CN103965906A - Yttrium aluminum garnet fluorescent powder material and preparation method thereof - Google Patents
Yttrium aluminum garnet fluorescent powder material and preparation method thereof Download PDFInfo
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- CN103965906A CN103965906A CN201310041701.5A CN201310041701A CN103965906A CN 103965906 A CN103965906 A CN 103965906A CN 201310041701 A CN201310041701 A CN 201310041701A CN 103965906 A CN103965906 A CN 103965906A
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Abstract
The invention relates to a yellow or orange fluorescent powder for LED (light emitting diode) use. The stoichiometric formula of the fluorescent powder is Ln2M' M''2-alphaAl2alphaSi3-alpha O12-2underlined beta M' '' underlined beta N underlined beta, wherein Ln is at least one of Y, Lu and Gd, M' is at least one of Ca, Sr and Ba, M'' is at least one of Mg and Zn, M' '' is F and Cl, alpha is greater than or equal to 0 and smaller than or equal to 2, and underlined beta is greater than or equal to 0.2 and smaller than or equal to 0.5. The fluorescent material prepared by the invention has the crystal structure of yttrium aluminum garnet, and is excited by blue light with a wavelength of 450-470nm to emit orange red light with a wavelength of 570nm-610nm. The invention also discloses a preparation method of the fluorescent powder. The fluorescent powder synthesized by the invention can emit 570-610nm yellow orange light under excitation of 450-470nm light rays. Also, by fine-tuning the formula composition, the luminous efficiency and mobile wavelength of the fluorescent powder can be improved.
Description
Technical field
The present invention relates to a kind of fluorescent material with yttrium aluminum garnet structure, this fluorescent material can be excited by the blue light part of spectral region and send blood orange light.The present invention also relates to the preparation method of this fluorescent material, belong to rare earth class mineral compound luminescent material preparation method's technical field.
Background technology
Solid state lighting refers to and adopts the lighting engineering of all solid state luminescent device as light source.Mainly semiconductor lighting, the i.e. photodiode of transmitting white at present---white light LEDs (Light Emitting Diode) lamp.Contrast incandescent light and luminescent lamp, this LED light fixture has significant advantage: volume is little, the life-span is long, power saving, do not contain the mercury of contaminate environment, high-level efficiency, low maintenance etc.
Since there is LED, people are laying siege to always and are realizing solid light source, along with the continuous progress of LED manufacturing process and exploitation and the application of type material (element nitride crystal and fluorescent material), make the LED semiconductor solid-state optical source performance emitting white light constantly improve and enter the practical stage.Commercial product is mainly that two wavelength blue light single-chips add yellow fluorescent powder at present, although what be expected in future is three-wavelength light, add R.G.B tri-color fluorescent material with inorganic UV-light wafer, but UV-light chip, also in the laboratory study stage, scale operation to need Hen Chang road to walk.Now only limit to cerium ion-doped (Y, the Gd) with yttrium aluminum garnet structure for the yellow fluorescent powder of white light LEDs
3(Al, Ga)
5o
12material.YAG:Ce
3+to have luminous efficiency high due to it for fluorescent material, stable performance, the advantages such as good thermal conductivity and good physicochemical property.Day, the patent US5998925 of sub-chemistry reported inorganic fluorescent powder (Y1-x-yGdxCey)
3al
5o
12, recently control the position of launching crest by the Y/Gd ratio and the Al/Ga that adjust wherein.The Ou Silang of the U.S., in order to avoid a day sub-patent, has applied for patent US6669866, has prepared equally the fluorescent material Tb of yttrium aluminum garnet structure with Tb replacement Y
3al
5o
12.But, the LED that this blue-light excited yellow fluorescent powder produces white light is because it lacks stronger transmitting in ruddiness region, exist colour rendering index on the low side, can not show well the original color of article, the shortcomings such as colour temperature higher (>4500K), have limited its application in White-light LED illumination field greatly.
Summary of the invention
In order to overcome the deficiencies in the prior art part, technical solution of the present invention is to provide a kind of novel fluorescence powder material, and what this phosphor material powder can be 450-470nm by wavelength is blue-light excited, and launching emission peak wavelength is the orange red light of 570-610nm.
The present invention also provides the preparation method of above-mentioned phosphor material powder, and the method can be conducive to obtain high brightness, epigranular, the particle diameter superfine fluorescent powder at 10-20 micron.
