CN101012375A - Rare earth red fluorescent powder and preparing method thereof - Google Patents
Rare earth red fluorescent powder and preparing method thereof Download PDFInfo
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- CN101012375A CN101012375A CN 200710019706 CN200710019706A CN101012375A CN 101012375 A CN101012375 A CN 101012375A CN 200710019706 CN200710019706 CN 200710019706 CN 200710019706 A CN200710019706 A CN 200710019706A CN 101012375 A CN101012375 A CN 101012375A
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- 239000000843 powder Substances 0.000 title claims abstract description 31
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 8
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 8
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 8
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 8
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 7
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 6
- 229910052788 barium Inorganic materials 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 abstract 1
- 239000011812 mixed powder Substances 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 6
- 239000003086 colorant Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 238000005090 crystal field Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种稀土红色荧光粉，其特征在于结构式为MaNbSicO(2c+a+3b/2)：Eux，Ry；其中，M为Mg、Ca、Sr或Ba中的至少一种，0.05＜a＜3.0；N为Y、La或Gd中的至少一种，0＜b＜5.0；R为Ce、Pr、Nd、Sm、Tb、Dy或Er中的至少一种；1.0＜c＜4.0；0.001＜x＜5；0.0001＜y＜0.5。一种制备稀土红色荧光粉的方法，该方法包括下述步骤：以Si、Mg、Ca、Sr、Ba、Y、La、Gd、Ce、Pr、Nd、Sm、Tb、Dy或Er的氧化物或它们的碳酸盐或硝酸盐为原料，并按材料的结构式组成及化学计量比称取所述原料；将各原料搅拌充分混匀，置于空气中灼烧，混匀粉体的灼烧温度为900～1550℃，灼烧时间为2～12h；经研磨、筛选后，即制成稀土激活的红色荧光粉。
A rare earth red phosphor, characterized in that the structural formula is M a N b Si c O (2c+a+3b/2) : Eu x , R y ; wherein, M is at least one of Mg, Ca, Sr or Ba species, 0.05<a<3.0; N is at least one of Y, La or Gd, 0<b<5.0; R is at least one of Ce, Pr, Nd, Sm, Tb, Dy or Er; 1.0<c<4.0;0.001<x<5;0.0001<y<0.5. A method for preparing rare earth red fluorescent powder, the method comprising the steps of: using Si, Mg, Ca, Sr, Ba, Y, La, Gd, Ce, Pr, Nd, Sm, Tb, Dy or Er oxide or their carbonates or nitrates as raw materials, and weigh the raw materials according to the structural formula composition and stoichiometric ratio of the materials; stir and mix the raw materials thoroughly, place them in the air for burning, and burn the mixed powder The temperature is 900-1550°C, and the burning time is 2-12 hours; after grinding and screening, it is made into rare earth-activated red phosphor.
Description
One, technical field
The present invention relates to a kind of rare earth red fluorescent powder and manufacture method thereof.
Two, background technology
Reported first in 1997 with Y
3Al
5O
12: Ce
3+(YAG:Ce) yellow emission fluorescence is as light-converting material, the white light LEDs that combines with the GaN blue-ray LED, because it has miniaturization, long lifetime, no mercury and advantage such as energy-conservation, thus be described as with surmount incandescent light, luminescent lamp and HID lamp the 4th generation lighting source.5998925 couples of YAG:Ce of United States Patent (USP) Y/Gd than and Al/Ga than aspect adjust and optimize.Up to the present, the luminous efficiency of the white light LEDs of blue led and YAG phosphor combination has surpassed 100lm/W, has surpassed the luminous efficiency of luminescent lamp.
Yet still there is its inherent defective in the high-brightness white-light LED that combines with the sodium yellow of the blue light of blue led and YAG fluorescent material using with general place and general lighting field: lack red light and cause the bad problem of color developing.
In order to address this problem, the someone has proposed to add the method for red fluorescence powder to improve the purpose of colour rendering index (Ra) in YAG fluorescent material.Patent WO01/24229A2 has proposed blue-light excited alkaline earth sulfide series phosphor powder, but because the luminous efficiency of sulphide fluorescent material is very low, although can be after adding so that colour rendering index makes moderate progress, but can cause the remarkable decline of the lumen brightness of white light LEDs, simultaneously because the poor chemical stability of sulphide fluorescent material, rapid decay can take place in its luminous efficiency in the working process, is difficult to satisfy the actual needs that use.
