CN105331365A - Preparation method of LED fluorescent powder - Google Patents
Preparation method of LED fluorescent powder Download PDFInfo
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- CN105331365A CN105331365A CN201510829338.2A CN201510829338A CN105331365A CN 105331365 A CN105331365 A CN 105331365A CN 201510829338 A CN201510829338 A CN 201510829338A CN 105331365 A CN105331365 A CN 105331365A
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Abstract
The invention discloses a preparation method of LED fluorescent powder. The preparation method comprises the steps of respectively weighing corresponding raw materials according to the mole ratio of various components of the fluorescent powder needing to be prepared; adding a carbon-containing solid matter, wherein the carbon atom mole number of the carbon-containing solid matter is 1-10 times of the doping ion mole number of the fluorescent powder; adding a catalyst, wherein the addition quantity of the catalyst is 0.5 percent-5 percent of the mass of the raw materials; adding a fluxing agent, wherein the addition quantity of the fluxing agent is 0.5 percent-5 percent of the mass of the raw materials; then evenly mixing the materials, putting into a high-temperature crucible, arranging in a high-temperature atmosphere oven, introducing reducing gas with the hydrogen gas volume content of 0-5 percent to serve as reducing atmosphere, then heating to a resultant temperature of the fluorescent powder and keeping micro positive pressure 1-100kpa, after the heating is ended, cooling to room temperature under the reducing atmosphere, taking out, smashing, sieving, heat-cleaning, drying and porphyrizing, thus obtaining the fluorescent powder. By adopting the preparation method, the reducibility is good, and the content of hydrogen serving as the gas of the reducing atmosphere is reduced, so that the safety is increased in the preparation process.
Description
Technical field
The present invention relates to LED luminescent material field, particularly relate to a kind of preparation method of LED fluorescent powder.
Background technology
LED fluorescent powder is a kind of critical material in LED illumination, has been widely used at present in various LED illumination lamp, and the light that the monochromatic ray for being sent by LED converts other color to forms white light.
The fluorescent material color combinationally used with blue-ray LED has blue-greenish colour, green, yellow, orange, red etc., composition material mainly contains rear-earth-doped rare earth aluminate, alkaline-earth silicate and alkaline earth aluminium silicon nitride and oxynitride etc., these fluorescent material generally adopt high temperature solid state reaction to prepare, by fluorescent material composition each element compound solid material mixing together, then through high-temperature firing formed fluorescent material.In above-mentioned LED fluorescent powder composition, doping active ions (light emitting ionic) mainly contains Ce
3+, Eu
2+ion etc., and the composition compound of these low price ions is unstable, so the raw material that these active ions that adulterate use is Ce
4+, Eu
3+the compounds such as high valence ion.These high valence ions must carry out reduction could form Ce
3+, Eu
2+ion at a low price, so the process need of synthetizing phosphor powder carries out in reducing atmosphere.The effect of reducing atmosphere not only can make high valence ion reduce, and can also prevent that the high valence ion that is reduced is oxidized returns high valence ion state.
