CN102517016A - Solid solution fluorescent light-emitting material for blue light excitation and preparation method thereof - Google Patents
Solid solution fluorescent light-emitting material for blue light excitation and preparation method thereof Download PDFInfo
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- CN102517016A CN102517016A CN2011103636316A CN201110363631A CN102517016A CN 102517016 A CN102517016 A CN 102517016A CN 2011103636316 A CN2011103636316 A CN 2011103636316A CN 201110363631 A CN201110363631 A CN 201110363631A CN 102517016 A CN102517016 A CN 102517016A
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Abstract
The invention provides a solid solution fluorescent light-emitting material for blue light excitation, which has the atomic ratio as shown in formula (I). The invention further provides a preparation method of the solid solution fluorescent light-emitting material for the blue light excitation, and the preparation method comprises the following steps of: mixing an RE-containing compound, a Ce-containing compound, an M-containing compound, an Mn-containing compound, an A-containing compound and a D-containing compound to get a mixture; and baking the mixture under a reducing atmosphere to get the solid solution fluorescent light-emitting material for the blue light excitation. The solid solution fluorescent light-emitting material provided by the invention is stable in performances, so that a white LED (light-emitting diode) is also stabler in the performances; and the solid solution fluorescent light-emitting material provided by the invention can obviously expand an emission spectrum to a red light district under the excitation of blue light and improve the color rendering property of the solid solution fluorescent light-emitting material, and the emission spectrum of the solid solution fluorescent light-emitting material is adjustable and can further meet the demands under different occasions. In addition, the preparation method of the solid solution fluorescent light-emitting material, provided by the invention is simple, feasible and easy to operate.
Description
Technical field
The invention belongs to the luminescent material technical field, relate in particular to a kind of blue-light excited sosoloid fluorescence luminescent material and preparation method thereof that is used for.
Background technology
White light emitting diode (LED) is a kind of semiconducter device that can electric energy be transformed visible light, has plurality of advantages such as volume is little, energy-conservation, the life-span is long, pollution-free, has wide application value and huge market outlook.At present; White light LEDs is applied at numerous areas such as backlight of LCD, PL, general lighting lamps; And will replace the various bulb that uses at present and become a new generation's illumination green illumination light source with luminescent lamp, have extensive and profound significance to energy-saving and environmental protection, the aspects such as quality of life that improve the people.
Prior art discloses the concocting method of multiple white light LEDs, mainly comprises following three kinds:
(1) polycrystalline sheet mixed light technology: be fixed in same package interior to red, blue and green three wafers or blue light and gold-tinted twin lamella respectively; Again via the size of current of adjusting each wafer; Adjust the amount of light of each wafer and control the mixed light ratio, to reach the target that blendes together white light;
(2) excite mixed uniformly blueness, green and red fluorescent powder with ultraviolet leds, carry out mixed light output white thereby make it inspire a certain proportion of three primary colors;
(3) be mixed with gold-tinted YAG (Yttrium Aluminum Garnet) phosphor powder filling of blue-ray LED on every side; And the use wavelength is the blue-ray LED of 400～530nm; Emit beam and excite gold-tinted YAG phosphor powder to produce sodium yellow; Simultaneously also with blue light originally, and then form blue yellow blended two wavelength white lights.
Wherein, (3) kind mode has method advantage simple, with low cost, is method comparatively commonly used.At present, prior art is generally with doped with cerium ionic yttrium aluminum garnet (YAG:Ce
3+) fluorescent material combines with blue-ray LED to realize white light through the complementary color principle.But red composition is not enough in this fluorescent material, and color developing is relatively poor.
