CN102134488B - Vacuum ultraviolet induced high colour purity red phosphor and preparation method thereof - Google Patents
Vacuum ultraviolet induced high colour purity red phosphor and preparation method thereof Download PDFInfo
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- CN102134488B CN102134488B CN2010101031920A CN201010103192A CN102134488B CN 102134488 B CN102134488 B CN 102134488B CN 2010101031920 A CN2010101031920 A CN 2010101031920A CN 201010103192 A CN201010103192 A CN 201010103192A CN 102134488 B CN102134488 B CN 102134488B
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Abstract
The invention provides vacuum ultraviolet induced high colour purity red phosphor. The concrete chemical formula of phosphor is as follows: M (1plus x) M' (1 minus 2x) BP208: Eux, wherein x is more than 0 and less than or equal to 0.3, M is one or several of Li, Na and K, and the M' is one or several of Ba, Sr and Ca. The invention also provides a method for preparing the red phosphor, comprising the following steps: firstly, weighing corresponding raw materials according to the weight ratio expressed in the chemical formula; secondly, carrying out high-temperature roasting on the raw materials and rinsing coasted materials; and thirdly, carrying out separation, filtration, size grading and drying on the rinsed materials to obtain the vacuum ultraviolet induced high colour purity red phosphor having good colour purity and stable chemical property.
Description
Technical field
The present invention relates to fluorescent material of a kind of vacuum ultraviolet (VUV) optical excitation and preparation method thereof, relate in particular in a kind of plasma display and adopt the red integral part in three primary colors fluorescent powder.
Background technology
At present, in fierce market competition, traditional cathode-ray tube display has been faded in declining trend, the substitute is frivolous with the bodily form, without X-radiation, the famous flat-panel monitor of advantage such as low in energy consumption.Wherein the display effect of plasma flat-panel display is particularly outstanding, has that high-contrast, color reducibility are good, gray scale abundant and the advantage such as fast response time, in global large screen television market in occupation of absolute predominance.The principle of luminosity of plasma display is to utilize the noble gas discharge such as Xe or Xe-He, become isoionic state, give off the vacuum ultraviolet ray of 147nm and 172nm, ultraviolet ray excitedly be coated on the fluorescent material of inwall and send red, green, blue three primary colours light, control and just can realize colored the demonstration by spacing color mixed and circuit.
The red fluorescence powder that current plasma display is used is (Y, Gd) BO
3: Eu
3+, but due at (Y, Gd) BO
3: Eu
3+In crystalline structure, Eu
3+Be in highly centrosymmetric position, make its emission main peak be positioned at 593nm (corresponding to Eu
3+ 5D
0→
7F
1Transition), color is orange partially, and purity of color is far below the NTSC standard, yet the purity of color of fluorescent material is the principal element that affects the panchromatic demonstration of display device.Therefore, the purity of color of raising red fluorescence powder is one of key of improving the Plasmia indicating panel display quality.For improving the purity of color of rouge and powder, people have made very large effort, adopt Y if any the people
2O
3: Eu
3+Substitute (Y, Gd) BO
3: Eu
3+, Y
2O
3: Eu
3+The emission main peak be positioned at 611nm (corresponding to Eu
3+ 5D
0→
7F
2Transition), purity of color is better, but not enough (Y, the Gd) BO of its luminous efficiency
3: Eu
3+60%.
Summary of the invention
The purpose of the embodiment of the present invention is to provide that a kind of purity of color is good, the vacuum ultraviolet-excited high color purity red fluorescence powder of stable chemical performance.
The embodiment of the present invention is achieved in that the concrete chemical formula of described red fluorescence powder is: M
(1+x)M '
(1-2x)BP
2O
8: Eu
x, 0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca.The span of described x is preferably 0.005≤x≤0.2.
Another purpose of the embodiment of the present invention is also to provide the preparation method of above-mentioned red fluorescence powder, comprises the steps:
1), by chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xComposition metering than after the former abrasive lapping taken, mixing, 0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca;
2), by the at high temperature roasting of above-mentioned mixed material, and the material after sintering is washed;
3), will wash after material carry out separating and filtering, then according to its size classification;
4), the drying materials after classification is processed after, namely obtain the high color purity red fluorescence powder.
