CN108913127A - A kind of narrowband green light fluorescent powder and preparation method thereof and White LED light-emitting device - Google Patents
A kind of narrowband green light fluorescent powder and preparation method thereof and White LED light-emitting device Download PDFInfo
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- CN108913127A CN108913127A CN201810748727.6A CN201810748727A CN108913127A CN 108913127 A CN108913127 A CN 108913127A CN 201810748727 A CN201810748727 A CN 201810748727A CN 108913127 A CN108913127 A CN 108913127A
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910020440 K2SiF6 Inorganic materials 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims 2
- 239000000463 material Substances 0.000 claims 1
- 230000005284 excitation Effects 0.000 abstract description 10
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 4
- 238000010791 quenching Methods 0.000 abstract description 4
- 230000000171 quenching effect Effects 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 3
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 2
- 150000001340 alkali metals Chemical class 0.000 abstract description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract description 2
- 150000001342 alkaline earth metals Chemical class 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 230000003407 synthetizing effect Effects 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 150000004645 aluminates Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000002284 excitation--emission spectrum Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
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Abstract
A kind of narrowband green light fluorescent powder and preparation method and LED light emission device for display device, belongs to phosphor field.Green light fluorescent powder chemical constitution formula is RbxLiySiOz:aEu2+, preparation method is：The raw material of synthetizing phosphor powder use the oxide of the carbonate of various alkali metal, the carbonate of alkaline-earth metal, silica or silicic acid, rare earth element.According to molecular formula RbxLiySiOz:aEu2+The ratio of middle each element carries out accurately weighing raw material, and ground and mixed is uniform, grinding is taken out after 400-550 DEG C of pre-burning 2-6h of batch-type furnace, natural cooling, then in N2/H2It carries out heat preservation 3-12h under atmosphere at 600-1000 DEG C, grinds, washs after cooling, being sieved and the post-processing of baking step.Green light fluorescent powder luminous intensity in narrowband of the present invention is high, excitation purity is high, halfwidth is small, temperature quenching characteristic is good, excites scope is wide, it is combined with narrowband red light fluorescent powder in the prior art, it can get a series of efficient white light under blue light excitation, it can satisfy the demand of field of liquid crystal display, while having the advantages that gamut range is wide, color temperature uniformity is good and is not susceptible to light decay.
Description
Technical field
The invention belongs to phosphor technical fields；Be related to a kind of narrowband green light fluorescent powder for display device and
Preparation method and White LED light-emitting device.
Background technique
In recent years, white light LEDs have the advantages such as green, environmental protection, long-life as novel solid state light emitter, illuminate with
Display field, which has been obtained, to be widely applied.
The implementation of white light LEDs is mainly chip and phosphor combination at present：(1) blue-light LED chip and yellow fluorescence
Powder composition；(2) blue-light LED chip and red green fluorescent powder form；(3) near ultraviolet LED chip and red-green-blue fluorescent powder
Composition.In lighting area, as red, green, blue three primary colors fluorescent powder needed for white light LEDs synthesis, the performance of single paragraph fluorescent powder
(luminous intensity, peak wavelength, halfwidth etc.) directly determines the light efficiency and colour rendering index of synthesis white light LED part；In liquid crystal
During the realization for showing LED backlight, the performance (luminous intensity, chromaticity coordinates, peak wavelength, halfwidth) of fluorescent powder is directly certainly
Determine the gamut range of liquid crystal display.Therefore, the luminescent properties of fluorescent powder directly affect and determine the performance of white light LED part.
