CN100367523C - White LED parts, mono-component dual-wavelength rare earth fluoresent powder for fluorescence conversion therefor and preparation method thereof - Google Patents
White LED parts, mono-component dual-wavelength rare earth fluoresent powder for fluorescence conversion therefor and preparation method thereof Download PDFInfo
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- CN100367523C CN100367523C CNB2005101206182A CN200510120618A CN100367523C CN 100367523 C CN100367523 C CN 100367523C CN B2005101206182 A CNB2005101206182 A CN B2005101206182A CN 200510120618 A CN200510120618 A CN 200510120618A CN 100367523 C CN100367523 C CN 100367523C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 title abstract description 24
- 238000006243 chemical reaction Methods 0.000 title abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 239000004065 semiconductor Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 30
- 238000005245 sintering Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 239000003610 charcoal Substances 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000005864 Sulphur Substances 0.000 claims description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 230000005284 excitation Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract 3
- 108010043121 Green Fluorescent Proteins Proteins 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 230000009977 dual effect Effects 0.000 abstract 1
- 241001025261 Neoraja caerulea Species 0.000 description 14
- 239000002002 slurry Substances 0.000 description 14
- 238000005538 encapsulation Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 10
- 238000000465 moulding Methods 0.000 description 7
- 238000000576 coating method Methods 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 4
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910005224 Ga2O Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Led Device Packages (AREA)
Abstract
The present invention relates to the LED field, more specifically white light LED parts, mono-component dual-wavelength rare earth fluorescent powder for fluorescence conversion thereof and a preparation method thereof. The white light LED parts comprise a GaN-base inorganic semiconductor LED crystal grain driven by a voltage to emit blue visible light, and the mono-component dual-wavelength rare earth fluorescent powder to at least partially absorb the blue light emitted by the GaN-base inorganic semiconductor LED crystal grain and to convert the blue light into at least partial yellow light and red light; at last, the white light is generated by mixing the residual blue light of the LED crystal grain and the yellow light and the red light generated by the conversion of the fluorescent powder. The present invention overcomes the defect of blue light LED plus YAG in traditional technique which is short of the red light, can adjust the white light more conveniently than other blue light LED plus green fluorescent powder plus red fluorescent powder technique. The fluorescent powder provided by the present invention has the advantages of mono-component, dual emission wavelength, simple preparing process, is applicable in blue light LED excitation and is applied to the white light LED, etc.
Description
Technical field
The present invention relates to the LED field, be specifically related to a kind of white light LED part and fluorescence thereof conversion one-component dual-wavelength rare earth fluorescent material and preparation method thereof.
Background technology
Along with the breakthrough of the key technology area of efficient purple light and blue light-emitting diode, white light LEDs becomes the focus that people pay close attention to day by day.At present, the technical scheme that obtains white light LEDs mainly is divided into led chip combination and fluorescence conversion, and the latter is the mainstream technology in present white light LEDs field.Wherein, the white light LEDs of industrialization mainly by blue-light LED chip and fluorescent material Y
3Al
5O
12: Ce
3+(YAG:Ce) form, i.e. " blue-ray LED+YAG " white light version, its main technology of preparing is fluorescent material to be mixed in certain proportion with colloid be made into slurries, then by applying or some glue mode, directly or indirectly slurries are coated in the blue-ray LED grain surface, at last, curing molding at a certain temperature.The cardinal principle that this technical scheme produces white light is: the blue light that sends when LED crystal grain is during by resin, the part blue light is by the absorption of the YAG:Ce fluorescent powder grain in the light path and be converted to yellow visible light, another part blue light is not then owing to have the YAG:Ce fluorescent powder grain in the light path, so directly see through resin the fluorescence conversion does not take place, finally the gold-tinted after blue light that is not converted and the conversion produces white light by mixing.Yet, because the white light LED part spectral power distribution lacks red long wave visible light part, had a strong impact on the quality of white light in this technology.
Summary of the invention
The objective of the invention is to lack red long wave visible light part owing to spectral power distribution, thereby have a strong impact on the problem of white light quality, provide a kind of LED device of high white light quality, to overcome this problem in order to overcome existing white light LED part.
Another object of the present invention provides a kind of one-component dual-wavelength rare earth fluorescent material, and it can launch gold-tinted and ruddiness simultaneously.
Further purpose of the present invention provides the preparation method of above-mentioned one-component dual-wavelength rare earth fluorescent material.