Technical scheme of the present invention is as follows:
A kind of Yttrium aluminium garnet (YAG) type fluorescent powder, is characterized in that: chemometric equation is Ln
2m ' M "
2-αal
2 αsi
3-αo
12-2
β m ' "
β n
β , wherein, Ln is at least one in Y, Lu, Gd, M ' is at least one in Ca, Sr, Ba, M " be one or both in Mg, Zn, M ' " be in F, Cl one or both,
0 ≦ α≤2 0.2≤
β≤ 0.5.Described fluorescent material, under 455-470nm is blue-light excited, is launched the light that emission peak wavelength is 570-610nm.
Described fluorescent material can be for making pink LED.
The preparation method of phosphor material powder, the chemometric equation of described fluorescent material is Ln
2m ' M "
2-αal
2 αsi
3-αo
12-2
β m ' "
β n
β , wherein, Ln is at least one in Y, Lu, Gd, M ' is at least one in Ca, Sr, Ba, M, and " being at least one in Mg, Zn, Mn, M ' " is F, Cl, Br,
0 ≦ α≤2 0.2≤
β≤ 0.5; Its preparation process comprises: (1) takes with the raw material of the corresponding weight of fluorescent material as phosphor precursor to be restored by stoichiometric ratio, and grinding mixture makes it even; (2) in presoma, add fusing assistant, it is mixed; (3) powdered mixture is dissolved in to ethanol, is placed on ball mill device and carries out ball milling, make it form rheology phase; (4) before ball milling, add grain diameter conditioning agent.(5) rheology phase solution heated at the temperature of 100 DEG C to 120 DEG C and stir, obtaining grey shape thing.(6) by grey shape thing pre-burning 2-5 hour at 800 DEG C to 1200 DEG C temperature, cooling after, grind, grind, cross 200 mesh sieves.(7) at 1300 DEG C to the product of roasting after pre-burning in reducing atmosphere at 1550 degree temperature.(8) by the chamotte crushing of naturally cooling gained, grind, to sieve, washing, dries, and obtains even particle size distribution after 400 mesh sieves, and size is the product of 5-20nm.
Described grain diameter conditioning agent is one in polyoxyethylene glycol, polycarbonate, alkyl sulfhydryl, two kinds or all, the 0.5-2wt% that its consumption is presoma.
Beneficial effect of the present invention:
(1) the synthetic fluorescent material of the present invention can send the yellow orange light of 570-610nm under 450-470nm light excites, and (2) and can consist of fine-tuning recipes improve luminous efficiency and the mobile wavelength of fluorescent material.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrum with yttrium aluminum garnet structure fluorescent material with embodiment 1.
Fig. 2 is the emmission spectrum of embodiment 1.
Fig. 3 is the excitation spectrum of embodiment 1.
Embodiment
Following embodiment further illustrates the present invention, can make that those skilled in the art are clearer knows technology contents of the present invention, so following embodiment should not be regarded as limitation of the scope of the invention.
(embodiment 1)
Fluorescent material Lu
1.5y
0.45caMg
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, CaCO3, MgCO3, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add cetomacrogol 1000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 1000 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1300 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
(embodiment 2)
Fluorescent material Lu
1.5y
0.45caZn
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, CaCO3, ZnO, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add Macrogol 2000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 1000 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1500 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
(embodiment 3)
Fluorescent material Lu
1.5y
0.45srMg
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, SrCO3, MgCO3, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add cetomacrogol 1000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 900 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1500 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
(embodiment 4)
Fluorescent material LuY
0.95caMg
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, CaCO3, MgCO3, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add cetomacrogol 1000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 1000 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1300 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
(embodiment 5)
Fluorescent material LuY
0.95caZn
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, CaCO3, ZnO, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add Macrogol 2000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 1000 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1500 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
(embodiment 6)
Fluorescent material LuY
0.95srMg
2si
3o
11.5f:0.05Ce prepares example
Raw material chosen in chemical structural formula according to above-mentioned fluorescent material, and raw material is Lu2O3, Y2O3, SrCO3, MgCO3, CeO2, SiO2, NaF, by former abrasive lapping and mix, in powder after grinding, add composite fluxing agent BaF2 and boric acid, its content is the 5w% of raw material total amount, mixed again, become the presoma of fluorescent material; Presoma is joined in the ethanol of 99.7w%, be placed in ball mill device and carry out ball milling, after ball milling 2 hours, add cetomacrogol 1000, add-on is the 1w% of raw material total amount, then ball milling 2 hours; Material good ball milling heated at the temperature of 100 DEG C and stir, obtaining grey shape thing; By the pre-burning 3 hours at 900 DEG C of temperature of grey shape thing, cross 200 mesh sieves, obtain powder 1; By powder 1 roasting in reducing atmosphere at 1500 DEG C of degree temperature, obtain powder 2; The powder of naturally cooling gained 2, through fragmentation, is ground, sieve, washing, dries, and after the processing such as sieve, obtains even particle size distribution, and size is the powder 3 of 5-20nm.