Red component content is to improve the color developing and the tunability of white light in the fluorescent material in order to increase, and prior art discloses the method that adopts blue led and green emitting phosphor and red fluorescence powder combination to produce white light.But green emitting phosphor and red fluorescence powder are mainly oxide-base fluorescent material, sulfide base fluorescent powder and nitride based fluorescent material etc. at present, and wherein, oxide-base fluorescent material is difficult to mate with blue led a little less than visible region ground absorbs; The thermostability and the chemicalstability of sulfide base fluorescent powder are relatively poor, and long-time use can cause luminous decay; Though nitride based fluorescent material excellent in optical properties, preparation condition is harsh, cost is higher.In addition, there are nature difference in red fluorescence powder and green emitting phosphor, and problems such as unstable properties can appear in the white light LEDs that obtains in practical application.Therefore, to obtain the adjustable single substrate luminescent material of emmission spectrum be the important topic that LED faces with luminescent material in research and development.
Summary of the invention
In view of this, the technical problem that the present invention will solve is to be provided for blue-light excited sosoloid fluorescence luminescent material and preparation method thereof, and sosoloid fluorescence luminescent material provided by the invention stable performance, color developing and tunable performance are better.
The invention provides a kind of blue-light excited sosoloid fluorescence luminescent material that is used for, have atomic ratio shown in the formula (I):
(1-x)[RE
3-yCe
yM
5O
12]·x[A
3-zMn
zM
2(DO
4)
3](I)；
In the formula (I), RE is one or more among Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu;
M is one or more among B, Al, Ga and the In;
A is one or more of Mg, Ca, Sr and Ba;
D is one or more of Si, Ge and Sn;
0＜x≤0.50；
0＜y≤0.30；
0＜z≤3。
Preferably, said M is one or both among B and the Al.
The present invention also provides a kind of technique scheme the described preparation method who is used for blue-light excited sosoloid fluorescence luminescent material, may further comprise the steps:
To contain the RE compound, contain the Ce compound, contain the M compound, contain the Mn compound, contain the A compound and contain the D compound, obtain mixture;
With the roasting under reducing atmosphere of said mixture, obtain being used for blue-light excited sosoloid fluorescence luminescent material.
Preferably, the said RE of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains RE.
Preferably, the said Ce of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Ce.
Preferably, the said M of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains M.
Preferably; The said A of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains A, and the said Mn of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Mn.
Preferably, the said D of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains D.
Preferably, said mixture also comprises fluoride flux.
Preferably, the temperature of said roasting is 1400 ℃～1700 ℃, and the time of said roasting is 1h～20h.
Compared with prior art, provided by the inventionly be used for blue-light excited sosoloid fluorescence luminescent material and have atomic ratio shown in the formula (I) and form, be the sosoloid of garnet-base, and be doped with Ce and Mn.Sosoloid fluorescence luminescent material provided by the invention stable performance makes that the performance of white light LEDs is also comparatively stable; Excitation spectrum a wider range of sosoloid fluorescence luminescent material provided by the invention, and strong absorption is arranged at the 450nm place, can with commercial blue chip perfect adaptation, obtain well behaved white light LEDs; Sosoloid fluorescence luminescent material provided by the invention is blue-light excited following, and emmission spectrum is obviously expanded to red light district, improved the color developing of sosoloid fluorescence luminescent material, and its emmission spectrum is adjustable, satisfies the demand of different occasions.In addition, preparing method's simple possible, the easy handling of sosoloid fluorescence luminescent material provided by the invention, be easy to volume production, pollution-free, cost is low.
Description of drawings
The XRD figure spectrum of the fluorescent material that Fig. 1 prepares for the embodiment of the invention 8;
The photic emmission spectrum of the fluorescent material that Fig. 2 prepares for the embodiment of the invention 8 under 450nm is blue-light excited;
The XRD figure spectrum of the fluorescent material that Fig. 3 prepares for the embodiment of the invention 16;
The photic emmission spectrum of the fluorescent material that Fig. 4 prepares for the embodiment of the invention 16 under 450nm is blue-light excited;
The photic emmission spectrum of fluorescent material under 450nm is blue-light excited that Fig. 5 prepares for comparative example 1 of the present invention;
The photic emmission spectrum of fluorescent material under 450nm is blue-light excited that Fig. 6 prepares for comparative example 2 of the present invention.