Compare to prior art, technical solution of the present invention has following technique effect:
(1) red fluorescence powder emission main peak of the present invention is positioned at 611nm, has good purity of color;
(2) red fluorescence powder of the present invention has stronger emission under the vacuum ultraviolet (VUV) optical excitation, is well suited for for Plasmia indicating panel and non-mercury florescent lamp;
(3) red fluorescence powder chemical property of the present invention is highly stable, and after bubble, heat etc. were processed, its performance did not change substantially;
(4) red fluorescence powder, preparation method thereof of the present invention is simple, cost is low, be easy to realize industrialization.
Red fluorescence powder of the present invention is well suited for vacuum ultraviolet (VUV) and burst of ultraviolel, has good purity of color, and chemical stability is good, therefore can be widely used in Plasmia indicating panel and non-mercury florescent lamp.
The accompanying drawing explanation
Fig. 1 is the utilizing emitted light spectrogram of the embodiment of the present invention 5;
Fig. 2 is red G and red R, blue B fluorescent material form in XYZ chromaticity diagram RGB colour triangle, and wherein sequence number 11 is (Y, Gd) BO
3: Eu
3+RGB colour triangle with red G, blue B fluorescent material formation; Sequence number 22 is the RGB colour triangle that the embodiment of the present invention 5 and red G, blue B fluorescent material form.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of vacuum ultraviolet-excited high color purity red fluorescence powder, and the concrete chemical formula of described red fluorescence powder is: M
(1+x)M '
(1-2x)BP
2O
8: Eu
x, 0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca.
The span of described x is preferably 0.005≤x≤0.2.
Above-mentioned chemical structure is mainly by BO
4And PO
4Form, M and M ' chaotic distribution in lattice, have the center of asymmetry structure, so after the Eu3+ doping enters in lattice, can be under the vacuum ultraviolet (VUV) optical excitation, by the transmission ofenergy of matrix absorption to luminescence center Eu
3+, by Eu
3+Produce red emission, with
5D0-
7F
2The transition red-emitting is main, can demonstrate good purity of color.
That the present invention adopts is a class trivalent rare earth ions Eu
3+The borophosphate red fluorescence powder activated, due to Eu
3+While being in strict inversion center of symmetry, with
5D
0-
7F
1It is main that light is sent out in transition orange, works as Eu
3+While being in low symmetry centre case, with
5D
0-
7F
2The transition red-emitting is main, and therefore, the borophosphate of selecting to have low symmetry centre case, as matrix, passes through Eu
3+Doping enters the low symmetrical case center in borophosphate, thereby obtains having the red fluorescence powder of high color purity.
In the present invention's chromaticity diagram shown in Figure 2, with red fluorescence powder (Y, the Gd) BO of current commercialization
3: Eu
3+Compare, red fluorescence powder chromaticity coordinates x value of the present invention is large, and chromaticity coordinates y value is little, wider with colour triangle area blue and that red fluorescence powder forms, thereby can be so that the presenting property of color of display device is better.Simultaneously, boron oxygen tetrahedron group and phosphorus oxygen tetrahedron group all have stronger absorption at the vacuum ultraviolet (VUV) wave band, so the present invention has stronger emission under the vacuum ultraviolet (VUV) optical excitation, are suitable for plasma display and use.
The preparation method of above-mentioned red fluorescence powder, comprise the steps:
1), by chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xComposition metering than after the former abrasive lapping taken, mixing, namely the molar ratio according to respective element in the said structure formula takes.0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca;
2), by the at high temperature roasting of above-mentioned mixed material, and the material after sintering is washed;
3), will wash after material carry out separating and filtering, then according to its size classification;
4), the drying materials after classification is processed after, namely obtain the high color purity red fluorescence powder.
Wherein, raw material described step 1) is compound or the simple substance that contains Li, the compound that contains Na or simple substance, the compound that contains K or simple substance, the compound that contains Ba or simple substance, the compound that contains Sr or simple substance, the compound that contains Ca or simple substance, the compound that contains B or simple substance, the compound that contains P or simple substance, the compound that contains Eu or simple substance.
The compound of the described Li of containing, Na, K can be preferably carbonate, nitrate, oxalate, the oxyhydroxide of Li, Na, K; The compound of the described Ba of containing, Sr, Ca is preferably carbonate, nitrate, oxalate, the oxyhydroxide of Ba, Sr, Ca; Described preferred its oxide compound of compound, acid or the salt that contains B, P; Described oxide compound or the salt that contains the preferred Eu of compound of Eu.