In the making processes of LED fluorescent powder, the reducing atmosphere of employing is generally hydrogen, decomposed ammonia, hydrogen and nitrogen mixture, hydrogen and argon gas gas mixture etc.In order to make doping active ions be reduced completely, even if the Ce of doping
4+or Eu
3+ion Restore All becomes Ce
3+or Eu
2+ion at a low price, need the high hydrogen content gas adopting pure hydrogen or hydrogen content to reach more than 20%, these inflammable gases at high temperature use danger higher as reducing atmosphere, need strictly to control, otherwise easily cause an explosion accident, be unfavorable for production safety.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the invention provides a kind of preparation method of LED fluorescent powder, this preparation method is not only Well-recovered, and reduces the content of hydrogen in the gas as reducing atmosphere, and safe preparation process is increased.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of LED fluorescent powder, is characterized in that, the method comprises the following steps:
1. according to the mol ratio of each component of the fluorescent material of required preparation, corresponding starting material are taken respectively;
2. add carbonaceous solids material, the carbon atom mole number of described carbonaceous solids material is 1-10 times of the dopant ion mole number of the fluorescent material of required preparation; Add the catalyzer that described carbonaceous solids material can be made to gasify, the add-on of described catalyzer is the 0.5%-5% of described raw material quality; Add fusing assistant, the add-on of described fusing assistant is the 0.5%-5% of described raw material quality;
3. by above-mentioned starting material, carbonaceous solids material, catalyzer and fusing assistant Homogeneous phase mixing, load in high-temperature crucible, and be placed in high-temperature atmosphere furnace, passing into hydrogen volume content is that the reducing gas of 0-5% is as reducing atmosphere, then be heated to the synthesis temperature of fluorescent material and keep pressure-fired power 1-100kpa, insulation 2-6 hour, is cooled to room temperature after terminating under reducing atmosphere, takes out and fires thing;
4. will fire thing and remove macrobead after pulverizing, sieving, then size mixing with water or organic solvent in ball mill container and carry out Ball milling and obtain slurry, then paste fluor is obtained through superheated water or hot organic solvent washing, filtration and further washing, paste fluor is dry in an oven, through porphyrize or sieve and obtain LED fluorescent powder after cooling.
Described step 3. in reducing gas be rare gas element or the mixed gas for hydrogen and rare gas element; Described rare gas element is nitrogen, argon gas or their mixed gas.
The fluorescent material of described required preparation is Ce
3+the rare earth aluminate fluorescent material of ion doping, Eu
2+the alkaline-earth silicate fluorescent powder of ion doping, Eu
2+the alkaline earth aluminium silicon nitride complex chemical compound fluorescent material of ion doping, Eu
2+the fluorescent material that the alkaline earth silicon oxynitride aluminium complex chemical compound fluorescent material of ion doping or other needs are prepared under reducing gas.
When the fluorescent material of described required preparation is rare earth aluminate fluorescent material, its starting material used are: rare earth oxide and aluminum oxide; When the fluorescent material of described required preparation is alkaline-earth silicate fluorescent powder, its starting material used are: alkaline earth carbonate and silicon-dioxide; When the fluorescent material of described required preparation is alkaline earth aluminium silicon nitride complex chemical compound, its starting material used are: alkaline earth nitride, silicon nitride and aluminium nitride; When the fluorescent material of described required preparation is alkaline earth silicon oxynitride aluminium complex chemical compound, its starting material used are: alkaline earth nitride, alkaline-earth oxide, silicon nitride, silicon oxide, aluminium nitride and aluminum oxide.
Described step 2. in carbonaceous solids material be carbon simple substance, carbon compound or their mixture.
Described carbon simple substance is carbon black, Graphite Powder 99 or their mixture.
Described carbon compound is glucose, sucrose, Mierocrystalline cellulose or their mixture.
Described step 2. in catalyzer be salt of wormwood, sodium carbonate, Quilonum Retard, potassium sulfate, sodium sulfate or their mixture.
Described step 2. in fusing assistant be carbonate, borate, halogenide or their mixture.
Described step 4. in the Ball milling time be 2-4 hour; Described hot water or hot organic solvent washing process are specially the water or organic solvent that add 5-10 times of volume in the slurry, and are placed in the container that 50-90 DEG C of hot water or hot organic solvent are housed and stir 5-10 hour; Temperature dry in described baking oven is 120-180 DEG C.
Wherein, the catalyzer of carbonaceous solids material refers to can be strengthened carbonaceous solids material and gasify and the material producing reducing gas, mainly contains salt of wormwood, sodium carbonate, Quilonum Retard, potassium sulfate, sodium sulfate etc., or the mixture between them.Catalyzer can be strengthened carbonaceous solids on the one hand and at high temperature decompose, and produces H
2, CO, CO
2deng gas, on the other hand, catalyzer itself can decompose generation CO
2or SO
3, can react further and generate reducing gas CO with adding or decompose the simple substance C obtained.Such carbonaceous solids material, under the effect of catalyzer, at high temperature not only can produce reducing gas H
2, CO etc., make the dopant ion Ce in fluorescent material
4+, Eu
3+ion reduction becomes Ce
3+, Eu
2+ion, and add or decompose the simple substance C obtained and also can become CO gas and can not be retained in fluorescent material product and affect its lighting function.