The invention provides a kind of white light LED part, comprise blue-light LED chip and fluorescent material, described blue-light LED chip is a GaN base inorganic semiconductor LED crystal grain, and described fluorescent material is one-component dual-wavelength rare earth fluorescent material.Wherein, GaN base inorganic semiconductor LED crystal grain is launched blue visible light under driven, and its peak wavelength scope is 440～48nm; Fluorescent RE powder partially absorbs the blue light that GaN base inorganic semiconductor LED crystal grain sends at least, and converts thereof into to small part gold-tinted and ruddiness, and is last, and gold-tinted and ruddiness mixing that LED crystal grain residue blue light and fluorescent material conversion are produced produce white light.
The chemical composition expression of above-mentioned one-component dual-wavelength rare earth fluorescent material is:
(Ca
1+x-y-zEu
yRE
z)Ga
2S
4+x
Wherein RE is selected from a kind of element among Ce, Pr, Nd, Sm, Tb, Dy, Ho, Er and the Tm; 0.1≤x≤0.8,0.01≤y≤0.20,0≤z≤0.18;
The concrete preparation method of above-mentioned one-component dual-wavelength rare earth fluorescent material is as follows: the raw materials such as simple substance, compound or salt that take by weighing respective element according to above-mentioned chemical composition expression, after mixture grinds and mixes, under reducing atmosphere, 700～1100 ℃ of sintering 5～10 hours promptly obtain product.Described reducing atmosphere is hydrogen sulfide, curing charcoal, nitrogen or hydrogen and hydrogen sulfide gaseous mixture or charcoal and sulphur.
Gained one-component dual-wavelength rare earth fluorescent material mixed with certain proportion with colloid be made into slurries, by applying or some glue mode, directly or indirectly slurries are coated in the blue-ray LED grain surface then, last, curing molding promptly gets white light LED part at a certain temperature.
Compared with prior art, the present invention has following beneficial effect:
1, to have an one-component, two emission wavelength, preparation technology simple and be applicable to that blue-ray LED excites and be applied to advantage such as white light LEDs for fluorescent RE powder provided by the invention.
2, white light LED part provided by the invention is a kind of non-" blue-ray LED+YAG " white light technology.Compare with tradition " blue-ray LED+YAG " technology, comprised blue light, gold-tinted and ruddiness in this device white-light spectrum Energy distribution, remedied the deficiency of tradition " blue-ray LED+YAG " technology shortage ruddiness.Simultaneously, compare,, make that the regulation and control of white light are simpler owing to only need to use a kind of fluorescent material and blue-ray LED combination with other " blue-ray LED+green emitting phosphor+red fluorescence powder " technology.
Description of drawings
Fig. 1 is fluorescent material (Ca of the present invention
1.09Eu
0.06) Ga
2S
4.6Emission spectrum figure;
Fig. 2 is fluorescent material (Ca
1.09Eu
0.06) Ga
2S
4.6The spectral distribution graph of the white light LED part of encapsulation;
Fig. 3 is fluorescent material (Ca
1.09Eu
0.06) Ga
2S
4.6The chromatic diagram of the white light LED part of encapsulation.
Wherein, the excitation wavelength of Fig. 1 is 460nm; Asterisk among Fig. 3 is a sample device white point.
Embodiment
Implement 1:
(Ca
1.09Eu
0.01) Ga
2S
4.1(x=0.1, y=0.01, z=0) preparation; Take by weighing oxide respectively
CaCO
3：0.5450g
Ga
2O
3：0.9373g
Eu
2O
3：0.0088g
After mixture ground and mix, in hydrogen sulfide atmosphere, 700 ℃ of sintering 10 hours promptly obtained product.
White light LEDs encapsulates: gained fluorescent material mixed at 1: 5 being made into slurries with epoxy resin according to weight ratio, by coating method, directly slurries is coated in the blue-ray LED grain surface then, and last, at 150 ℃ of following curing moldings, promptly get white light LED part.Fluorescent RE powder (Ca
1.09Eu
0.01) Ga
2S
4.1Absorb the light of blue-light LED chip, and launch gold-tinted and ruddiness.
Implement 2:
(Ca
1.42Eu
0.2Ce
0.18) Ga
2S
4.8(x=0.8, y=0.2, z=0.18) preparation: take by weighing oxide respectively
CaCO
3：0.71g
Ga
2O
3：0.9373g
Eu
2O
3：0.1760g
CeO
2：0.1549g
After mixture ground and mix, in curing charcoal atmosphere, 900 ℃ of sintering 8 hours promptly obtained product.
The white light LEDs encapsulation; Gained fluorescent material mixed at 1: 6 being made into slurries with epoxy resin according to weight ratio, by coating method, directly slurries are coated in the blue-ray LED grain surface then, last, at 150 ℃ of following curing moldings, promptly get white light LED part.Fluorescent RE powder (Ca
1.42Eu
0.2Ce
0.18) Ga
2S
4.8Absorb the light of blue-light LED chip, and launch gold-tinted and ruddiness.