In described step 2) in, high-temperature roasting is that former abrasive lapping is fully mixed and is placed in box-type high-temperature furnace, can under any one atmosphere in air, nitrogen, hydrogen or CO (carbon monoxide converter) gas, carry out, or carry out under the mixed atmosphere of nitrogen and hydrogen, and at high temperature roasting 1-3 time, it is each that roasting is complete carries out subsequent processing after being cooled to room temperature again, each maturing temperature is 400-1300 ℃, preferred 800-1000 ℃, the time is 1-24 hour, preferably 10-16 hour.
In described step 2) in, washing is to adopt a kind of in deionized water or dehydrated alcohol or two kinds.
Described step 3) separating and filtering comprises a kind of in Büchner funnel suction filtration, vacuum filtration, centrifuging, with other impurity of screening and separating; Size classification is to adopt air classification or liquid hierarchical approaches to sub-elect 1-10 micron powder, and preferred size is the 2-6 micron.
Described step 4) bake out temperature is 60-160 ℃, is preferably 80-120 ℃.
Below by a plurality of embodiment, illustrate the borophosphate green emitting phosphor difference form and the preparation method, and the aspect such as performance.
Embodiment 1: consist of Na
1.002Ba
0.996BP
2O
8: Eu
0.002Red fluorescence powder
Press chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.002, M are Na, and M ' is Ba, and then the metering ratio according to above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, BaCO
3, Na
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 24 hours under 400 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 800 ℃
2/ H
2=95: 5) lower sintering is 24 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 8-10 micron, finally under 60 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 2: consist of K
1.05Sr
0.9BP
2O
8: Eu
0.05Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.05, M are K, and M ' is Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, SrCO
3, K
2CO
3, Eu
2O
3Raw material, after grinding and fully mixing, first sintering 20 hours under 600 ℃ of air atmospheres, take out mix grinding even, and then in reducing atmosphere (the volume ratio N of 800 ℃
2/ H
2=95: 5) lower sintering is 18 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after the Büchner funnel suction filtration carrying out the liquid classification, chooses the powder that granularity is the 5-7 micron, finally under 100 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 3: consist of Li
1.15Ca
0.7BP
2O
8: Eu
0.15Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.15, M are Li, and M ' is Ca, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, CaCO
3, Li
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 18 hours under 800 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 850 ℃
2/ H
2=95: 5) lower sintering is 15 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, finally under 120 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 4: consist of Li
0.3KSr
0.4BP
2O
8: Eu
0.3Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.3, M are that Li, K, M ' are Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, CaCO
3, Li
2CO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 15 hours under 1000 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 750 ℃
2/ H
2=95: 5) lower sintering is 10 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after vacuum filtration carrying out the liquid classification, chooses the powder that granularity is the 4-6 micron, finally under 140 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 5: consist of K
1.08Sr
0.62Ba
0.22BP
2O
8: Eu
0.08Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.08, M are K, and M ' is Sr, Ba, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, BaCO
3, SrCO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 10 hours under 1000 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 1000 ℃
2/ H
2=95: 5) lower sintering is 8 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 3-5 micron, finally under 120 ℃, dries and obtains the PDP red fluorescence powder.
As shown in Figure 1, the red fluorescence powder excitation wavelength of the present embodiment is 172nm.
