CN1482208A - Blue light-excitated white phosphor powder for LED and production method thereof - Google Patents
Blue light-excitated white phosphor powder for LED and production method thereof Download PDFInfo
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- CN1482208A CN1482208A CNA021309493A CN02130949A CN1482208A CN 1482208 A CN1482208 A CN 1482208A CN A021309493 A CNA021309493 A CN A021309493A CN 02130949 A CN02130949 A CN 02130949A CN 1482208 A CN1482208 A CN 1482208A
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- phosphor powder
- white phosphor
- blue
- fusing assistant
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- 239000000843 powder Substances 0.000 title claims abstract description 19
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000000975 co-precipitation Methods 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 229910052738 indium Inorganic materials 0.000 claims abstract description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 6
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 6
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 5
- 229910052796 boron Inorganic materials 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052728 basic metal Inorganic materials 0.000 claims description 2
- 150000003818 basic metals Chemical class 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 229910052777 Praseodymium Inorganic materials 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 229910052772 Samarium Inorganic materials 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 229910052732 germanium Inorganic materials 0.000 abstract 1
- 229910052746 lanthanum Inorganic materials 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 239000012190 activator Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- -1 add fusing assistant Substances 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Abstract
The phosphor powder for blue light excited white LED has the structural expression of R(3-x-y)M5O12:CexR'y, where R is at least one of Y, Gd, Lu, Sc, La and Sm; M is at least one of B, Al, Ga, In, P, Ge and Zn; x is 0.01-1; R' is one or several of Tb, Eu, Dy, Pr and Mn; and y is 0-0.5. The material is prepared with the simple substance, oxide or corresponding salts and through grinding, coprecipitation, mixing fluxing agent, reduction at high temperature and post-treatment. The phosphor powder of the present invention has high light-emitting brightness, homogeneous granularity, emitting wavelength capable of being regulated based on requirement, wide excited wavelength, high chemical stability and other features. The preparation process is simple, pollution-less and low cost.
Description
Technical field
The present invention relates to a kind of blue-light excited white phosphor powder for LED and manufacture method thereof.
Background technology
Coating can effectively be excited by blue light efficiently and launch the fluorescent material of gold-tinted on the blue led chip, can obtain White LED.The research success of White LED light source is for condition has been created in the application of LED in general lighting.Be characterized in having little electric current, at room temperature can obtain enough brightness, luminescence response is fast, stable performance, the life-span is long, and volume is little, durable in use, therefore advantages such as shock resistance are widely used in fields such as general lighting, pilot lamp, signals, will replace more than 30% of existing general lighting incandescent light according to relevant expert's prediction its consumption in 30 years of future.
At present, the White LED that this kind method is made is very high to the performance requriements of fluorescent material, mainly is that luminosity is wanted height, and excitation wave length and width, powder granule size want little and even.This kind fluorescent material mainly is the YAG yttrium aluminum garnet, and chemical formula is: (Y, Gd)
3(Al, Ga)
5O
12: Ce.
Y/Gd ratio in the United States Patent (USP) 5998925 report YAG:Ce fluorescent material, the changing conditions of light-emitting phosphor peak wavelength behind Al/Ga ratio and the adding Sm.
Summary of the invention
The purpose of this invention is to provide a kind of blue-light excited white phosphor powder for LED that a kind of luminous intensity height, excitation wave length and width and emission main peak can move in very wide scope.
Another object of the present invention provides a kind of manufacture method of simple, pollution-free, blue-light excited white phosphor powder for LED that cost is low.
For achieving the above object, the present invention takes following technical scheme: material structure formula of the present invention is: R
(3-x-y)M
5O
12: Ce
xR '
y, wherein R is Y, Gd, and Lu, Sc, at least a among La and the Sm; M is B, Al, and Ga, In, P, at least a among Ge and the Zn; 0.001＜x＜1; R ' can be Tb, Eu, Dy, among Pr and the Mn one or more; 0≤y＜0.5.
The present invention systematically studies matrix, the activator of fluorescent material, add multiple new rare earth and non-rare earth therein, and study the proportionlity of various element the bests, the light-emitting phosphor intensity height of acquisition, the excitation wave length and width, and the emission main peak can move in very wide scope.
In blue-light excited white phosphor powder for LED of the present invention, the medium particle diameter (D of described fluorescent material
50) in 1～5um scope.