Fusing assistant can reduce the temperature of reaction that phosphor raw material forms fluorescent material composition, promotes fluorescent material composition crystal growth, can control the crystallization direction of fluorescent material composition and surface property etc. simultaneously.Fusing assistant is generally low melting point mineral compound, as carbonate, borate, halogenide etc., can be the mixture of a kind of compound or several compound.Different phosphor raw materials and fluorescent material composition, the fusing assistant of employing is different.
The fluorescent material of required preparation can be Ce
3+the rare earth aluminate fluorescent material of ion doping, Eu
2+the alkaline-earth silicate fluorescent powder of ion doping, Eu
2+the alkaline earth aluminium silicon nitride complex chemical compound fluorescent material of ion doping, Eu
2+the alkaline earth silicon oxynitride aluminium complex chemical compound fluorescent material etc. of ion doping.Some main concrete rare earth aluminate fluorescent material have: bloom Y
3al
5o
12: Ce, yellowish green powder Lu
3al
5o
12: Ce, bloom Tb
3al
5o
12: Ce, yellowish green powder (Y, Lu)
3al
5o
12: Ce, yellow orange powder (Y, Gd)
3al
5o
12: Ce, yellowish green powder (Y, Lu, Gd)
3al
5o
12: Ce etc., they are in blue-light excited lower effective luminescence; Some main concrete alkaline-earth silicate fluorescent powders have: green powder Ba
2siO
4: Eu, bloom Sr
2siO
4: Eu, yellowish green powder (Ba, Sr)
2siO
4: Eu, orange powder Sr
3siO
5: Eu etc., they are in purple or blue-light excited lower effective luminescence; Some main concrete alkaline earth aluminium silicon nitride complex chemical compound fluorescent material have: rouge and powder CaAlSiN
3: Eu, rouge and powder (Ca, Sr) AlSiN
3: Eu, rouge and powder Sr
2si
5n
8: Eu, rouge and powder (Sr, Ca, Ba)
2si
5n
8: Eu etc., they are in purple or blue-light excited lower effective luminescence; Some main concrete alkaline earth silicon oxynitride aluminium complex chemical compound fluorescent material have: green powder β-SiAlON:Eu, green powder BaSi
2o
2n
2: Eu, bloom M-α-SiAlON:Eu, blue powder α-SiAlON:Eu etc., they are in purple or blue-light excited lower effective luminescence.
Compared with prior art, the advantage of the preparation method of a kind of LED fluorescent powder of the present invention is: on the one hand, reduces the content of hydrogen in the gas as reducing atmosphere, and safe preparation process is increased, the usage quantity of hydrogen can be reduced simultaneously, cost-saving; On the other hand, by preparing in phosphor raw material the catalyzer adding carbonaceous solids material and impel this carbonaceous solids material to gasify, carbonaceous solids material is made to produce H under catalyzer and high temperature action
2, the reducing gas such as CO, reductibility is high, and the simple substance C adding or decompose also becomes the gases such as CO and can not be retained in fluorescent material product and affects its luminescent properties.
Accompanying drawing explanation
Fig. 1 is the (Lu of the embodiment of the present invention 1
1.5y
1.47ce
0.03) (Al
4ga) O
12the emmission spectrum of fluorescent material under blue light (460nm) excites;
Fig. 2 is the (Lu of the embodiment of the present invention 1
1.5y
1.47ce
0.03) (Al
4ga) O
12the electron microscope scanning figure of fluorescent material.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but not as a limitation of the invention.
Embodiment 1:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
According to chemical formula (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12in the mol ratio of each component, take the starting material prepared needed for fluorescent material respectively: yttrium oxide Y
2o
3244.8g, lutecium oxide Lu
2o
3512.2g, cerium oxide CeO
28.9g, aluminium oxide Al
2o
3350g, gallium oxide Ga
2o
3160.8g.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is carbon black 3.1g, in carbonaceous solids material carbon atom mole number for needed for prepare 5 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
313g, catalyst quality is 1% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o11.5g and Na
3alF
6the mixture of 3.3g, fusing assistant quality is 1.16% of corresponding raw material quality.