Embodiment 6: consist of NaK
0.2Sr
0.6BP
2O
8: Eu
0.2Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.2, M are Na, K, and M ' is Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, SrCO
3, Na
2CO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 4 hours under 1100 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 1000 ℃
2/ H
2=95: 5) lower sintering is 2 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 2-4 micron, finally under 100 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 7: consist of Li
0.3K
0.8Sr
0.6Ba
0.2BP
2O
8: Eu
0.1Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.1, M are that Li, K, M ' are Sr, Ba, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, SrCO
3, BaCO
3, Li
2CO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 4 hours under 400 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 1000 ℃
2/ H
2=95: 5) lower sintering is 2 hours, naturally cools to room temperature, uses deionized water wash after the taking-up porphyrize, carries out the laggard row air classification of centrifuging, chooses the powder that granularity is the 4-6 micron, finally under 100 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 8: consist of Na
0.02KSr
0.7Ca
0.26BP
2O
8: Eu
0.02Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.02, M are that Na, K, M ' are Sr, Ca, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, H
3BO
3, SrCO
3, CaCO
3, Na
2CO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 1 hour under 1300 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 1000 ℃
2/ H
2=95: 5) lower sintering is 2 hours, naturally cools to room temperature, uses absolute ethanol washing after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 3-5 micron, finally under 160 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 9: consist of Li
0.03Na
0.2K
0.8Ba
0.5Sr
0.3Ca
0.14BP
2O
8: Eu
0.03Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.03, M are Li, Na, K, and M ' is Ba, Sr, Ca, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, B
2O
3, SrCO
3, CaCO
3, Na
2CO
3, K
2CO
3, Eu
2O
3After former abrasive lapping fully mixed, first sintering 1 hour under 900 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 750 ℃
2/ H
2=95: 5) lower sintering is 24 hours, naturally cools to room temperature, uses absolute ethanol washing after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 1-3 micron, finally under 160 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 10: consist of Li
0.15K
0.9Ba
0.2Sr
0.7BP
2O
8: Eu
0.05Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)B P
2O
8: Eu
xPrepare burden, wherein: X=0.05, M are that Li, K, M ' are Ba, Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes P
2O
5, B
2O
3, BaCO
3, SrCO
3, Li
2CO
3, K
2CO
3, EuCO
3After former abrasive lapping fully mixed, first sintering 1 hour under 650 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 900 ℃
2/ H
2=95: 5) lower sintering is 6 hours, naturally cools to room temperature, uses absolute ethanol washing after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 4-6 micron, finally under 160 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 11: consist of Li
0.2Na
0.12K
0.8Sr
0.76BP
2O
8: Eu
0.12Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.12, M are Li, Na, K, and M ' is Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes (NH
4)
2HPO
4, B
2O
3, BaCO
3, SrCO
3, CaCO
3, Li
2CO
3, Na
2CO
3, K
2CO
3, EuC
2O
4After former abrasive lapping fully mixed, first sintering 1 hour under 1200 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 950 ℃
2/ H
2=95: 5) lower sintering is 12 hours, naturally cools to room temperature, uses absolute ethanol washing after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 3-5 micron, finally under 160 ℃, dries and obtains the PDP red fluorescence powder.
Embodiment 12: consist of Na
0.2KBa
0.3Sr
0.3BP
2O
8: Eu
0.2Red fluorescence powder
According to chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xPrepare burden, wherein: X=0.2, M are that Na, K, M ' are Ba, Sr, and then the stoichiometric ratio by above-mentioned chemical formula takes P
2O
5, B
2O
3, BaCO
3, SrCO
3, Na
2CO
3, K
2CO
3, EuNO
3After former abrasive lapping fully mixed, first sintering 1 hour under 500 ℃ of air atmospheres, took out mix grinding even, and then in reducing atmosphere (the volume ratio N of 1000 ℃
2/ H
2=95: 5) lower sintering is 8 hours, naturally cools to room temperature, uses absolute ethanol washing after the taking-up porphyrize, carries out after centrifuging carrying out the liquid classification, chooses the powder that granularity is the 4-5 micron, finally under 160 ℃, dries and obtains the PDP red fluorescence powder.
To sum up, the embodiment of the present invention adopts trivalent rare earth ions Eu
3+Make activator, work as Eu
3+While being in strict inversion center of symmetry, with
5D
0-
7F
1It is main that light is sent out in transition orange, works as Eu
3+While being in low symmetry centre case, with
5D
0-
7F
2The transition red-emitting is main, and therefore, the borophosphate of selecting to have low symmetry centre case, as matrix, passes through Eu
3+Doping enters the low symmetrical case center in borophosphate, thereby obtains having high color purity, the red fluorescence powder of stable chemical performance.Highly stable by the red fluorescence powder that preparation method of the present invention obtains, it is after bubble, heat etc. are processed, and its performance does not change substantially, and the preparation method is simple, cost is low, is easy to realize industrialization.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a vacuum ultraviolet-excited high color purity red fluorescence powder, is characterized in that, the concrete chemical formula of described fluorescent material is: M
(1+x)M '
(1-2x)BP
2O
8: Eu
x, 0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca.
2. vacuum ultraviolet-excited high color purity red fluorescence powder according to claim 1, is characterized in that, the span of described x is preferably 0.005<x≤0.2.
3. the preparation method of a vacuum ultraviolet-excited high color purity red fluorescence powder, is characterized in that, comprises the steps:
1), by chemical formula M
(1+x)M '
(1-2x)BP
2O
8: Eu
xComposition metering than after the former abrasive lapping taken, mixing, 0<x≤0.3 wherein, M is one or more of Li, Na, K, M ' is one or more in Ba, Sr, Ca;
2), by above-mentioned mixed material first in air roasting in reducing atmosphere again, the temperature of described roasting is 400-1300 ℃, and the material after sintering is washed;
3), will wash after material carry out separating and filtering, then according to its size classification;
4), the drying materials after classification is processed after, namely obtain the high color purity red fluorescence powder.