The method of blue-light excited white phosphor powder for LED of the present invention comprises the steps:
(1) presses structural formula: R
(3-x-y)M
5O
12: Ce
xR '
yPrepare burden, wherein: R is Y, Gd, Lu, Sc, at least a among La and the Sm, M is B, Al, Ga, In, P, at least a among Ge and the Zn, 0.001＜x＜1, R ' can be Tb, Eu, Dy, among Pr and the Mn one or more, 0≤y＜0.5, according to
The proportioning of above-mentioned structural formula takes by weighing simple substance or its oxide compound or its corresponding salt of above-mentioned element, as raw material;
(2) carry out reducing roasting then;
(3) with above-mentioned reduzate washing, filter, oven dry obtains the finished product, and promptly obtaining body colour is light yellow or the xanchromatic powder---fluorescent material of the present invention.
The present invention obtains a series of various aspects of performance excellences by aforesaid method, can be widely used in the fluorescent material of White LED.
In aforesaid method,, be about to above-mentioned raw materials and carry out co-precipitation and handle in described step (2) also (2 ') in steps before.With coprecipitation method raw material is carried out pre-treatment, the particle diameter by co-precipitation control raw material can obtain the fluorescent material of scope at any medium particle diameter of 1～4um, and improve the homogeneity of size-grade distribution.On the other hand since co-precipitation that raw material is mixed is more even, thereby the luminous intensity of fluorescent material is increased.The size of the particle size of powder and homogeneity also are the important indicators of fluorescent material, and it rings more obvious to the system lamp shadow.The present invention has obtained medium particle diameter (D by control and soft chemical preparation method to raw material particle size
50) white phosphor powder for LED that can in 1～5um scope, change arbitrarily, and improved the homogeneity of size-grade distribution.
In aforesaid method, between described step (2 ') and step (2) (2 ") also in steps, promptly in above-mentioned raw materials, add fusing assistant, and mix.Add fusing assistant and can improve crystal formation quality, thereby can improve the performance of fluorescent material.
In aforesaid method, described fusing assistant is any one fluorochemical or muriate of alkaline-earth metal, basic metal, rare earth metal, aluminium, gallium, indium, and is at least a in boric acid, the boron oxide.
In aforesaid method, the per-cent that described fusing assistant accounts for gross weight (being the weight of fusing assistant and above-mentioned raw materials) is 0.001%～10wt%.
In aforesaid method, in the described step (2), the reducing roasting temperature is 1100～1600 ℃.
In aforesaid method, in the described step (2), the reducing roasting time is 0.5～15h.
Advantage of the present invention is: (1) can obtain the white phosphor powder for LED that the high peak position of luminous intensity can change arbitrarily by composition that changes the matrix element and the ratio of regulating each element; (2) in activator, add Tb, Eu, Dy, Pr, novel substances such as Mn can change the emission peak position of powder; Improved the luminous intensity (3) of powder and starting material have been carried out pre-treatment, can obtain the fluorescent material of scope, and improved the homogeneity of size-grade distribution at any medium particle diameter of 1～4um by coprecipitation method.
The fluorescent material of gained of the present invention can be used for making white light-emitting diode.
Embodiment
Embodiment 1: take by weighing Y
2O
33.1316g, Gd
2O
31.6753g, Al (OH)
34.9736g, CeO
20.2195g, add the fusing assistant BaF of gross weight 1% again
2, H
3BO
3, it is pure that above raw material is top grade, with above raw material mix grinding evenly after, roasting is 2 hours under 1400 ℃ of reductive conditions, promptly obtaining molecular composition is Y
2.175Gd
0.725Al
5O
12: Ce
0.1Sample, its emission peak wavelength be higher than comparative example, brightness is higher than comparative example.
Comparative example: take by weighing Y
2O
34.596g, Al (OH)
35.2874g, CeO
20.1166g its fusing assistant content and manufacture method are all identical with embodiment 1, obtaining molecular composition is Y
2.94Al
5O
12: Ce
0.1Sample.
Embodiment 2～embodiment 71: change matrix, the activator of embodiment 1, list in the table according to its relative brightness of chemical dosage ratio synthetic sample and the emission peak wavelength of following molecular formula.