Above-mentioned materials is mixed in Double cone mixer, 200# sieves and removes the uneven part of mixing and impurity, load in the corundum crucible of 500-1000ml, add a cover and be placed in high-temperature atmosphere furnace, through the nitrogen of the hydrogen and volume content 95% exhaust and be filled with volume content 5% as reducing atmosphere, be heated to the synthesis temperature 1600 DEG C of fluorescent material and keep pressure-fired 5kpa, and being incubated 2-6 hour, being cooled to room temperature after terminating under reducing atmosphere and taking out.Firing thing is that bright orange green is loose block, after jaw crusher is pulverized, then 200# sieves removing macrobead, then the ball mill container tank placing ball milling pearl is placed in, size mixing with water, wherein stock quality is than being fluorescent material: ball milling pearl: water=1:1:2, and carries out Ball milling 2-4 hour, sieve through 400#, obtain slurry.Add 5-10 water doubly in the slurry and stir 5-10 hour in the hot water of 80-90 DEG C, then paste fluor is obtained through filtering and washing further, paste fluor to be placed in the baking oven of 120-180 DEG C dry, through porphyrize or sieve and obtain fluorescent material finished product after cooling.
Fig. 1 is rare earth aluminate (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12the emmission spectrum of fluorescent material under blue light (460nm) excites, sends yellowish green light under the exciting of blue-ray LED (emission peak wavelength 460nm), and peak wavelength is 535nm, peak width at half height 110nm.As can be seen from this phosphor emission spectrum, the LED fluorescent powder obtained by the inventive method is identical with existing fluorescent material performance, and as seen when low hydrogen content gas makes reducing atmosphere, reducing property is still better.
Fig. 2 is rare earth aluminate (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12the electron micrograph of fluorescent material.As can be seen from the figure, fluorescent material is made up of various molecule, even particle size, and particle shape is polyhedron spherical solid, and well-crystallized, diameter is at about 10um.Compared with existing fluorescent material, grain crystalline state consistency, but distribution is more even, and similar spherical, without grain breakage phenomenon, the LED fluorescent powder that therefore the inventive method is obtained has better properties.
Embodiment 2:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
According to chemical formula (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12in the mol ratio of each component, take the starting material prepared needed for fluorescent material respectively: yttrium oxide Y
2o
3244.8g, lutecium oxide Lu
2o
3512.2g, cerium oxide CeO
28.9g, aluminium oxide Al
2o
3350g, gallium oxide Ga
2o
3160.8g.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is glucose 7.8g, in carbonaceous solids material carbon atom mole number for needed for prepare 5 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
313g, catalyst quality is 1% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o11.5g and Na
3alF
6the mixture of 3.3g, fusing assistant quality is 1.16% of corresponding raw material quality.
Method said mixture being prepared into fluorescent material finished product is identical with embodiment 1, and difference is only that the carbonaceous solids material added is different.
Embodiment 3:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
According to chemical formula (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12in the mol ratio of each component, take the starting material prepared needed for fluorescent material respectively: yttrium oxide Y
2o
3244.8g, lutecium oxide Lu
2o
3512.2g, cerium oxide CeO
28.9g, aluminium oxide Al
2o
3350g, gallium oxide Ga
2o
3160.8g.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is glucose 7.8g, in carbonaceous solids material carbon atom mole number for needed for prepare 5 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
313g, catalyst quality is 1% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o11.5g and Na
3alF
6the mixture of 3.3g, fusing assistant quality is 1.16% of corresponding raw material quality.
Method said mixture being prepared into fluorescent material finished product is identical with embodiment 1, and difference is only that the carbonaceous solids material added is different.