Currently, being applied to the fluorescent powder of white light LEDs mainly has aluminate, silicate and nitride/nitrogen oxides, fluoride
Four big systems.Wherein, with the aluminate YAG of garnet structure:Ce has luminous efficiency height, thermal stability good and chemical structure
The advantages that stablizing is presently the most classical liquid crystal display yellow fluorescent powder.And the green fluorescence of low and middle-end liquid crystal display
Powder is mainly based on silicate fluorescent powder, and the green emitting phosphor of high-end display is with β-sialon:Based on Eu nitrogen oxides；Illumination
Red fluorescence powder is with MAlSiN3:Based on Eu (one or more in M Ca, Sr, Ba), and liquid crystal display LED backlight is used
Red fluorescence powder with K2SiF6:Based on Mn.For the gamut range for improving liquid crystal display, it is badly in need of at present than β-sialon:Eu half is high
Wide smaller, the purer narrowband green light fluorescent powder of excitation purity.
Summary of the invention
One of the object of the invention is there is provided a kind of luminous intensity height, excitation purity height, and halfwidth is small, temperature quenching characteristic is good
Narrowband green light fluorescent powder for display device good, excites scope is wide.
The second object of the present invention is to providing, a kind of gamut range is big, color temperature uniformity is good and is not susceptible to the white light of light decay
LED light emission device.
To achieve the above object, the present invention for display device narrowband green light fluorescent powder using silicate as matrix, with two
Valence Eu is activator, and the molecular formula of the fluorescent powder is：RbxLiySiOz:aEu2+, wherein 3 < x+y < 5,3.8≤z≤4.2,
0.005≤a≤0.2。
Preferably, the present invention is Rb for the chemical constitution formula of the narrowband green light fluorescent powder of display devicexLiySiOz:aEu2 +, wherein 3.5 < x+y < 4.5,3.9≤z≤4.1,0.04≤a≤0.1.
It is highly preferred that the present invention is Rb for the chemical constitution formula of the narrowband green light fluorescent powder of display devicexLiySiOz:
aEu2+, wherein 3.8 < x+y < 4.2, z=4,0.06≤a≤0.08.
On the other hand, the side for the narrowband green light fluorescent powder of display device as described above is prepared the present invention provides a kind of
Method, preparation method are as follows：The raw material of synthetizing phosphor powder use the carbonate of various alkali metal, the carbonate of alkaline-earth metal, oxygen
The oxide of SiClx or silicic acid, rare earth element.According to molecular formula RbxLiySiOz:aEu2+The ratio of middle each element is accurately claimed
Raw material is taken, ground and mixed is uniform, grinding is taken out after 400-550 DEG C of pre-burning 2-6h of batch-type furnace, natural cooling, then in N2/H2Atmosphere
It carries out heat preservation 3-12h at 600-1000 DEG C lower, after natural cooling, takes out powder and carry out including that grinding, washing, sieving and drying walk
Rapid post-processing.
Above-mentioned preparation method is simple, easily operated, equipment cost is low and pollution-free.It is preparation-obtained to be used for display device
Narrowband green light fluorescent powder luminous intensity is high, excitation purity is high, halfwidth is small, temperature quenching characteristic is good, near ultraviolet and blue light
Wave band has wider strong excitation, and can be assembled into wide colour gamut liquid crystal display LED component with blue chip and narrowband red fluorescence powder,
Industry demand can largely be met.
Another aspect, that the present invention provides a kind of gamut ranges is big, color temperature uniformity is good and is not susceptible to the white of light decay
Light LED light emission device.The White LED light-emitting device includes package substrate, blue-light LED chip and can effectively absorb LED
Chip light emitting simultaneously discharges red, green light two kinds of fluorescent powders；Wherein, green light fluorescent powder is aforementioned present invention for display device
Narrowband green light fluorescent powder, chemical constitution formula RbxLiySiOz:aEu2+, wherein 3 < x+y < 5,3.8≤z≤4.2,0.005≤
a≤0.2；Preferably, chemical constitution formula RbxLiySiOz:aEu2+, wherein 3.5 < x+y < 4.5,3.9≤z≤4.1,0.04
≤a≤0.1.It is highly preferred that its chemical constitution formula is RbxLiySiOz:aEu2+, wherein 3.8 < x+y < 4.2, z=4,0.06≤a
≤0.08。
Wherein, blue-light LED chip is InGaN semiconductor chip, peak luminous wavelength 455nm.Narrowband feux rouges fluorescence
Powder is K2SiF6:Mn4+。
LED light emission device generates white light by following principle, i.e., LED chip is fixed on package substrate, is connected to electrode
And two kinds of fluorescent powders are directly or indirectly applied to blue-ray LED core (InGaN semiconductor chip) surface in a manner of coating or is for dispensing glue,
Red, green light is generated using blue light excitated fluorescent powder, obtains white light with blue light colour mixture.
