CN1246420C - Luminescent powder in user for LED with GaN as base and preparing method - Google Patents
Luminescent powder in user for LED with GaN as base and preparing method Download PDFInfo
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- CN1246420C CN1246420C CN 200310111931 CN200310111931A CN1246420C CN 1246420 C CN1246420 C CN 1246420C CN 200310111931 CN200310111931 CN 200310111931 CN 200310111931 A CN200310111931 A CN 200310111931A CN 1246420 C CN1246420 C CN 1246420C
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- fluorescent material
- oxide
- gram
- carbonate
- fluorescent powder
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- 239000000843 powder Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052788 barium Inorganic materials 0.000 claims abstract description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 23
- 238000001354 calcination Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 19
- 208000035619 Back crushing Diseases 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 4
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000007789 gas Substances 0.000 abstract description 9
- 230000005284 excitation Effects 0.000 abstract description 2
- 239000012190 activator Substances 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 238000010671 solid-state reaction Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 229910052786 argon Inorganic materials 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 239000010431 corundum Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000012856 packing Methods 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 4
- 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 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The present invention relates to fluorescent powder for a GaN base light emitting diode (LED) and a preparation method thereof. The through formula of the fluorescent powder is (M<1-x>REx)AGa3S6O, wherein M represents elements selected from one or some of calcium, strontium or barium; A represents elements selected from one or some of La, Y or Gd; RE represents Eu<2+> or the comnination of the Eu<2+> and other activator ions; x is greater than or equal to 0.01, but is smaller than or equal to 1. The fluorescent powder has the preparation method that raw materials are accurately weighed according to the proportion of the general formula, and are porphyrized and uniformly mixed, the raw materials carry out solid-state reaction for one time or multiple times under the conditions of the hydrogen sulfide shielding gas atmosphere and the temperature of 800 DEG C to 1000 DEG C, and thus, the fluorescent powder is prepared. The fluorescent powder can send out light rays of 510 nm to 650 nm under the excitation of the light rays of 300 nm to 500 nm (particularly 400 nm and 470 nm), and is suitable to prepare green or white GaN base light emitting diodes. The preparation method is simple and convenient.
Description
Technical field
The present invention relates to fluorescent material that a kind of GaN based light-emitting diode uses and preparation method thereof.
Background technology
GaN based light-emitting diode LED (Light Emitting Diode) is a kind of novel luminescent device, it is little to have volume, life-span is long, save the energy and do not need to use the advantages such as mercury of contaminate environment, can be widely used on the various lighting installations, comprise indoor lamp, traffic lights, stop-light, street lamp, automobile taillight, indicator, brake lamp, outdoor jumbotron, display screen and billboard etc., gradually the function that replaces various bulbs can also be as the pilot lamp of various instrument.This novel light source will become the light source of new generation of 21 century, to energy-saving and environmental protection, improve aspects such as people's quality of life and all be significant.The fluorescent material that can be used for GaN based light-emitting diode LED at present is also few, as mixes yttrium aluminum garnet (YAG) the type fluorescent material of Ce, but because it is the white light LEDs that utilizes blue led and YAG type fluorescent material to be made by yellow, blue two mixture of colours, colour rendering index is not high.Existing purple pipe (UV-LED) the excited fluorescent powder that can be used for launching 400nm, common as the high-pressure mercury lamp phosphor, but these fluorescent material can't satisfy the needs of UV-LED on excitation wavelength.
Summary of the invention
The purpose of this invention is to provide a kind of can exciting and send down fluorescent material that GaN based light-emitting diode 500nm～560nm light, that be adapted to use in market uses and preparation method thereof at 300nm～500nm light.
The general formula of fluorescent material of the present invention is (M
1-xRE
x) AGa
3S
6O, wherein on behalf of one or more, M be selected from the element of calcium, strontium or barium; A represents one or more to be selected from La, Y or/and the element of Gd; RE represents Eu
2+Or Eu
2+And Tm
3+The ionic combination; 0.01≤x≤0.5.
The preparation method of fluorescent material of the present invention is as follows:
Adopt solid-phase synthesis, will contain oxide compound or the carbonate of M, the oxide compound that contains A, RE
2O
3And Ga
2O
3Press general formula (M
1-xRE
x) AGa
3S
6O expresses the mole proportioning that requires, and accurately weighing behind the porphyrize mixing, feeds hydrogen sulfide, and 800 ℃～1000 ℃ calcinations 2～4 hours, cooling back crushing screening obtained required fluorescent material.
In order to guarantee to react completely, can be after the calcination first time, calcination was ground evenly under similarity condition 2～4 hours in the cooling back again.
