttrium oxide, 10% gadolinium sesquioxide, 10% Quilonum Retard, 10% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 1 hour, after the powder of pre-burning is ground, through 1100 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 2
First by mole% by 70% yttrium oxide, 10% gadolinium sesquioxide, 10% Quilonum Retard, 10% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1200 ℃, burn and within 1 hour, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 3
First by mole% by 70% yttrium oxide, 10% gadolinium sesquioxide, 10% Quilonum Retard, 10% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 2 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 8 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 4
First by mole% by 70% yttrium oxide, 10% gadolinium sesquioxide, 10% Quilonum Retard, 10% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 8 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 5 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 90 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 5
First by mole% by 70% yttrium oxide, 10% gadolinium sesquioxide, 10% Quilonum Retard, 10% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 5 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 3 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 120 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 6
First by mole% by 85% yttrium oxide, 5% gadolinium sesquioxide, 5% magnesium oxide, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 7 hours, after the powder of pre-burning is ground, through 1100 ℃, burn and within 3 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 7
First by mole% by 85% yttrium oxide, 5% gadolinium sesquioxide, 5% sodium carbonate, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 2 hours, after the powder of pre-burning is ground, through 1200 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 8
First by mole% by 85% yttrium oxide, 5% gadolinium sesquioxide, 5% Quilonum Retard, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 6 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 4 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 9
First by mole% by 85% yttrium oxide, 5% gadolinium sesquioxide, 5% Quilonum Retard, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 90 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 10
First by mole% by 85% yttrium oxide, 5% gadolinium sesquioxide, 5% Quilonum Retard, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drops in mixer, then mixes after adding water, by the raw material drying mixing, sieve, through 900 ℃ of high temperature pre-burnings 9 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 9 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 120 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Implement 11
First by mole% by 85% yttrium oxide, 10% gadolinium sesquioxide, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drop in mixer, after adding water, mix, the raw material drying by mixing, sieves again, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1100 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 12
First by mole% by 85% yttrium oxide, 10% gadolinium sesquioxide, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drop in mixer, after adding water, mix, the raw material drying by mixing, sieves again, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1200 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 13
First by mole% by 85% yttrium oxide, 10% gadolinium sesquioxide, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drop in mixer, after adding water, mix, the raw material drying by mixing, sieves again, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 80 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 14
First by mole% by 85% yttrium oxide, 10% gadolinium sesquioxide, 5% europium sesquioxide is mixed into the raw material of fluorescent material, then drop in mixer, after adding water, mix, the raw material drying by mixing, sieves again, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1300 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 90 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
Embodiment 15
First by mole% by 99% yttrium oxide, 0.5% gadolinium sesquioxide, 0.5% europium sesquioxide is mixed into the raw material of fluorescent material, then drop in mixer, after adding water, mix, the raw material drying by mixing, sieves again, through 900 ℃ of high temperature pre-burnings 10 hours, after the powder of pre-burning is ground, through 1400 ℃, burn and within 10 hours, become powder agglomates again; After the powder agglomates burning till is sieved, drop into disperse in bottle, through Ball milling, wash, be drying to obtain fluorescent material, the fluorescent material making is put into polyglycol solution, under 120 ℃ of magnetic agitation, the MgF generating with sol-gel method
2, MgO, Al
2o
3, SiO
2deng particle, be coated on phosphor surface, after filtration, obtain the red fluorescence powder of coating after dry.
The red fluorescence powder that above-described embodiment 1-15 is made, carries out the mensuration of correlated performance parameter, and result is as follows:
1. fluorescent material of the present invention has stronger absorption at 147nm and 172nm place (especially 172nm), and under 147nm and 172nm optical excitation, there is the stronger red light transmitting that is positioned at 618nm left and right, show that the vacuum-ultraviolet light that this fluorescent material can be produced by the xenon base rare gas plasma discharge in the PDP device of main application at present efficiently excites, and meets the requirement of PDP application.
2. as a comparison,, under identical test condition, vacuum tightness is greater than 1 * 10
-3pa, the emmission spectrum demonstration under 172nm optical excitation, the fluorescent material sunset glow time of the present invention reaches 3-4ms, far below borate rouge and powder 8-10ms and alum phosphoric acid salt rouge and powder 6-7ms.
3, as a comparison, under identical test condition, vacuum tightness is greater than 1 * 10
-3pa, the emmission spectrum demonstration under 172nm optical excitation, the resistance to ion bombardment of fluorescent material of the present invention is far above the rouge and powder that does not carry out coating processing, and life is more than 20%.
And fluorescent material synthesis step of the present invention is simple, easy handling, advantages of nontoxic raw materials, environmental protection.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a plasma body red fluorescence powder, is characterized in that, comprises red fluorescence powder raw material and is coated on the film of described red fluorescence powder raw material outside surface.
2. red fluorescence powder according to claim 1, is characterized in that, described film contains MgF
2, MgO, Al
2o
3, or SiO
2in one or more.
3. red fluorescence powder according to claim 1, is characterized in that, the chemical formula of described red fluorescence powder raw material is (Y
1-x-y-zln
xr
yeu
z)
2o
3, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, R is basic metal or alkaline-earth metal.
4. a preparation method for the use of the plasma body described in any one red fluorescence powder in claim 1-3, is characterized in that, comprises the preparation of red fluorescence powder raw material and the processing of the coating of red fluorescence powder raw material, and wherein, described coating is processed and comprised the following steps:
Described red fluorescence powder raw material is placed in to polyglycol solution, adopts sol-gel method film former to be coated on phosphor surface, through stirring, filter, be dried to obtain described plasma body red fluorescence powder.
5. preparation method according to claim 4, is characterized in that, in the described film of generation, contains MgF
2, MgO, Al
2o
3, or SiO
2in one or more particles.
6. preparation method according to claim 4, is characterized in that, the molecular weight of described polyoxyethylene glycol is 10000-40000.
7. preparation method according to claim 4, is characterized in that, described stirring for carrying out magnetic agitation in the temperature range of 50-150 ℃.
8. preparation method according to claim 4, is characterized in that, the preparation of described red fluorescence powder raw material comprises the following steps:
1) according to chemical formula (Y
1-x-y-zln
xr
yeu
z)
2o
3in the mol ratio of each element take Y
2o
3, Ln
2o
3, Eu
2o
3and containing R compound, wherein, 0.005≤x≤0.10,0.00≤y≤0.10,0.005≤z≤0.10, is describedly selected from one or more in rare earth oxide, alkaline carbonate, alkaline metal fluoride cpd containing R compound;
2) above-mentioned each feed composition taking being added to water mixes, drying, sieve after in 900-1400 ℃ of pre-burning 1～10 hour, products therefrom again in 900-1400 ℃ of sintering 1～10 hour, and then makes described red fluorescence powder raw material through grinding, washing, filtration, baking step after grinding.
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|---|---|---|---|
| CN201110459900.9A CN103756666A (en) | 2011-12-31 | 2011-12-31 | Red phosphor for plasma and preparation method thereof |
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| CN104357043A (en) * | 2014-11-24 | 2015-02-18 | 北京大学工学院包头研究院 | Fluorescent material as well as preparation method and application thereof |
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Application publication date: 20140430 |