Implement 3:
(Ca
1.17Eu
0.08Nd
0.05) Ga
2S
4.3(x=0.3, y=0.08, z=0.05) preparation: take by weighing oxide respectively
CaCO
3：0.5850g
Ga
2O
3：0.9373g
Eu
2O
3：0.0704g
Nd
2O
3：0.0421g
After mixture ground and mix, in nitrogen and hydrogen sulfide mixed atmosphere, 1100 ℃ of sintering 5 hours promptly obtained product.
White light LEDs encapsulates: gained fluorescent material mixed at 1: 7 being made into slurries with epoxy resin according to weight ratio, by coating method, directly slurries is coated in the blue-ray LED grain surface then, and last, at 150 ℃ of following curing moldings, promptly get white light LED part.Fluorescent RE powder (Ca
1.17Eu
0.08Nd
0.05) Ga
2S
4.3Absorb the light of blue-light LED chip, and launch gold-tinted, orange light and ruddiness.
Implement 4:
(Ca
1.54Eu
0.06) Ga
2S
4.6(x=0.6, y=0.06, z=0) preparation: take by weighing oxide respectively
CaCO
3：0.7700g
Ga
2O
3：0.9373g
Eu
2O
3：0.0528g
After mixture ground and mix, in hydrogen and hydrogen sulfide mixed atmosphere, 800 ℃ of sintering 4 hours promptly obtained product.
White light LEDs encapsulates: gained fluorescent material mixed at 1: 5 being made into slurries with epoxy resin according to weight ratio, by coating method, directly slurries is coated in the blue-ray LED grain surface then, and last, at 150 ℃ of following curing moldings, promptly get white light LED part.Fluorescent RE powder (Ca
1.54Eu
0.06) Ga
2S
4.6Absorb the light of blue-light LED chip, and launch gold-tinted and ruddiness.
Implement 5:
(Ca
1.32Eu
0.05Pr
0.03) Ga
2S
4.4(x=0.4, y=0.05, z=0.03) preparation: take by weighing oxide respectively
CaCO
3：0.7700g
Ga2O
3：0.9373g
Eu
2O
3：0.0440g
Pr
6O
11：0.0255g
After mixture ground and mix, in hydrogen sulfide atmosphere, 850 ℃ of sintering 4 hours promptly obtained product.
White light LEDs encapsulates: gained fluorescent material mixed at 1: 8 being made into slurries with epoxy resin according to weight ratio, by coating method, directly slurries is coated in the blue-ray LED grain surface then, and last, at 150 ℃ of following curing moldings, promptly get white light LED part.Fluorescent RE powder (Ca
1.32Eu
0.05Pr
0.03) Ga
2S
4.4Absorb the light of blue-light LED chip, and launch gold-tinted and ruddiness.
Implement 6:
(Ca
1.41Eu
0.05Sm
0.04) Ga
2S
4.5(x=0.5, y=0.05, z=0.04) preparation: take by weighing oxide respectively
CaCO
3：0.7050g
Ga
2O
3：0.9373g
Eu
2O
3：0.0440g
Sm
2O
3：0.0349g
After mixture ground and mix, in charcoal and sulphur atmosphere, 850 ℃ of sintering 4 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.41Eu
0.05Sm
0.04) Ga
2S
4.5Absorb the light of blue-light LED chip, and launch gold-tinted, orange red light and ruddiness.
Implement 7:
(Ca
1.09Eu
0.07Tb
0.04) Ga
2S
4.2(x=0.2, y=0.07, z=0.04) preparation: take by weighing oxide respectively
CaCO
3：0.5450g
Ga
2O
3：0.9373g
Eu
2O
3：0.0616g
Tb
4O
7：0.0374g
After mixture ground and mix, in charcoal and sulphur atmosphere, 1000 ℃ of sintering 4 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.09Eu
0.07Tb
0.04) Ga
2S
4.2Absorb the light of blue-light LED chip, and launch blue green light, gold-tinted and ruddiness.
Implement 8:
(Ca
1.19Eu
0.07Dy
0.04) Ga
2S
4.3(x=0.3, y=0.07, z=0.04) preparation: take by weighing oxide respectively
CaCO
3：0.5950g
Ga
2O
3：0.9373g
Eu
2O
3：0.0616g
Dy
2O
3：0.0373g
After mixture ground and mix, in charcoal and sulphur atmosphere, 950 ℃ of sintering 6 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.19Eu
0.07Dy
0.04) Ga
2S
4.3Absorb the light of blue-light LED chip, and launch blue light, gold-tinted and ruddiness.