The oxide compound of M described in the invention described above method is generally: calcium oxide, strontium oxide are or/and barium oxide.The carbonate of described M is generally: lime carbonate, Strontium carbonate powder are or/and barium carbonate.The oxide compound of described A is generally: lanthanum trioxide, yttrium oxide are or/and gadolinium sesquioxide.Described RE
2O
3Be generally: europium sesquioxide is or/and trioxide.
Adopt the inventive method synthetic fluorescent material under 300nm～500nm light excites, to send 510nm～560nm light, being fit to the GaN based light-emitting diode uses, can be complementary required green emitting phosphor and yellow fluorescent powder when being used for the preparation of white light LEDs with UV-LED.Its synthetic method is simple and convenient in addition.
Description of drawings
Fig. 1 is embodiment 1 (Ca
0.96Eu
0.04) LaGa
3S
6The X-ray powder diffraction figure of O.
Fig. 2 is embodiment 2 (Sr
0.96Eu
0.04) YGa
3S
6Exciting light spectrogram (the λ of O
Em=540nm).
Fig. 3 is embodiment 2 (Sr
0.96Eu
0.04) YGa
3S
6Emmission spectrum figure (the λ of O
Ex=400nm).
Fig. 4 is embodiment 3 (Ca
0.5Eu
0.5) YGa
3S
6Emmission spectrum figure (the λ of O
Ex=470nm).
Embodiment
Embodiment one: (Ca
0.96Eu
0.04) LaGa
3S
6Synthesizing of O fluorescent material:
CaCO
3(analytical pure) 0.3844 gram;
La
2O
3(99.9%) 0.6516 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0282 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations of S atmosphere 4 hours, cooling back were ground evenly under similarity condition calcination 2 hours again, and cooling back crushing screening obtains outward appearance and is the xanchromatic powder, sends gold-tinted under 250nm-500nm light excites, and peak wavelength is 560nm.Its X-ray powder diffraction figure sees Fig. 1.
Embodiment two: (Sr
0.96Eu
0.04) YGa
3S
6Synthesizing of O fluorescent material:
SrCO
3(analytical pure) 0.5668 gram;
Y
2O
3(99.9%) 0.4516 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0282 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 2 hours in the S atmosphere, and calcination was ground evenly under similarity condition 3 hours in the cooling back again, and cooling back crushing screening obtains the greeny powder of outward appearance, sends green glow under 250nm-500nm light excites, and peak wavelength is 540nm.Its exciting light spectrogram (λ
Em=540nm) see Fig. 2, emmission spectrum (λ
Ex=400nm) see Fig. 3.
Embodiment three: (Ba
0.96Eu
0.04) YGa
3S
6Synthesizing of O fluorescent material:
BaCO
3(analytical pure) 0.7894 gram;
Y
2O
3(99.9%) 0.4336 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0282 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 2 hours in the S atmosphere, and calcination was ground evenly under similarity condition 2 hours in the cooling back again, and cooling back crushing screening obtains outward appearance and is jade-green powder, sends blue green light under 250nm-500nm light excites, and peak wavelength is 510nm.
Embodiment four: (Ca
0.5Eu
0.5) YGa
3S
6Synthesizing of O fluorescent material:
CaCO
3(analytical pure) 0.2002 gram;
Y
2O
3(99.9%) 0.4516 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.3520 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 2 hours in the S atmosphere, and cooling back crushing screening obtains outward appearance and is the xanchromatic powder, sends gold-tinted under 250nm-500nm light excites, and peak wavelength is 560nm.Emmission spectrum (λ
Ex=470nm) see Fig. 4.
Embodiment five: (Sr
0.94Eu
0.06) GdGa
3S
6Synthesizing of O fluorescent material:
SrCO
3(analytical pure) 0.5550 gram;
Gd
2O
3(99.9%) 0.7250 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0422 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 2 hours in the S atmosphere, and calcination was ground evenly under similarity condition 2 hours in the cooling back again, and cooling back crushing screening obtains the greeny powder of outward appearance, sends green glow under 250nm-500nm light excites, and peak wavelength is 540nm.
Embodiment six: (Sr
0.94Eu
0.02Tm
0.04) GdGa
3S
6Synthesizing of O fluorescent material:
SrCO
3(analytical pure) 0.6939 gram;
Gd
2O
3(99.9%) 0.9063 gram;
Ga
2O
3(99.9%) 1.4058 gram;
Eu
2O
3(99.9%) 0.0176 gram;
Tm
2O
3(99.9%) 0.0385 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 4 hours in the S atmosphere, and calcination was ground evenly under similarity condition 4 hours in the cooling back again, and cooling back crushing screening obtains the greeny powder of outward appearance, sends green glow under 250nm-500nm light excites, and peak wavelength is 538nm.