Embodiment 4:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
Take the starting material prepared needed for fluorescent material same as the previously described embodiments.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is carbon black 0.62g, in carbonaceous solids material carbon atom mole number for needed for prepare 1 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
36.5g, catalyst quality is 0.5% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o5g and Na
3alF
6the mixture of 1.4g, fusing assistant quality is 0.5% of corresponding raw material quality.
Method said mixture being prepared into fluorescent material finished product is identical with embodiment 1.
Embodiment 5:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
Take the starting material prepared needed for fluorescent material same as the previously described embodiments.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is glucose 4.68g, in carbonaceous solids material carbon atom mole number for needed for prepare 3 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is salt of wormwood K
2cO
313g, catalyst quality is 1% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o10g and Na
3alF
6the mixture of 2.8g, fusing assistant quality is 1% of corresponding raw material quality.
Method said mixture being prepared into fluorescent material finished product is identical with embodiment 1.
Embodiment 6:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
Take the starting material prepared needed for fluorescent material same as the previously described embodiments.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is carbon black 4.96g, in carbonaceous solids material carbon atom mole number for needed for prepare 8 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
339g, catalyst quality is 3% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o30g and Na
3alF
6the mixture of 8.4g, fusing assistant quality is 3% of corresponding raw material quality.
Embodiment 7:
A kind of rare earth aluminate fluorescent material of the present invention (Lu
1.5y
1.47ce
0.03) (Al
4ga) O
12can obtain by the following method:
Take the starting material prepared needed for fluorescent material same as the previously described embodiments.
Add carbonaceous solids material, in the present embodiment, carbonaceous solids material is carbon black 6.2g, in carbonaceous solids material carbon atom mole number for needed for prepare 10 times of the doping active ions mole number of fluorescent material.
Add the catalyzer that carbonaceous solids material can be made to gasify, in the present embodiment, catalyzer is sodium carbonate Na
2cO
365g, catalyst quality is 5% of corresponding raw material quality.
Add fusing assistant, in the present embodiment, fusing assistant is AlF
33H
2o50g and Na
3alF
6the mixture of 14g, fusing assistant quality is 5% of corresponding raw material quality.
Method said mixture being prepared into fluorescent material finished product is identical with embodiment 1.
Solid carbonaceous substance in the present invention and catalyzer are applicable to the preparation of all fluorescent material, such as: the fluorescent material that rare earth aluminate fluorescent material, alkaline-earth silicate fluorescent powder, alkaline earth aluminium silicon nitride complex chemical compound fluorescent material, alkaline earth silicon oxynitride aluminium complex chemical compound fluorescent material or other needs are prepared under reducing gas.The fluorescent material of other preparation condition and required preparation adapts.
The LED fluorescent powder hydrogen usage quantity that the inventive method prepares is low, be conducive to safety in production, and the fluorescent material performance obtained is similar to existing fluorescent material or be better than existing fluorescent material.
It should be noted that; the foregoing is only preferred embodiment of the present invention; not thereby limit scope of patent protection of the present invention, those of ordinary skill in the art, to the conversion of any equivalence that technical solution of the present invention is taked, are claim of the present invention and contain.
Claims (10)
1. a preparation method for LED fluorescent powder, is characterized in that, the method comprises the following steps:
1. according to the mol ratio of each component of the fluorescent material of required preparation, corresponding starting material are taken respectively;
2. add carbonaceous solids material, the carbon atom mole number of described carbonaceous solids material is 1-10 times of the dopant ion mole number of the fluorescent material of required preparation; Add the catalyzer that described carbonaceous solids material can be made to gasify, the add-on of described catalyzer is the 0.5%-5% of described raw material quality; Add fusing assistant, the add-on of described fusing assistant is the 0.5%-5% of described raw material quality;
3. by above-mentioned starting material, carbonaceous solids material, catalyzer and fusing assistant Homogeneous phase mixing, load in high-temperature crucible, and be placed in high-temperature atmosphere furnace, passing into hydrogen volume content is that the reducing gas of 0-5% is as reducing atmosphere, then be heated to the synthesis temperature of fluorescent material and keep pressure-fired power 1-100kpa, insulation 2-6 hour, is cooled to room temperature after terminating under reducing atmosphere, takes out and fires thing;
4. will fire thing and remove macrobead after pulverizing, sieving, then size mixing with water or organic solvent in ball mill container and carry out Ball milling and obtain slurry, then paste fluor is obtained through superheated water or hot organic solvent washing, filtration and further washing, paste fluor is dry in an oven, through porphyrize or sieve and obtain LED fluorescent powder after cooling.