4. vacuum ultraviolet-excited high color purity red fluorescence powder, preparation method thereof according to claim 3, is characterized in that, the span of described x is preferably 0.005<x≤0.2.
5. according to the described vacuum ultraviolet-excited high color purity red fluorescence powder, preparation method thereof of claim 3 or 4, it is characterized in that described step 1) raw material be the compound, the compound that contains Na that contain Li, in the compound that contains K a kind of and contain Ba compound, contain Sr compound, contain a kind of in the compound of Ca and contain B compound, contain the compound of P and contain the compound of Eu.
6. vacuum ultraviolet-excited high color purity red fluorescence powder, preparation method thereof according to claim 5, is characterized in that, the compound of the described Li of containing, Na, K is preferably carbonate, nitrate, oxalate, the oxyhydroxide of Li, Na, K; The compound of the described Ba of containing, Sr, Ca is preferably carbonate, nitrate, oxalate, the oxyhydroxide of Ba, Sr, Ca; Described preferred its oxide compound of compound, acid or the salt that closes B, P; Described oxide compound or the salt that contains the preferred Eu of compound of Eu.
7. the manufacture method of vacuum ultraviolet-excited high color purity red fluorescence powder according to claim 3, it is characterized in that, described step 2) high-temperature roasting in is first at air, under any one atmosphere in nitrogen, hydrogen or CO (carbon monoxide converter) gas, to carry out again, or carry out under the mixed atmosphere of nitrogen and hydrogen, and at high temperature roasting 1-3 time, each roasting time is 1-24 hour.
8. the manufacture method of vacuum ultraviolet-excited high color purity red fluorescence powder according to claim 3, is characterized in that described step 2) in washing be to adopt a kind of in deionized water or dehydrated alcohol or two kinds to wash.
9. the manufacture method of vacuum ultraviolet-excited high color purity red fluorescence powder according to claim 3, is characterized in that described step 3) separating and filtering comprises a kind of in vacuum filtration or centrifuging; Described step 3) size classification is to adopt air classification or liquid classification and sorting to go out 1-10 micron powder.
10. the manufacture method of vacuum ultraviolet-excited high color purity red fluorescence powder according to claim 3, is characterized in that described step 4) bake out temperature is 60-160 ℃.
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| CN2010101031920A CN102134488B (en) | 2010-01-26 | 2010-01-26 | Vacuum ultraviolet induced high colour purity red phosphor and preparation method thereof |
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| EP2447338B1 (en) * | 2010-10-26 | 2012-09-26 | Leuchtstoffwerk Breitungen GmbH | Borophosphate phosphor and light source |
| CN102660276A (en) * | 2012-04-20 | 2012-09-12 | 中国海洋大学 | Near ultraviolet stimulated borophosphate white light fluorescent powder and preparation method |
| CN109929553B (en) * | 2018-12-25 | 2021-12-24 | 云南大学 | Borophosphate orange-red fluorescent powder and preparation method and application thereof |
| CN109929555B (en) * | 2018-12-25 | 2022-01-18 | 云南大学 | White boron phosphate fluorescent powder and preparation method and application thereof |
| CN110003906A (en) * | 2019-02-18 | 2019-07-12 | 云南大学 | A kind of europium boron phosphorus doped hydrochlorate orange-red fluorescence powder and its preparation method and application |
| CN110003905A (en) * | 2019-04-04 | 2019-07-12 | 云南大学 | A kind of Pr activation borophosphate red fluorescence powder and preparation method thereof |
| CN110003904A (en) * | 2019-04-04 | 2019-07-12 | 云南大学 | A kind of Ce boron phosphorus doped hydrochlorate ultraviolet fluorescence powder and preparation method thereof |
| CN112094645A (en) * | 2020-09-30 | 2020-12-18 | 华南理工大学 | Eu doped2+Blue light fluorescent material, preparation method thereof and white light LED light-emitting device |
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| CN1814694A (en) * | 2005-02-02 | 2006-08-09 | 中国科学院上海硅酸盐研究所 | Rare-earth-mixed barium borophosphate flashing luminous material, its preparing method and use |
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