Embodiment
The invention provides a kind of blue-light excited sosoloid fluorescence luminescent material that is used for, have atomic ratio shown in the formula (I):
(1-x)[RE
3-yCe
yM
5O
12]·x[A
3-zMn
zM
2(DO
4)
3](I)；
In the formula (I), RE is one or more among Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu, is preferably among Y, Pr, Nd, Sm, Gd, Tb, Dy, Er, Tm, Yb and the Lu one or more;
M is one or more among B, Al, Ga and the In, is preferably among B and the Al one or both;
A is one or more of Mg, Ca, Sr and Ba, is preferably among Mg, Ca and the Sr one or more;
D is one or more of Si, Ge and Sn, is preferably among Si and the Ge one or more;
0＜x≤0.50, preferred, x meets the following conditions: 0.01≤x≤0.45; Preferred, x meets the following conditions: 0.05≤x≤0.40;
0＜y≤0.30, preferred, y meets the following conditions: 0.01≤y≤0.25; Preferred, y meets the following conditions: 0.05≤y≤0.20;
0＜z≤3, preferred, z meets the following conditions: 0.01≤z≤2.5; Preferred, z meets the following conditions: 0.05≤z≤2.
In the present invention, said sosoloid fluorescence luminescent material is the sosoloid of garnet-base, and is doped with Ce and Mn, makes it expand to red light district at the emmission spectrum under blue-light excited, thereby has good color developing; In addition, said sosoloid fluorescence luminescent material has good adjustability, makes that its emmission spectrum under blue light is adjustable, thereby satisfies the demand of different occasions.
The present invention also provides a kind of technique scheme the described preparation method who is used for blue-light excited sosoloid fluorescence luminescent material, may further comprise the steps:
To contain the RE compound, contain the Ce compound, contain the M compound, contain the Mn compound, contain the A compound and contain the D compound, obtain mixture;
With the roasting under reducing atmosphere of said mixture, obtain being used for blue-light excited sosoloid fluorescence luminescent material.
In the present invention, at first, obtain mixture with each raw materials mix, wherein:
The said RE of containing compound is preferably one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains RE, more preferably contains in oxide compound, oxyhydroxide, halogenide and the carbonate of RE one or more; Said RE is one or more among Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu, is preferably among Y, Pr, Nd, Sm, Gd, Tb, Dy, Er, Tm, Yb and the Lu one or more;
The said Ce of containing compound is preferably one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Ce, more preferably contains in oxide compound, oxyhydroxide, halogenide and the carbonate of Ce one or more;
The said M of containing compound is preferably one or more in oxide compound, oxyhydroxide and the oxygen acid that contains M, more preferably contains the oxide compound of M and in the oxyhydroxide one or both; Said M is one or more among B, Al, Ga and the In, is preferably among B and the Al one or both;
The said A of containing compound is preferably one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains A, more preferably contains in oxide compound, oxyhydroxide, halogenide and the carbonate of A one or more; Said A is one or more of Mg, Ca, Sr and Ba, is preferably among Mg, Ca and the Sr one or more;
The said Mn of containing compound is preferably one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Mn, more preferably contains in oxide compound, oxyhydroxide, halogenide and the carbonate of Mn one or more;
The said D of containing compound is preferably one or more in oxide compound, oxyhydroxide and the oxygen acid that contains D, more preferably contains the oxide compound of D and in the oxyhydroxide one or both; Said D is one or more of Si, Ge and Sn, is preferably among Si and the Ge one or more.
Mix after each raw material fully ground, obtain mixture; With the roasting under reducing atmosphere of said mixture, the atomic ratio shown in (I) that obtains having formula, be used for blue-light excited sosoloid fluorescence luminescent material.In the present invention; The gas atmosphere that said reducing atmosphere can burn in air and produce for carbon; Also can be the reducing gas atmosphere of hydrogen and nitrogen composition, the volume ratio of said hydrogen and nitrogen is preferably (1～20): (99～80), more preferably (5～15): (95～85); The temperature of said roasting is preferably 1400 ℃～1700 ℃, more preferably 1450 ℃～1650 ℃, most preferably is 1500 ℃～1600 ℃; The time of said roasting is preferably 1h～20h, more preferably 3h～18h, more preferably 5h～15h.