Meanwhile, people transfer to the emphasis of research on the three primary colours white light LEDs gradually, and near the LED efficient of the InGaN system the near-ultraviolet light 400nm is very high at present, can be applied to the White-light LED illumination of three primary colours.It is found that when 405nm, its external quantum efficiency reaches 43%.In this case, the three primary colours white light LEDs wants to develop to the direction of high light efficiency, then must further improve the transformation efficiency of red, green, blue three primary colors fluorescent powder when excited target.For this reason, the new fluorescent material of research then seems particularly important.And present known red fluorescence powder Y
2O
2S:Eu
3+Its transformation efficiency this shows that far below green and blue colour fluorescent powder this development for three-primary color LED is a bottleneck when using.So, demand researching and developing the red fluorescence material that makes new advances urgently.
The present invention adds the crystal field that other elements are regulated fluorescent material simultaneously by adding rare earth element as activator in alkaline-earth silicate in matrix, further improve the luminosity of fluorescent material, has obtained a kind of red fluorescence powder of novel light-emitting excellent performance.
Three, summary of the invention
The present invention is directed to above-mentioned technical problem, a kind of silicate red fluorescence powder of activated by rare earth elements is provided, have good luminous property, chemical stability and job stability; And provide a kind of preparation technology's method of above-mentioned fluorescent material.
Technical solution of the present invention is: material structure formula of the present invention is M
aN
bSi
cO
(2c+a+3b/2): Eu
x, R
yWherein, M is at least a among Mg, Ca, Sr or the Ba, 0.05＜a＜3.0; N is at least a among Y, La, the Gd, 0＜b＜5.0; R is at least a among Ce, Pr, Nd, Sm, Tb, Dy or the Er; 1.0＜c＜4.0; 0.001＜x＜5; 0.0001＜y＜0.5.
The manufacture method of rare earth red fluorescent powder of the present invention comprises the steps:
(1) is raw material with the oxide compound of Si, Mg, Ca, Sr, Ba, Y, La, Gd, Ce, Pr, Nd, Sm, Tb, Dy or Er or their corresponding carbonate or nitrate, takes by weighing described raw material according to above-mentioned structural formula and stoichiometric ratio;
(2) with the abundant mixing of each raw material stirring, place the air calcination, the calcination temperature of mixing powder is 900～1550 ℃, and calcination time is 2～12h;
(3) powder agglomates after will burning till grinds, washing, and oven dry after the screening, is promptly made rare-earth activated red fluorescence powder.
The present invention can be widely used in white light LEDs by the fluorescent material excellent performance that aforesaid method obtains.Rare earth red fluorescent powder provided by the invention has the following advantages: (1) the invention provides new europium and the coactivated silicate red fluorescence powder of other rare earth elements; By other rare earth elements that mix, utilize doped with rare-earth elements to effective absorption of exciting light and to the transmission ofenergy of Eu, promoted the absorption of fluorescent material to excitation energy, effectively improved the emissive porwer of fluorescent material; (2) with the matrix of silicate as fluorescent material, chemical property is stable; This fluorescent material manufacture method is simple, and easy handling is pollution-free, cost is low.The resulting red fluorescence powder of the present invention can be used for ultraviolet LED, constitutes three primary colors fluorescent powder with green and blue colour fluorescent powder, sends white light under ultraviolet excitation, satisfies the needs of illumination.
Four, description of drawings
Fig. 1 is Ca
0.52Si
3O
6.76: Eu
0.24, Tb
0.0024Emmission spectrum.
Fig. 2 is Ca
0.52Si
3O
6.76: Eu
0.24, Tb
0.0024Excitation spectrum.
Fig. 3 is Ca
0.55Mg
0.087La
0.48Si
3O
8.32: Eu
0.24, Tb
0.019Emmission spectrum.
Fig. 4 is Ca
0.55Mg
0.087La
0.48Si
3O
8.32: Eu
0.24, Tb
0.019Excitation spectrum.