Table 1
| Embodiment | Molecular formula | Relative brightness (%) | Emission main peak (nm) |
| ????1 | ????Y 2.175Gd 0.725A l5O 12:Ce 0.1 | ????115 | ????548 |
| ????2 | ????Y 1.933Gd 0.967Al 5O 12:Ce 0.1 | ????120 | ????553 |
| ????3 | ????Y 1.45Gd 1.45Al 5O 12:Ce 0.1 | ????123 | ????559 |
| ????4 | ????Y 0.967Gd 1.933Al 5O 12:Ce 0.1 | ????118 | ????565 |
| ????5 | ????Y 0.725Gd 2.175Al 5O 12:Ce 0.1 | ????117 | ????573 |
| ????6 | ????Y 1.48Gd 1.48AL 5O 12:Ce 0.04 | ????114 | ????560 |
| ????7 | ????Y 1.47Gd 1.47Al 5O 12:Ce 0.06 | ????116 | ????557 |
| ????8 | ????Y 1.46Gd 1.46Al 5O 12:Ce 0.08 | ????118 | ????557 |
| ????9 | ????Y 1.425Gd 1.425Al 5O 12:Ce 0.15 | ????119 | ????557 |
| ????10 | ????Y 1.4Gd 1.4Al 5O 12:Ce 0.2 | ????110 | ????559 |
| ????11 | ????Y 2.61Lu 0.29Al 5O 12:Ce 0.1 | ????118 | ????538 |
| ????12 | ????Y 2.232Lu 0.58Al 5O 12:Ce 0.1 | ????122 | ????535 |
| ????13 | ????Y 1.933Lu 0.967Al 5O 12:Ce 0.1 | ????116 | ????534 |
| ????14 | ????Y 2.61Sc 0.29Al 5O 12:Ce 0.1 | ????110 | ????538 |
| ????15 | ????Y 2.232Sc 0.58Al 5O 12:Ce 0.1 | ????115 | ????534 |
| ????16 | ????Y 1.933Sc 0.967Al 5O 12:Ce 0.1 | ????111 | ????532 |
| ????17 | ????Y 1.933La 0.967Al 5O 12:Ce 0.1 | ????113 | ????535 |
| ????18 | ????Y 1.74La 1.16Al 5O 12:Ce 0.1 | ????118 | ????534 |
| ????19 | ????Y 1.45La 1.45Al 5O 12:Ce 0.1 | ????116 | ????536 |
| ????20 | ????Y 1.933Sm 0.967Al 5O 12:Ce 0.1 | ????102 | ????536 |
| ????21 | ????Y 2.61Sm 0.29Al 5O 12:Ce 0.1 | ????105 | ????538 |
| ????22 | ????Y 1.724Gd 0.872Lu 0.304Al 5O 12:Ce 0.1 | ????123 | ????550 |
| ????23 | ????Y 1.440Gd 0.872Lu 0.588Al 5O 12:Ce 0.1 | ????125 | ????547 |
| ????24 | ????Y 1.156Gd 0.872Lu 0.872Al 5O 12:Ce 0.1 | ????124 | ????549 |
| ????25 | ????Y 1.440Gd 0.872Sc 0.588Al 5O 12:Ce 0.1 | ????123 | ????546 |
| ????26 | ????Y 1.440Gd 0.872La 0.588Al 5O 12:Ce 0.1 | ????125 | ????545 |
| ????27 | ????Y 1.440Gd 0.872Sm 0.588Al 5O 12:Ce 0.1 | ????124 | ????543 |
| ????28 | ????Y 1.435Gd 0.867Lu 0.299Sc 0.299Al 5O 12:Ce 0.1 | ????129 | ????542 |
| ????29 | ????Y 1.435Gd 0.867Lu 0.299La 0.299Al 5O 12:Ce 0.1 | ????113 | ????541 |
| ????30 | ????Y 1.435Gd 0.867Lu 0.299Sm 0.299Al 5O 12:Ce 0.1 | ????111 | ????544 |
| ????31 | ????Y 1.148Gd 0.864Lu 0.296Sc 0.296La 0.296Al 5O 12:Ce 0.1 | ????125 | ????538 |
| ????32 | ????Y 1.148Gd 0.864Lu 0.296Sc 0.296Sm 0.296Al 5O 12:Ce 0.1 | ????120 | ????533 |
| ????33 | ????Y 2.9Al 4.5Ga 0.5O 12:Ce 0.1 | ????126 | ????530 |
| ????34 | ????Y 2.9Al 4.0Ga 1.0O 12:Ce 0.1 | ????129 | ????524 |
| ????35 | ????Y 2.9Al 3.5Ga 1.5O 12:Ce 0.1 | ????133 | ????520 |
| ????36 | ????Y 2.9Al 3.0Ga 2.0O 12:Ce 0.1 | ????134 | ????515 |
| ????37 | ????Y 2.9Al 2.5Ga 2.5O 12:Ce 0.1 | ????138 | ????511 |
| ????38 | ????Y 2.9Al 4.0B 1.0O 12:Ce 0.1 | ????109 | ????531 |
| ????39 | ????Y 2.9Al 3.5B 1.5O 12:Ce 0.1 | ????115 | ????535 |
| ????40 | ????Y 2.9Al 3.0B 2.0O 12:Ce 0.1 | ????113 | ????534 |
| ????41 | ????Y 2.9Al 3.5In 1.5O 12:Ce 0.1 | ????107 | ????532 |
| ????42 | ????Y 2.9Al 3.5P 1.5O 12:Ce 0.1 | ????103 | ????546 |
| ????43 | ????Y 2.9Al 3.5Ge 1.5O 12:Ce 0.1 | ????105 | ????537 |
| ????44 | ????Y 2.9Al 3.5Zn 1.5O 12:Ce 0.1 | ????111 | ????549 |
| ????45 | ????Y 2.9Al 4.0B 0.5Zn 0.5O 12:Ce 0.1 | ????119 | ????540 |
| ????46 | ????Y 2.9Al 3.5B 1.0Zn 0.5O 12:Ce 0.1 | ????113 | ????535 |
| ????47 | ????Y 2.899Al 5O 12:Ce 0.1Eu 0.001 | ????106 | ????546 |