In order to reduce the roasting difficulty; The present invention preferably adds fluoride flux in the mixture that each raw material is formed; Said fluoride flux is preferably one or more in Neutral ammonium fluoride, matt salt, lithium fluoride, alkaline-earth metal fluoride and the rare earth metal fluorochemical, more preferably one or more in alkaline-earth metal fluoride and the rare earth metal fluorochemical.The addition of said fusing assistant is preferably below 5% of mixture that said each raw material is formed, and more preferably 0.5%～4.5%, most preferably be 1%～4%.
After roasting finishes, after the sintered compact grinding dispersion that obtains, obtain being used for blue-light excited sosoloid fluorescence luminescent material.
After obtaining the sosoloid fluorescence luminescent material, said sosoloid fluorescence luminescent material is carried out XRD analysis, the result shows that it has atomic ratio shown in the formula (I) and forms;
Use the blue-light excited said sosoloid fluorescence luminescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the sosoloid fluorescence luminescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the preparation of the present invention is simultaneously obviously widened to red light district, can improve the color developing of white light.
Provided by the inventionly be used for blue-light excited sosoloid fluorescence luminescent material and have atomic ratio shown in the formula (I) and form, be the sosoloid of garnet-base, and be doped with Ce and Mn.Sosoloid fluorescence luminescent material provided by the invention stable performance makes that the performance of white light LEDs is also comparatively stable; Excitation spectrum a wider range of sosoloid fluorescence luminescent material provided by the invention, and strong absorption is arranged at the 450nm place, can with commercial blue chip perfect adaptation, obtain well behaved white light LEDs; Sosoloid fluorescence luminescent material provided by the invention is blue-light excited following, and emmission spectrum is obviously expanded to red light district, improved the color developing of sosoloid fluorescence luminescent material, and its emmission spectrum is adjustable, satisfies the demand of different occasions.In addition, preparing method's simple possible, the easy handling of sosoloid fluorescence luminescent material provided by the invention, be easy to volume production, pollution-free, cost is low.
In order to further specify the present invention, the blue-light excited sosoloid fluorescence luminescent material and preparation method thereof that is used for provided by the invention is described in detail below in conjunction with embodiment.
Embodiment 1
Take by weighing Y
2O
333.02 gram, Al
2O
325.24 gram, SiO
20.15 gram, MnCO
30.29 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible; At said mixture surface coverage one deck carbon dust, build crucible cover, put into High Temperature Furnaces Heating Apparatus; 1700 ℃ of following roastings 4 hours, take out when being cooled to 1000 ℃, remove carbon elimination; After grinding dispersion, obtain being used for blue-light excited garnet-base sosoloid fluorescent material, it consists of Y
2.925Ce
0.05Mn
0.025Al
4.975Si
0.025O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 2
Take by weighing Y
2O
332.46 gram, Pr
6O
118.51 gram, Al
2O
325.24 gram, SiO
20.15 gram, MnCO
30.29 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible; At said mixture surface coverage one deck carbon dust, build crucible cover, put into High Temperature Furnaces Heating Apparatus; 1700 ℃ of following roastings 4 hours, take out when being cooled to 1000 ℃, remove carbon elimination; After grinding dispersion, obtain being used for blue-light excited garnet-base sosoloid fluorescent material, it consists of Y
2.875Pr
0.50Ce
0.05Mn
0.025Al
4.975Si
0.025O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 3
Take by weighing Y
2O
329.07 gram, Nd
2O
34.21 gram, Al
2O
324.85 gram, SiO
20.75 gram, MgO 0.40 gram, MnCO
30.29 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 20 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.575Nd
0.25Ce
0.05Mg
0.10Mn