From Fig. 1～4 as can be seen, the fluorescent material that the present invention proposes can effectively be excited by the UV-light of 300～350nm wave band, and producing peak wavelength is the ruddiness of 605nm.Comparison diagram 1 and Fig. 3 are as can be seen, in matrix, add elements such as Mg, La, the excitation spectrum of fluorescent material and the peak position of emmission spectrum are not exerted an influence, but the intensity of emmission spectrum has had certain raising, this is because after having added elements such as Mg, La, can change the crystal field strength of fluorescent material, and then improve the energy transfer efficiency of fluorescent material matrix, finally make the luminous intensity of fluorescent material rise.
Five, embodiment
Embodiment 1:
The phosphor structure formula is M
aN
bSi
cO
(2c+a+3b/2): Eu
x, R
yWherein, M can be Mg, Ca, Sr or Ba, and a desirable 0.05,0.09,0.15,0.54,0.98,1.21,1.64,2.02,2.68,2.89; N can be Y, La, Gd; B can be 0.33,0.81, and 1.25,1.61,2.46,3.43,3.88,4.42,4.85; R can be Ce, Pr, Nd, Sm, Tb, Dy or Er; C can be 1.23,1.64, and 2.34,2.65,2.91,3.14,3.42,3.84; X can be 0.009,0.26, and 1.24,2.14,3.54,4.05,4.98; Y can be 0.0008,0.0074, and 0.012,0.064,0.091,0.16,0.24,0.35,0.48.
Structural formula according to above-mentioned fluorescent material, the manufacture method of fluorescent material comprises the steps: that (1) is raw material with the oxide compound of Si, Mg, Ca, Sr, Ba, Y, La, Gd, Sc, Ce, Pr, Nd, Sm, Tb, Dy or Er or their corresponding carbonate or nitrate, takes by weighing described raw material according to above-mentioned structural formula and stoichiometric ratio; (2) with the abundant mixing of each raw material stirring, place the air calcination, the calcination temperature of mixing powder can be 950,980, and 1050,1260,1320,1475 or 1525 ℃, calcination time can be 2,2.5, and 3,5,6,8,10 or 12h; (3) powder agglomates after will burning till grinds, washing, and oven dry after the screening, is promptly made rare-earth activated red fluorescence powder.
Embodiment 2:
Take by weighing CaCO
310.50g, Eu
2O
38.62g, Tb
4O
70.378g, SiO
237.54g it is pure that above raw material is top grade, with above raw material mix grinding evenly after, pack in the corundum crucible, calcination 3.5h under 1300 ℃ of conditions, again firing product being washed till pH with deionized water is 6.5～7.5, after the filtration, filter cake is dried under 120 ℃ of conditions, promptly obtain molecular formula and consist of: Ca
0.52Si
3O
6.76: Eu
0.24, Tb
0.0024, its emmission spectrum is seen Fig. 1.
Embodiment 3:
Take by weighing CaCO
39.48g, MgO0.61g, La
2O
313.54g, Eu
2O
37.15g, CeO
20.57g, SiO
231.42g it is pure that above raw material is top grade, with above raw material mix grinding evenly after, in the corundum crucible of packing into, calcination 3.5h under 1300 ℃ of conditions is washed till neutrality with firing product again, filters, and dries under 120 ℃ of conditions, promptly obtains molecular formula and consists of Ca
0.55Mg
0.087La
0.48Si
3O
8.32: Eu
0.24, Tb
0.019, its emmission spectrum is seen Fig. 3.
Embodiment 4:
Take by weighing CaCO
39.58g, SrCO
32.36g, Eu
2O
36.52g, CeO
20.97g, SiO
238.46g it is pure that above raw material is top grade, with above raw material mix grinding evenly after, in the corundum crucible of packing into, calcination 5h under 1250 ℃ of conditions is washed till neutrality with firing product again, filters, and dries under 120 ℃ of conditions, promptly obtains molecular formula and consists of Ca
0.45Sr
0.075Si
3O
7.53: Eu
0.35, Ce
0.028
Claims (4)
1. a rare earth red fluorescent powder is characterized in that structural formula is M
aN
bSi
cO
(2c+a+3b/2): Eu
x, R
yWherein, M is at least a among Mg, Ca, Sr or the Ba, 0.05＜a＜3.0; N is at least a among Y, La or the Gd, 0＜b＜5.0; R is at least a among Ce, Pr, Nd, Sm, Tb, Dy or the Er; 1.0＜c＜4.0; 0.001＜x＜5; 0.0001＜y＜0.5.