Claims (8)
1. a Yttrium aluminium garnet (YAG) type fluorescent powder, is characterized in that: chemometric equation is Ln
2m ' M "
2-αal
2 αsi
3-αo
12-2
β m ' "
β n
β , wherein, Ln is at least one in Y, Lu, Gd, M ' is at least one in Ca, Sr, Ba, M, and " being at least one in Mg, Zn, M ' " is F, Cl,
0 ≦ α≤2 0.2≤
β≤ 0.5.
2. yttrium aluminium garnet fluorescent powder according to claim 1, is characterized in that: fluorescent material is subject to wavelength while being 450nm to 470nm scope blue-light excited, and can send wavelength is the orange red light of 570nm to 610nm.
3. yttrium aluminium garnet fluorescent powder according to claim 1, is characterized in that: described fluorescent material is used for making pink LED.
4. a preparation method for Yttrium aluminium garnet (YAG) type fluorescent powder as claimed in claim 1, is characterized in that: the method comprises the steps:
(1) by stoichiometric ratio take with the raw material of the corresponding weight of fluorescent material as fluorescent material to be restored before
bodybody, grinding mixture makes it even;
(2) in presoma, add fusing assistant, mix and obtain powdered mixture;
(3) powdered mixture is dissolved in to ethanol, is placed on and on ball mill device, carries out ball milling, add grain diameter conditioning agent at ball milling in intermittently, obtain rheology phase solution;
(4) rheology phase solution heated at the temperature of 100 DEG C to 120 DEG C and stir, obtaining grey shape thing;
(5) by grey shape thing pre-burning 2-5 hour at 800 DEG C to 1200 DEG C temperature, cross 200 mesh sieves, obtain the product of pre-burning;
(6) at 1300 DEG C to the product of roasting after pre-burning in reducing atmosphere at 1550 degree temperature;
(7) by the grog of the product naturally cooling gained of step (6) through fragmentation, grind, sieve, washing, dry, after sieving and obtain even particle size distribution, size is the product of 5-20nm.
5. the preparation method of Yttrium aluminium garnet (YAG) type fluorescent powder according to claim 4, is characterized in that: described raw material is oxycompound system, carbonate system, phosphate system, borate salt system, aluminates system, one or more in oxyhydroxide system.
6. the preparation method of Yttrium aluminium garnet (YAG) type fluorescent powder according to claim 4, is characterized in that: described grain diameter conditioning agent is one or more in polyoxyethylene glycol, polycarbonate, alkyl sulfhydryl.
7. the preparation method of Yttrium aluminium garnet (YAG) type fluorescent powder according to claim 4, is characterized in that: described fusing assistant is BaF
2, H
3in BO3 one or both, its consumption is the 2-10wt% of presoma powder.
8. the preparation method of Yttrium aluminium garnet (YAG) type fluorescent powder according to claim 4, is characterized in that: described reducing atmosphere is the one in ammonia, coal gas, methane, carbon monoxide, nitrogen and hydrogen mixture.
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| CN109874803A (en) * | 2019-04-15 | 2019-06-14 | 兰州大学 | It is a kind of to promote fluorescent powder of plant growth and preparation method thereof |
| CN110589889A (en) * | 2019-10-12 | 2019-12-20 | 景德镇陶瓷大学 | Inorganic composite orange pigment and preparation method thereof |
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| CN109874803A (en) * | 2019-04-15 | 2019-06-14 | 兰州大学 | It is a kind of to promote fluorescent powder of plant growth and preparation method thereof |
| CN110589889A (en) * | 2019-10-12 | 2019-12-20 | 景德镇陶瓷大学 | Inorganic composite orange pigment and preparation method thereof |
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Application publication date: 20140806 |