0.025Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 4
Take by weighing Y
2O
331.90 gram, Al
2O
324.85 gram, SiO
20.75 gram, MnCO
31.44 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 12 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.825Ce
0.05Mn
0.125Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Take by weighing Y
2O
330.77 gram, Sm
2O
31.74 gram, Al
2O
324.85 gram, SiO
20.75 gram, CaCO
30.50 gram, MnCO
30.87 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 6 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.725Sm
0.10Ce
0.05Ca
0.05Mn
0.075Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 6
Take by weighing Y
2O
330.48 gram, Al
2O
324.22 gram, SiO
21.50 gram, MnCO
32.87 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1550 ℃ of conditions, 15%H
2/ N
2Roasting is 6 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.70Ce
0.05Mn
0.25Al
4.75Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 7
Take by weighing Y
2O
319.19 gram, Gd
2O
318.13 gram, Al
2O
324.22 gram, SiO
21.50 gram, SrCO
31.47 gram, BaCO
31.97 gram, MnCO
30.57 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 15%H
2/ N
2Roasting is 5 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
1.70Gd
1.00Ce
0.05Sr
0.10Ba
0.10Mn
0.05Al
4.75Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 8
Take by weighing Y
2O
329.92 gram, Al
2O
323.96 gram, SiO
21.80 gram, MnCO
33.45 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1600 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.65Ce
0.05Mn
0.30Al
4.70Si
0.30O
12
Said fluorescent material is carried out XRD analysis, and the result is referring to Fig. 1, and the XRD figure of the fluorescent material that Fig. 1 prepares for the embodiment of the invention 8 spectrum can be known by Fig. 1, and the fluorescent material that the embodiment of the invention prepares has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm; The result is referring to Fig. 2; The photic emmission spectrum of the fluorescent material that Fig. 2 prepares for the embodiment of the invention 8 under 450nm is blue-light excited can be known by Fig. 2, excitation spectrum a wider range of the fluorescent material of the present invention's preparation; At the 450nm place strong absorption is arranged, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 9
Take by weighing Y (OH)
330.78 gram, Tb
4O
79.35 gram, Al
2O
323.71 gram, H
3BO
30.62 gram, SiO
21.50 gram, CaCO
32.50 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 20%H
2/ N
2Roasting is 16 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.20Tb
0.50Ce
0.05Ca
0.25Al
4.65B
0.10Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Take by weighing YCl
331.24 gram, Lu
2O
319.90 gram, Al
2O
324.22 gram, H
2SiO
31.95 gram, MgO0.40 gram, SrCO
32.21 gram and CeF
32.96 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible; At said mixture surface coverage one deck carbon dust, build crucible cover, put into High Temperature Furnaces Heating Apparatus; 1650 ℃ of following roastings 3 hours, take out when being cooled to 1000 ℃, remove carbon elimination; After grinding dispersion, obtain being used for blue-light excited garnet-base sosoloid fluorescent material, it consists of Y
1.60Lu
1.00Ce
0.15Sr
0.15Mg
0.10Al
4.75Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 11
Take by weighing YCl
331.24 gram, Dy
2O
39.33 gram, Tb (NO
3)
317.25 gram, Al
2O
324.22 gram, SiO
21.50 gram, MnO
22.17 gram and CeO
22.58 gram carries out abundant ground and mixed, puts into alumina crucible, and the mixture that obtains is put into alumina crucible; At said mixture surface coverage one deck carbon dust, build crucible cover, put into High Temperature Furnaces Heating Apparatus; 1500 ℃ of following roastings 8 hours, take out when being cooled to 1000 ℃, remove carbon elimination; After grinding dispersion, obtain being used for blue-light excited garnet-base sosoloid fluorescent material, it consists of Y
1.60Tb
0.50Dy
0.50Ce
0.15Mn
0.25Al
4.75Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 12
Take by weighing Tb
4O
754.21 gram, Al
2O
325.24 gram, SiO
20.30 gram, CaCO
30.50 gram and Ce (NO
3)
31.63 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1700 ℃ of conditions, 20%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Tb