White LED light-emitting device of the invention is with gamut range is big, color temperature uniformity is good and is not susceptible to light decay
Advantage.
Compared with prior art, the present invention has following advantage：
1) present invention is high for the narrowband green light fluorescent powder luminous intensity of display device, excitation purity is high, and halfwidth is small, temperature
Quenching characteristic is good, excites scope is wide, and wide colour gamut liquid crystal display LED can be assembled into blue chip and narrowband red fluorescence powder
Device can largely meet industry demand.
2) preparation method of the invention is simple, easily operated, equipment cost is low and pollution-free；It can produce huge society's effect
Benefit and economic benefit are suitble to popularity to use.
3) present invention is combined for the narrowband green light fluorescent powder of display device with narrowband red light fluorescent powder in the prior art,
It can get a series of efficient white light under blue light excitation, can satisfy the demand of field of liquid crystal display, while there is colour gamut model
Enclose that wide, color temperature uniformity is good and the advantages of being not susceptible to light decay.
Detailed description of the invention
Fig. 1 is the XRD of narrowband green light fluorescent powder prepared by embodiment 1；
Fig. 2 is the excitation spectrum and emission spectrum of narrowband green light fluorescent powder prepared by embodiment 1；
Fig. 3 is White LED light-emitting device schematic diagram and its spectrogram made by embodiment 2.
Specific embodiment
Embodiment 1：
The embodiment is Rb for the chemical constitution formula of the narrowband green light fluorescent powder of display devicexLiySiOz:aEu2+, wherein
X+y=4, z=4, a=0.08.
Weigh 0.97g Rb2CO3、2.59g Li2CO3、1.20g SiO2、0.14g Eu2O3.After abundant mix grinding is uniform, turn
It moves in corundum crucible, 500 DEG C of pre-burning 4h in batch-type furnace, is taken out after natural cooling after powder is ground in N2/ 10%H2Gas
Lower 800 DEG C of atmosphere carry out heat preservation 12h, and powder is taken out after natural cooling to carry out includes grinding, washing, is sieved and the rear place of baking step
Reason.The XRD diffraction of object phase as shown in Figure 1, excites (530nm monitoring) and emission spectrum (460nm excitation) as shown in Figure 2.It can be with
Find out that its excitation wavelength range covers 300~500nm, launch wavelength covers 500~600nm, and peak wavelength is located at 530nm,
Halfwidth is 42nm.
Embodiment 2：
A kind of White LED light-emitting device.White LED light-emitting device of the invention is prepared in following manner.The white light
LED light emission device includes package substrate, blue-light LED chip and can effectively absorb LED chip and shine and discharge red, green light
Two kinds of fluorescent powders；Wherein, green light fluorescent powder is the narrowband green light fluorescent powder for display device of above-described embodiment 1, chemistry
Composition formula is RbxLiySiOz:AEu, wherein x+y=4, z=4, a=0.08.Wherein, blue-light LED chip is InGaN semiconductor
Chip, peak luminous wavelength 455nm, red light fluorescent powder are that red light fluorescent powder is K2SiF6:Mn4+.Two kinds of fluorescent powders are equal
It is even to be dispersed in silica gel, it is covered on chip in a manner of coating or is for dispensing glue, circuit is welded, obtains white light LEDs of the invention
Light emitting device.Under 20mA electric current, light efficiency 97.28lm/W, display colour gamut is 107%NTSC.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., is all included in the scope of protection of the present invention.