Embodiment seven: (Ca
0.56Sr
0.4Eu
0.04) GdGa
3S
6Synthesizing of O fluorescent material:
SrCO
3(analytical pure) 0.2362 gram;
CaCO
3(analytical pure) 0.2402 gram;
Gd
2O
3(99.9%) 0.7250 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0282 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 4 hours in the S atmosphere, and calcination was ground evenly under similarity condition 4 hours in the cooling back again, and cooling back crushing screening obtains the greeny powder of outward appearance, sends yellow green light under 250nm-500nm light excites, and peak wavelength is 555nm.
Embodiment eight: (Ba
0.4Sr
0.56Eu
0.04) GdGa
3S
6Synthesizing of O fluorescent material:
SrCO
3(analytical pure) 0.3544 gram;
BaCO
3(analytical pure) 0.3158 gram;
Gd
2O
3(99.9%) 0.7250 gram;
Ga
2O
3(99.9%) 1.1246 gram;
Eu
2O
3(99.9%) 0.0282 gram.
Above-mentioned raw materials ground mixing in agate mortar after, in the corundum crucible of packing into, feed high pure nitrogen or argon gas before the heating earlier the air in the silica tube is caught up with only, then at H
2900 ℃ of following calcinations are 4 hours in the S atmosphere, and calcination was ground evenly under similarity condition 2 hours in the cooling back again, and cooling back crushing screening obtains the greeny powder of outward appearance, sends blue green light under 250nm-500nm light excites, and peak wavelength is 530nm.
Claims (7)
1. fluorescent material that the GaN based light-emitting diode is used, the general formula that it is characterized in that this fluorescent material is (M
1-xRE
x) AGa
3S
6O, wherein on behalf of one or more, M be selected from the element of calcium, strontium, barium; On behalf of one or more, A be selected from the element of La, Y, Gd; RE represents Eu
2+Or Eu
2+And Tm
3+The ionic combination; 0.01≤x≤0.5.
2. the preparation method of the fluorescent material used of a GaN based light-emitting diode as claimed in claim 1 adopts solid-phase synthesis, will contain oxide compound or the carbonate of M, the oxide compound that contains A, RE
2O
3And Ga
2O
3Press general formula (M
1-xRE
x) AGa
3S
6O expresses the mole proportioning that requires, and accurately weighing behind the porphyrize mixing, feeds hydrogen sulfide, and 800 ℃～1000 ℃ calcinations 2～4 hours, cooling back crushing screening obtained required fluorescent material.
3. in accordance with the method for claim 2, it is characterized in that after the calcination first time that calcination was ground evenly under similarity condition 2～4 hours in cooling back again.
4. according to claim 2 or 3 described methods, it is characterized in that the oxide compound of described M is: calcium oxide, strontium oxide are or/and barium oxide.
5. according to claim 2 or 3 described methods, it is characterized in that the carbonate of described M is: lime carbonate, Strontium carbonate powder are or/and barium carbonate.
6. according to claim 2 or 3 described methods, it is characterized in that the oxide compound of described A is: lanthanum trioxide, yttrium oxide are or/and gadolinium sesquioxide.
7. according to claim 2 or 3 described methods, it is characterized in that described RE
2O
3For: europium sesquioxide is or/and trioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111931 CN1246420C (en) | 2003-10-29 | 2003-10-29 | Luminescent powder in user for LED with GaN as base and preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111931 CN1246420C (en) | 2003-10-29 | 2003-10-29 | Luminescent powder in user for LED with GaN as base and preparing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1539918A CN1539918A (en) | 2004-10-27 |
| CN1246420C true CN1246420C (en) | 2006-03-22 |
Family
ID=34336305
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310111931 Expired - Fee Related CN1246420C (en) | 2003-10-29 | 2003-10-29 | Luminescent powder in user for LED with GaN as base and preparing method |
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| Country | Link |
|---|---|
| CN (1) | CN1246420C (en) |
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|---|---|---|---|---|
| CN105713611A (en) * | 2016-01-20 | 2016-06-29 | 济宁学院 | Rare-earth light conversion fluorescent powder and preparation method thereof |
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2003
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| Publication number | Publication date |
|---|---|
| CN1539918A (en) | 2004-10-27 |
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Granted publication date: 20060322 Termination date: 20091130 |