2. the preparation method of LED fluorescent powder as claimed in claim 1, is characterized in that, described step 3. in reducing gas be rare gas element or the mixed gas for hydrogen and rare gas element; Described rare gas element is nitrogen, argon gas or their mixed gas.
3. the preparation method of LED fluorescent powder as claimed in claim 1, is characterized in that, the fluorescent material of described required preparation is Ce
3+the rare earth aluminate fluorescent material of ion doping, Eu
2+the alkaline-earth silicate fluorescent powder of ion doping, Eu
2+the alkaline earth aluminium silicon nitride complex chemical compound fluorescent material of ion doping, Eu
2+the fluorescent material that the alkaline earth silicon oxynitride aluminium complex chemical compound fluorescent material of ion doping or other needs are prepared under reducing gas.
4. the preparation method of LED fluorescent powder as claimed in claim 3, is characterized in that, when the fluorescent material of described required preparation is rare earth aluminate fluorescent material, its starting material used are: rare earth oxide and aluminum oxide; When the fluorescent material of described required preparation is alkaline-earth silicate fluorescent powder, its starting material used are: alkaline earth carbonate and silicon-dioxide; When the fluorescent material of described required preparation is alkaline earth aluminium silicon nitride complex chemical compound, its starting material used are: alkaline earth nitride, silicon nitride and aluminium nitride; When the fluorescent material of described required preparation is alkaline earth silicon oxynitride aluminium complex chemical compound, its starting material used are: alkaline earth nitride, alkaline-earth oxide, silicon nitride, silicon oxide, aluminium nitride and aluminum oxide.
5. the preparation method of the LED fluorescent powder as described in any one of claim 1-4, is characterized in that, described step 2. in carbonaceous solids material be carbon simple substance, carbon compound or their mixture.
6. the preparation method of LED fluorescent powder as claimed in claim 5, it is characterized in that, described carbon simple substance is carbon black, Graphite Powder 99 or their mixture.
7. the preparation method of LED fluorescent powder as claimed in claim 5, it is characterized in that, described carbon compound is glucose, sucrose, Mierocrystalline cellulose or their mixture.
8. the preparation method of the LED fluorescent powder as described in any one of claim 1-4, is characterized in that, described step 2. in catalyzer be salt of wormwood, sodium carbonate, Quilonum Retard, potassium sulfate, sodium sulfate or their mixture.
9. the preparation method of the LED fluorescent powder as described in any one of claim 1-4, is characterized in that, described step 2. in fusing assistant be carbonate, borate, halogenide or their mixture.
10. the preparation method of LED fluorescent powder as claimed in claim 1, is characterized in that, described step 4. in the Ball milling time be 2-4 hour; Described hot water or hot organic solvent washing process are specially the water or organic solvent that add 5-10 times of volume in the slurry, and are placed in the container that 50-90 DEG C of hot water or hot organic solvent are housed and stir 5-10 hour; Temperature dry in described baking oven is 120-180 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108130074A (en) * | 2018-01-15 | 2018-06-08 | 东南大学 | A kind of method for preparing high crystalline nano silicon nitride matter fluorescent powder |
| CN109054816A (en) * | 2018-07-24 | 2018-12-21 | 北京科技大学 | A kind of preparation method of the aluminium nitride fluorescent powder of europium ion activation |
| CN109504383A (en) * | 2019-01-16 | 2019-03-22 | 南昌工程学院 | A kind of preparation method of LED fluorescent powder |
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| CN109504383A (en) * | 2019-01-16 | 2019-03-22 | 南昌工程学院 | A kind of preparation method of LED fluorescent powder |
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