2. a method for preparing the described rare earth red fluorescent powder of claim 1 is characterized in that this method comprises the steps:
A. be raw material with the oxide compound of Si, Mg, Ca, Sr, Ba, Y, La, Gd, Ce, Pr, Nd, Sm, Tb, Dy or Er or their carbonate or nitrate, and form and stoichiometric ratio takes by weighing described raw material by the structural formula of the described material of claim 1;
B. with the abundant mixing of each raw material stirring, place the air calcination, the calcination temperature of mixing powder is 900～1550 ℃, and calcination time is 2～12h;
C. cooling after grind, screening, promptly make rare-earth activated red fluorescence powder.
3. a kind of method for preparing rare earth red fluorescent powder according to claim 2 is characterized in that preferred 1100～1350 ℃ of the calcination temperature of mixing powder.
4. a kind of method for preparing rare earth red fluorescent powder according to claim 2 is characterized in that the preferred 4～8h of calcination time of mixing powder.
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|---|---|---|---|
| CNB2007100197062A CN100415849C (en) | 2007-02-06 | 2007-02-06 | Rare earth red phosphor and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100197062A CN100415849C (en) | 2007-02-06 | 2007-02-06 | Rare earth red phosphor and manufacturing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101012375A true CN101012375A (en) | 2007-08-08 |
| CN100415849C CN100415849C (en) | 2008-09-03 |
Family
ID=38700104
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161887A (en) * | 2011-03-14 | 2011-08-24 | 中国计量学院 | Yellow silicate fluorescent powder excited by blue light and preparation method thereof |
| CN102471681A (en) * | 2009-07-11 | 2012-05-23 | 默克专利有限公司 | Co-doped silicooxynitrides |
| CN103612449A (en) * | 2013-11-15 | 2014-03-05 | 英利能源（中国）有限公司 | Insulating luminescent material, solar battery back plate comprising insulating luminescent material, and solar battery component |
| CN109370589A (en) * | 2018-11-08 | 2019-02-22 | 沈阳化工大学 | A kind of silicate-based spectrally tunable fluorescent material and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69215655T2 (en) * | 1992-01-07 | 1997-05-28 | Philips Electronics Nv | Low pressure mercury discharge lamp |
| CN1062581C (en) * | 1997-03-26 | 2001-02-28 | 肖志国 | Long persistence luminescent silicate material and its producing method |
| CN100454476C (en) * | 2003-12-16 | 2009-01-21 | 松下电器产业株式会社 | Plasma display device and manufacturing method thereof |
-
2007
- 2007-02-06 CN CNB2007100197062A patent/CN100415849C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102471681A (en) * | 2009-07-11 | 2012-05-23 | 默克专利有限公司 | Co-doped silicooxynitrides |
| CN102161887A (en) * | 2011-03-14 | 2011-08-24 | 中国计量学院 | Yellow silicate fluorescent powder excited by blue light and preparation method thereof |
| CN102161887B (en) * | 2011-03-14 | 2013-02-13 | 中国计量学院 | Yellow silicate fluorescent powder excited by blue light and preparation method thereof |
| CN103612449A (en) * | 2013-11-15 | 2014-03-05 | 英利能源（中国）有限公司 | Insulating luminescent material, solar battery back plate comprising insulating luminescent material, and solar battery component |
| CN109370589A (en) * | 2018-11-08 | 2019-02-22 | 沈阳化工大学 | A kind of silicate-based spectrally tunable fluorescent material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100415849C (en) | 2008-09-03 |
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Effective date of registration: 20100406 Address after: 211100 Jiangsu city of Nanjing Jiangning Science Park Road 69. Co-patentee after: Southeast University Patentee after: Jiangsu Borui Photoelectric Co., Ltd. Address before: 210008 No. 12 West Beijing Road, Jiangsu, Nanjing Co-patentee before: Southeast University Patentee before: Jiangsu Subute New Materials Co., Ltd. |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 211100 Building 5, No. 69, Liquan Road, Jiangning high tech Zone, Nanjing, Jiangsu Province Patentee after: Jiangsu Borui photoelectric Co.,Ltd. Patentee after: Southeast University Address before: No. 69, Liquan Road, Jiangning Science Park, Nanjing, Jiangsu 211100 Patentee before: JIANGSU BREE OPTRONICS Co.,Ltd. Patentee before: Southeast University |