| ????48 | ????Y 2.897Al 5O 12:Ce 0.1Eu 0.003 | ????108 | ????549 |
| ????49 | ????Y 2.895Al 5O 12:Ce 0.1Eu 0.005 | ????111 | ????555 |
| ????50 | ????Y 2.893Al 5O 12:Ce 0.1Eu 0.007 | ????113 | ????560 |
| ????51 | ????Y 2.89Al 5O 12:Ce 0.1Eu 0.010 | ????110 | ????559 |
| ????52 | ????Y 1.4495Gd 1.4495Al 5O 12:Ce 0.1Eu 0.001 | ????113 | ????556 |
| ????53 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Eu 0.003 | ????118 | ????560 |
| ????54 | ????Y 1.4475Gd 1.4475Al 5O 12:Ce 0.1Eu 0.005 | ????116 | ????565 |
| ????55 | ????Y 1.4465Gd 1.4465Al 5O 12:Ce 0.1Eu 0.007 | ????120 | ????581 |
| ????56 | ????Y 1.445Gd 1.445Al 5O 12:Ce 0.1Eu 0.010 | ????115 | ????580 |
| ????57 | ????Y 1.4495Gd 1.4495Al 5O 12:Ce 0.1Tb 0.001 | ????113 | ????541 |
| ????58 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Tb 0.003 | ????111 | ????556 |
| ????59 | ????Y 1.4475Gd 1.4475Al 5O 12:Ce 0.1Tb 0.005 | ????108 | ????533 |
| ????60 | ????Y 2.896Al 5O 12:Ce 0.1Eu 0.003Tb 0.001 | ????117 | ????550 |
| ????61 | ????Y 2.894Al 5O 12:Ce 0.1Eu 0.003Tb 0.003 | ????119 | ????538 |
| ????62 | ????Y 1.449Gd 1.449Al 5O 12:Ce 0.1Eu 0.001Tb 0.001 | ????118 | ????539 |
| ????63 | ????Y 1.448Gd 1.448Al 5O 12:Ce 0.1Eu 0.003Tb 0.001 | ????123 | ????554 |
| ????64 | ????Y 1.448Gd 1.448Al 5O 12:Ce 0.1Eu 0.001Tb 0.003 | ????117 | ????538 |
| ????65 | ????Y 1.447Gd 1.447Al 5O 12:Ce 0.1Eu 0.003Tb 0.003 | ????120 | ????546 |
| ????66 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Dy 0.003 | ????109 | ????534 |
| ????67 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Pr 0.003 | ????102 | ????536 |
| ????68 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Mn 0.003 | ????111 | ????533 |
| ????69 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Eu 0.001Tb 0.001Dy 0.001 | ????124 | ????530 |
| ????70 | ????Y 1.448Gd 1.448Al 5O 12:Ce 0.1Eu 0.001Tb 0.001Pr 0.002 | ????126 | ????532 |
| ????71 | ????Y 1.4485Gd 1.4485Al 5O 12:Ce 0.1Eu 0.001Tb 0.001Mn 0.001 | ????120 | ????529 |
| Comparative example | ????Y 2.9Al 5O 12:Ce 0.1 | ????100 | ????543 |
Embodiment 72: with coprecipitation method raw material is carried out pre-treatment, the particle diameter by co-precipitation control raw material can obtain the fluorescent material of scope at any medium particle diameter of 1～4um, and improve the homogeneity of size-grade distribution.On the other hand since the co-precipitation meeting that raw material is mixed is more even, thereby the luminous intensity of fluorescent material is increased.Press Y
1.45Gd
1.45Al
5O
12: Ce
0.1Ratio takes by weighing Y
2O
31.9637g, Gd
2O
33.1516g, Al (NO
3)
39H
2O 22.73g, CeO
20.2065g it is pure that above raw material is top grade, at first uses ebullient nitric acid with Y
2O
3, Gd
2O
3, Al (NO
3)
39H
2O, CeO
2, dissolving respectively, with the mutual uniform mixing of each solution, liquation is still clarified.To wherein adding oxalic acid solution, add the concentration of oxalic acid and the granularity that speed can be controlled raw material by control.The raw material of the material that precipitates after obtaining handling behind 850 ℃ of sintering, this sample donor center particle diameter 0.3um.The fusing assistant BaF that adds gross weight 1% again
2, H
3BO
3, mix grinding is even, and roasting obtained sample in 2 hours under 1400 ℃ of reductive conditions, and medium particle diameter is 0.934nm.Its brightness is higher than comparative example.