Claims (8)
1. a kind of narrowband green light fluorescent powder for display device, which is characterized in that its chemical constitution formula is RbxLiySiOz:aEu2 +, wherein 3 < x+y < 5,3.8≤z≤4.2,0.005≤a≤0.2.
2. narrowband green light fluorescent powder according to claim 1, which is characterized in that 3.5 < x+y < 4.5,3.9≤z≤4.1,
0.04≤a≤0.1。
3. narrowband green light fluorescent powder according to claim 1 or 2, which is characterized in that 3.8 < x+y < 4.2, z=4,0.06
≤a≤0.08。
4. a kind of method for preparing the described in any item narrowband green light fluorescent powders for display device of claim 1-3, including
The following steps：
1) general formula R b is pressedxLiySiOz:aEu2+Stoichiometric ratio accurately weigh raw material, wherein x, y, z and a value such as claim 1-
Described in 3；
2) the raw material ground and mixed obtained step 1) is uniform, and the pre-burning in batch-type furnace obtains intermediate；
3) intermediate for obtaining step 2) is pulverized last in N2/H2It is calcined in atmosphere, to obtain sintered body；
4) the sintered body grind into powder for obtaining step 3) is to get the luminescent material.
5. the preparation method of the narrowband green light fluorescent powder according to claim 4 for display device, which is characterized in that step
It is rapid 2) described in calcined temperature be 400-550 DEG C, time 2-6h.
6. the preparation method of the narrowband green light fluorescent powder according to claim 4 for display device, which is characterized in that step
It is rapid 3) described in calcination temperature be 600-1000 DEG C, calcination time 3-12h.
7. a kind of White LED light-emitting device, light emitting device includes package substrate, blue-light LED chip and can effectively absorb LED
Chip light emitting simultaneously discharges red, green light two kinds of fluorescent powders；It is characterized in that green light fluorescent powder is that chemical constitution formula is
RbxLiySiOz:aEu2+The narrowband green light fluorescent powder for display device.
8. a kind of White LED light-emitting device as claimed in claim 7, it is characterised in that the blue-light LED chip is that InGaN is partly led
Body chip, peak luminous wavelength 455nm, red light fluorescent powder K2SiF6:Mn4+。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810748727.6A CN108913127A (en) | 2018-07-10 | 2018-07-10 | A kind of narrowband green light fluorescent powder and preparation method thereof and White LED light-emitting device |
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| CN201810748727.6A CN108913127A (en) | 2018-07-10 | 2018-07-10 | A kind of narrowband green light fluorescent powder and preparation method thereof and White LED light-emitting device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484254A (en) * | 2019-07-12 | 2019-11-22 | 广东工业大学 | Narrow transmitting green luminescent material of a kind of efficient width excitation and its preparation method and application |
| CN115437179A (en) * | 2022-08-10 | 2022-12-06 | 江苏博睿光电股份有限公司 | Display device and liquid crystal display |
| CN116333737A (en) * | 2023-03-13 | 2023-06-27 | 陕西学前师范学院 | Narrow-band blue fluorescent powder and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018029299A1 (en) * | 2016-08-12 | 2018-02-15 | Osram Gmbh | Luminophore and process for producing a luminophore |
-
2018
- 2018-07-10 CN CN201810748727.6A patent/CN108913127A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018029299A1 (en) * | 2016-08-12 | 2018-02-15 | Osram Gmbh | Luminophore and process for producing a luminophore |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110484254A (en) * | 2019-07-12 | 2019-11-22 | 广东工业大学 | Narrow transmitting green luminescent material of a kind of efficient width excitation and its preparation method and application |
| CN115437179A (en) * | 2022-08-10 | 2022-12-06 | 江苏博睿光电股份有限公司 | Display device and liquid crystal display |
| CN115437179B (en) * | 2022-08-10 | 2024-02-02 | 江苏博睿光电股份有限公司 | Display device and liquid crystal display |
| CN116333737A (en) * | 2023-03-13 | 2023-06-27 | 陕西学前师范学院 | Narrow-band blue fluorescent powder and preparation method thereof |
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