2.90Ce
0.05Ca
0.05Al
4.95Si
0.05O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 13
Take by weighing TbCl
372.55 gram, Ho
2O
39.45 gram, Al
2O
322.59 gram, Ga
2O
34.69 gram, H
4SiO
40.72 gram, MnCO
30.86 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 10%H
2/ N
2Roasting is 20 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Tb
2.735Ho
0.50Ce
0.15Mn
0.075Al
4.425Ga
0.50Si
0.075O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 14
Take by weighing TbCl
372.55 gram, Er
2O
39.56 gram, Al
2O
322.59 gram, B
2O
31.74 gram, H
4SiO
40.72 gram, MnCO
30.86 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 10%H
2/ N
2Roasting is 20 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Tb
2.735Er
0.50Ce
0.15Mn
0.075Al
4.425B
0.50Si
0.075O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 15
Take by weighing Lu
2O
357.70 gram, Al
2O
325.24 gram, SiO
20.30 gram, MnCO
30.57 gram, B
2O
30.35 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1650 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.90Ce
0.05Mn
0.05Al
4.85B
0.10Si
0.05O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 16
Take by weighing Lu
2O
355.71 gram, Al
2O
324.72 gram, SiO
20.90 gram, MnCO
30.57 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1600 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.80Ce
0.05Mn
0.15Al
4.85Si
0.15O
12
Said fluorescent material is carried out XRD analysis, and the result is referring to Fig. 3, and the XRD figure of the fluorescent material that Fig. 3 prepares for the embodiment of the invention 16 spectrum can be known by Fig. 3, and the fluorescent material that the embodiment of the invention prepares has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm; The result is referring to Fig. 4; The photic emmission spectrum of the fluorescent material that Fig. 4 prepares for the embodiment of the invention 16 under 450nm is blue-light excited can be known by Fig. 4, excitation spectrum a wider range of the fluorescent material of the present invention's preparation; At the 450nm place strong absorption is arranged, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 17
Take by weighing Lu
2O
345.76 gram, Er
2O
39.56 gram, Al
2O
324.72 gram, SiO
20.30 gram, GeO
21.05 gram, MnCO
30.57 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1600 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.30Er
0.50Ce
0.05Mn
0.15Al
4.85Si
0.05Ge
0.10O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 18
Take by weighing Lu (OH)
345.20 gram, Y
2O
36.77 gram, Al (NO
3)
3.9H
2O 169.64 grams, SiO
21.50 gram, MnCO
30.57 gram, CaF
21.56 gram and CeO
22.58 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 10%H
2/ N
2Roasting is 8 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.00Y
0.60Ce
0.15Mn
0.05Ca
0.20Al
4.75Si
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 19
Take by weighing LuCl
356.27 gram, Tb
4O
713.08 gram, AlCl
366.00 gram, SiO
20.30 gram, MnCO
32.88 gram and CeO
22.58 gram carries out abundant ground and mixed, puts into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1450 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.00Tb
0.70Ce
0.25Mn
0.05Al
4.95Si
0.05O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Take by weighing Lu
2O
349.74 gram, Tm
2O
31.93 gram, Al
2O
324.98 gram, SiO
20.30 gram, GeO
20.52 gram, MnCl
21.26 gram and CeCl
37.39 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1550 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.50Tm
0.10Ce
0.30Mn
0.10Al
4.90Si
0.05Ge
0.05O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 21
Take by weighing Lu
2O
344.77 gram, Al
2O
312.75 gram, Ga
2O
314.06 gram, In
2O
36.94 gram, SiO
23.00 gram, MnCO
35.75 gram and CeO
28.63 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1600 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.25Ce
0.25Mn
0.50Al
2.50Ga
1.50In
0.50Si
0.50O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 22
Take by weighing Lu
2O
343.77 gram, Yb
2O
30.99 gram, Al
2O
312.75 gram, Ga
2O
318.74 gram, SiO
21.50 gram, GeO
22.60 gram, MnCO
35.75 gram and CeO
28.63 gram carries out abundant ground and mixed, puts into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.20Yb
0.05Ce