Embodiment 73～78: dissolve each raw material according to the method for embodiment 72, control settling velocity by the concentration and the speed that add oxalic acid, the raw material granularity of making is respectively 0.5,1.0,1.5,2.0,2.5, the fluorescent material of 3.0um.The relative brightness and the medium particle diameter of the sample made from this raw material are listed in table 2
Table 2
| Numbering | Donor center particle diameter (um) | Relative brightness % | Product center particle diameter (D 50) |
| ????72 | ????0.3 | ????116 | ????0.934 |
| ????73 | ????0.5 | ????123 | ????1.215 |
| ????74 | ????1.0 | ????130 | ????1.854 |
| ????75 | ????1.5 | ????137 | ????2.341 |
| ????76 | ????2.0 | ????132 | ????2.964 |
| ????77 | ????2.5 | ????126 | ????3.513 |
| ????78 | ????3.0 | ????124 | ????4.232 |
| Comparative example | ????100 | ????4.537 |
In sum, characteristics such as fluorescent material of the present invention has that luminosity height, epigranular, emission wavelength can be regulated as required, excitation wave length and width, chemical stability are good, manufacture method is simple, pollution-free, cost is low.
Claims (9)
1, a kind of blue-light excited white phosphor powder for LED, it is characterized in that: the structural formula of the white phosphor powder for LED that this is blue-light excited is: R
(3-x-y)M
5O
12: Ce
xR '
y
Wherein: R is Y, Gd, and Lu, Sc, at least a among La and the Sm;
M is B, Al, and Ga, In, P, at least a among Ge and the Zn;
0.001＜x＜1；
R ' can be Tb, Eu, Dy, one or more among Pr and the Mn;
0≤y＜0.5。
2, blue-light excited white phosphor powder for LED according to claim 2 is characterized in that: the medium particle diameter (D of described fluorescent material
50) in 1～5um scope.
3, a kind of method of making the described blue-light excited white phosphor powder for LED of claim 1, it is characterized in that: this method comprises the steps:
(1) structural formula: R
(3-x-y)M
5O
12: Ce
xR '
yPrepare burden, wherein: R is Y, Gd, and Lu,
Sc, at least a among La and the Sm, M is B, Al, Ga, In, P, at least a among Ge and the Zn,
0.001＜x＜1, R ' is Tb, Eu, Dy, among Pr and the Mn one or more, 0≤y＜0.5, according to
The proportioning of above-mentioned structural formula takes by weighing simple substance or its oxide compound or its corresponding salt of above-mentioned element, does
Be raw material;
(2) carry out reducing roasting then;
(3) with above-mentioned reduzate washing, filter, oven dry obtains the finished product.
4, method according to claim 3 is characterized in that: in described step (2) also (2 ') in steps before, be about to above-mentioned raw materials and carry out co-precipitation and handle.
5, method according to claim 4 is characterized in that: between described step (2 ') and step (2) (2 ") also in steps, promptly add fusing assistant in above-mentioned raw materials, and mix.
6, method according to claim 5 is characterized in that: described fusing assistant is any one fluorochemical or muriate of alkaline-earth metal, basic metal, rare earth metal, aluminium, gallium, indium, and is at least a in boric acid, the boron oxide.
7, method according to claim 6 is characterized in that: the per-cent that described fusing assistant accounts for gross weight (being the weight of fusing assistant and above-mentioned raw materials) is 0.001%～10wt%.
8, according to claim 3 or 4 or 7 described methods, it is characterized in that: in the described step (2), the reducing roasting temperature is 1100～1600 ℃.
9, method according to claim 8 is characterized in that: in the described step (2), the reducing roasting time is 0.5～15h.
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