Implement 9:
(Ca
1.3Eu
0.05Ho
0.05) Ga
2S
4.4(x=0.4, y=0.05, z=0.05) preparation: take by weighing oxide respectively
CaCO
3：0.5950g
Ga
2O
3：0.9373g
Eu
2O
3：0.0440g
Ho
2O
3：0.0472g
After mixture ground and mix, in charcoal and sulphur atmosphere, 850 ℃ of sintering 8 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.3Eu
0.05Ho
0.05) Ga
2S
4.4Absorb the light of blue-light LED chip, and launch green glow, gold-tinted and ruddiness.
Implement 10:
(Ca
1.29Eu
0.05Er
0.06) Ga
2S
4.4(x=0.4, y=0.05, z=0.06) preparation: take by weighing oxide respectively
CaCO
3：0.6450g
Ga
2O
3：0.9373g
Eu
2O
3：0.0440g
Er
2O
3：0.0574g
After mixture ground and mix, in charcoal and sulphur atmosphere, 850 ℃ of sintering 8 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.29Eu
0.05Er
0.06) Ga
2S
4.4Absorb the light of basket light led chip, and launch gold-tinted and ruddiness.
Implement 11:
(Ca
1.46Eu
0.08Tm
0.06) Ga
2S
4.6(x=0.6, y=0.08, z=0.06) preparation: take by weighing oxide respectively
CaCO
3：0.6450g
Ga
2O
3：0.9373g
Eu
2O
3：0.0440g
Tm
2O
3：0.0579g
After mixture ground and mix, in charcoal and sulphur atmosphere, 850 ℃ of sintering 8 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.46Eu
0.08Tm
0.06) Ga
2S
4.6Absorb the light of blue-light LED chip, and launch blue light, gold-tinted and ruddiness.
Implement 12:
(Ca
1.46Eu
0.08Tm
0.06) Ga
2S
4.6(x=0.6, y=0.08, x=0.06) preparation: take by weighing the simple substance oxide respectively
Ca：0.2920g
Ga：0.6973g
Eu：0.0608g
Tm：0.0507g
After mixture ground and mix, in charcoal and sulphur atmosphere, 850 ℃ of sintering 8 hours promptly obtained product.
White light LEDs encapsulation: with embodiment 1.Fluorescent RE powder (Ca
1.46Eu
0.08Tm
0.06) Ga
2S
4.6Absorb the light of blue-light LED chip, and launch blue light, gold-tinted and ruddiness.
Claims (5)
1. white light LED part, comprise blue-light LED chip and fluorescent material, described blue-light LED chip is a GaN base inorganic semiconductor LED crystal grain, it is characterized in that described fluorescent material is one-component dual-wavelength rare earth fluorescent material, and the chemical composition expression of one-component dual-wavelength rare earth fluorescent material is:
(Ca
1+x-y-zEu
yRE
z)Ga
2S
4+x
Wherein RE is selected from a kind of element among Ce, Pr, Nd, Sm, Tb, Dy, Ho, Er and the Tm; 0.1≤x≤0.8,0.01≤y≤0.20,0≤z≤0.18.
2. white light LED part as claimed in claim 1 is characterized in that light to the small part of two or more desirable wave bands of being produced behind the described one-component dual-wavelength rare earth fluorescent material converting blue light is gold-tinted and ruddiness.
3. one-component dual-wavelength rare earth fluorescent material is characterized in that the chemical composition expression is:
(Ca
1+x-y-zEu
yRE
z)Ga
2S
4+x
Wherein RE is selected from a kind of element among Ce, Pr, Nd, Sm, Tb, Dy, Ho, Er and the Tm; 0.1≤x≤0.8,0.01≤y≤0.20,0≤z≤0.18.
4. the preparation method of the described one-component dual-wavelength rare earth of claim 3 fluorescent material, the steps include: that the chemical composition expression according to this fluorescent material takes by weighing the simple substance or the compound of respective element, after grinding and mixing, under reducing atmosphere, 700～1100 ℃ of sintering 5～10 hours promptly obtain product.
5. preparation method as claimed in claim 4 is characterized in that described reducing atmosphere is hydrogen sulfide, carbon disulfide, nitrogen or hydrogen and hydrogen sulfide gaseous mixture or charcoal and sulphur.
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| CN100542693C (en) * | 2006-10-27 | 2009-09-23 | 中山大学 | A kind of LED excited fluorescent powder coating method that is used for |
| CN101958316B (en) * | 2010-07-20 | 2013-01-16 | 上海亚明灯泡厂有限公司 | LED integrated packaging power source module |
| CN108998028B (en) * | 2018-08-29 | 2021-02-12 | 东台市天源光电科技有限公司 | Sulfide green fluorescent powder, preparation method thereof and light-emitting device adopting fluorescent powder |
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| 稀土发光材料在固体白光LED照明中的应用. 苏锵，吴昊等.中国稀土学报，第23卷第5期. 2005 * |
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