0.25Mn
0.50Al
2.50Ga
2.00Si
0.25Ge
0.25O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 23
Take by weighing Lu
2O
344.77 gram, Al
2O
312.75 gram, Ga
2O
318.74 gram, SiO
21.50 gram, GeO
21.30 gram, SnO
21.88 gram, MnCO
35.75 gram and CeO
28.63 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 5 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Lu
2.25Ce
0.25Mn
0.50Al
2.50Ga
2.00Si
0.25Ge
0.125Sn
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 24
Take by weighing Y
2O
331.90 gram, Al
2O
324.85 gram, SiO
20.75 gram, MnCO
31.44 gram, CeO
20.86 gram, NaF 0.06 gram and NH
4HF
20.10 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1600 ℃ of conditions, 10%H
2/ N
2Roasting is 1 hour under the atmosphere, takes out when being cooled to room temperature, and grinding obtains being used for blue-light excited garnet-base sosoloid fluorescent material after disperseing, and it consists of Y
2.825Ce
0.05Mn
0.125Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 25
Take by weighing Y
2O
331.90 gram, Al
2O
324.85 gram, SiO
20.75 gram, MnCO
31.44 gram, CeO
20.86 gram and CaF
20.16 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 4 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Y
2.825Ce
0.05Mn
0.125Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 26
Take by weighing Y
2O
331.90 gram, Al
2O
324.85 gram, SiO
20.75 gram, SrCO
31.85 gram, CeO
20.86 gram, LiF 0.03 gram and SrF
20.13 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Y
2.825Ce
0.05Sr
0.125Al
4.875Si
0.125O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 27
Take by weighing Lu
2O
355.71 gram, Al
2O
324.72 gram, SiO
20.90 gram, MgO 0.60 gram, CeO
20.86 gram, LaF
30.12 gram and NH
4HF
20.10 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1450 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Lu
2.80Ce
0.05Mg
0.15Al
4.85Si
0.15O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 28
Take by weighing Lu
2O
355.71 gram, Al
2O
324.72 gram, SiO
20.90 gram, MnCO
30.57 gram, CeO
20.86 gram, NH
4F 0.10 gram and BaF
20.08 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1400 ℃ of conditions, 10%H
2/ N
2Roasting is 6 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Lu
2.80Ce
0.05Mn
0.15Al
4.85Si
0.15O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Embodiment 29
Take by weighing Lu
2O
355.71 gram, Al
2O
324.72 gram, SiO
20.90 gram, MnCO
30.57 gram, CeO
20.86 gram, AlF
30.14 gram and GdF
30.06 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1450 ℃ of conditions, 10%H
2/ N
2Roasting is 6 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Lu
2.80Ce
0.05Mn
0.15Al
4.85Si
0.15O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Take by weighing Lu
2O
355.71 gram, Al
2O
324.72 gram, SiO
20.90 gram, MnCO
30.57 gram, CeO
20.86 gram, LuF
30.10 gram and NH
4HF
20.10 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 1 hour under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Lu
2.80Ce
0.05Mn
0.15Al
4.85Si
0.15O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm, the result shows that excitation spectrum a wider range of the fluorescent material of the present invention's preparation has strong absorption at the 450nm place, can better combine by blue chip; The emmission spectrum of the fluorescent material of the present invention's preparation is widened to red light district, can improve the color developing of white light.
Comparative example 1
Take by weighing Y
2O
333.31 gram, Al
2O
325.49 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1650 ℃ of conditions, 10%H
2/ N
2Roasting is 3 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Y
2.95Ce
0.05Al
5O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms
Use the blue-light excited said fluorescent material of wavelength as 450nm; The result is referring to Fig. 5; The photic emmission spectrum of fluorescent material under 450nm is blue-light excited that Fig. 5 prepares for comparative example 1 of the present invention can be known by Fig. 5, and the emmission spectrum of the fluorescent material of comparative example 1 preparation is broad in the yellow green light district; Red light district is not enough, and the color developing of the white light that obtains is relatively poor.
Comparative example 2
Take by weighing Lu
2O
358.69 gram, Al
2O
325.49 gram and CeO
20.86 gram carries out abundant ground and mixed, and the mixture that obtains is put into alumina crucible, builds crucible cover, puts into High Temperature Furnaces Heating Apparatus, at 1500 ℃ of conditions, 10%H
2/ N
2Roasting is 8 hours under the atmosphere, takes out when being cooled to room temperature, and grinding obtains blue-light excited phosphor for white light LED after disperseing, and it consists of Lu
2.95Ce
0.05Al
5O
12
Said fluorescent material is carried out XRD analysis, and the result shows that it has above-mentioned atomic ratio and forms;
Use the blue-light excited said fluorescent material of wavelength as 450nm; The result is referring to Fig. 6; The photic emmission spectrum of fluorescent material under 450nm is blue-light excited that Fig. 6 prepares for comparative example 2 of the present invention can be known by Fig. 6, and the emmission spectrum of the fluorescent material of comparative example 2 preparations is at the green Region broad; Red light district is not enough, and the color developing of the white light that obtains is relatively poor.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. one kind is used for blue-light excited sosoloid fluorescence luminescent material, has atomic ratio shown in the formula (I):
(1-x)[RE
3-yCe
yM
5O
12]·x[A
3-zMn
zM
2(DO
4)
3](I)；
In the formula (I), RE is one or more among Y, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb and the Lu;
M is one or more among B, Al, Ga and the In;
A is one or more of Mg, Ca, Sr and Ba;
D is one or more of Si, Ge and Sn;
0＜x≤0.50；
0＜y≤0.30；
0＜z≤3。
2. sosoloid fluorescence luminescent material according to claim 1 is characterized in that, said M is one or both among B and the Al.
3. claim 1 or the 2 described preparing methods that are used for blue-light excited sosoloid fluorescence luminescent material may further comprise the steps:
To contain the RE compound, contain the Ce compound, contain the M compound, contain the Mn compound, contain the A compound and contain the D compound, obtain mixture;
With the roasting under reducing atmosphere of said mixture, obtain being used for blue-light excited sosoloid fluorescence luminescent material.
4. preparation method according to claim 3 is characterized in that, the said RE of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains RE.
5. preparation method according to claim 3 is characterized in that, the said Ce of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Ce.
6. preparation method according to claim 3 is characterized in that, the said M of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains M.
7. preparation method according to claim 3; It is characterized in that; The said A of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains A, and the said Mn of containing compound is one or more in oxide compound, oxyhydroxide, nitrate salt, halogenide and the carbonate that contains Mn.
8. preparation method according to claim 3 is characterized in that, the said D of containing compound is one or more in oxide compound, oxyhydroxide and the oxygen acid that contains D.
9. according to any described preparation method of claim 3～8, it is characterized in that said mixture also comprises fluoride flux.
10. preparation method according to claim 9 is characterized in that, the temperature of said roasting is 1400 ℃～1700 ℃, and the time of said roasting is 1h～20h.
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| CN105658763A (en) * | 2013-10-21 | 2016-06-08 | 默克专利有限公司 | Phosphors |
| CN110564419A (en) * | 2019-09-26 | 2019-12-13 | 广东省稀有金属研究所 | Cerium-manganese co-activated garnet-structured fluorescent powder and preparation method thereof |
| CN110746971A (en) * | 2019-11-19 | 2020-02-04 | 吉安县惠鑫实业有限责任公司 | Mn/Ce co-doped gadolinium aluminum garnet-based fluorescent powder |
| CN111285682A (en) * | 2018-12-07 | 2020-06-16 | 上海航空电器有限公司 | Full-spectrum complex phase fluorescent ceramic for laser illumination and display and preparation method thereof |
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