CN108753277A - White light LEDs narrow-band blue light fluorescent powder and preparation method and White LED light-emitting device - Google Patents
White light LEDs narrow-band blue light fluorescent powder and preparation method and White LED light-emitting device Download PDFInfo
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- CN108753277A CN108753277A CN201810748705.XA CN201810748705A CN108753277A CN 108753277 A CN108753277 A CN 108753277A CN 201810748705 A CN201810748705 A CN 201810748705A CN 108753277 A CN108753277 A CN 108753277A
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- fluorescent powder
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- blue light
- white light
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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 with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
Abstract
The invention belongs to luminescent material technical fields；It is related to a kind of controllable narrow-band blue light fluorescent powder of white light LEDs spectrum and preparation method thereof and White LED light-emitting device.Blue light fluorescent powder chemical constitution formula is Rb1‑x‑yNaxLi3SiO4:yEu2+.Preparation method of the present invention is simple, easily operated, equipment cost is low and pollution-free；Obtained white light LEDs high, chemical stability and temperature quenching characteristic is good, excites scope is wider with narrow-band blue light light-emitting phosphor intensity, transmitting range is narrow.It is combined with feux rouges in the prior art and green light fluorescent powder, and a series of efficient white light is can get under near ultraviolet excitation, demand of the general illumination field for different type light source is disclosure satisfy that, has the advantages that color temperature uniformity is good and is not susceptible to light decay.
Description
Technical field
The invention belongs to luminescent material technical fields；It is related to a kind of controllable narrow-band blue light fluorescent powder of white light LEDs spectrum
And preparation method thereof and White LED light-emitting device.
Background technology
In recent years, white light LEDs due to its low power consuming, strong applicability, stability is high, the response time is short, long lifespan, without dirt
The advantage of dye, multicolor luminous etc. gets more and more people's extensive concerning, and is known as forth generation lighting source.Its plurality of advantages is common
The numerous areas such as illumination, signal lamp, LED backlight have been obtained for being widely applied.
The mode for making white light LEDs at present mainly has three classes：(1) red, blue, green light chip or Huang, blue chip composition；
(2) blue-light LED chip is formed with red green color fluorescent powder or blue-light LED chip is formed with yellow fluorescent powder；(3) near ultraviolet LED core
Piece is formed with red-green-blue fluorescent powder.Based on the considerations of device cost, the complexity of realization and color quality etc.,
People pass through realizes that white light LEDs shine frequently with latter two mode.Correspondingly, in order to near ultraviolet chip or blue chip
Emission wavelength matches, and to prepare the white light LEDs of high efficiency and high brightness, develops near ultraviolet excitated or blue light activated three base
Color fluorescent material becomes the emphasis of people's research increasingly.
Invention content
High, chemical stability that the present invention provides a kind of luminous intensities and temperature quenching characteristic is good, excites scope is wider
White light LEDs narrow-band blue light fluorescent powder.
The two of the object of the invention are to provide a kind of preparation method preparing above-mentioned white light LEDs blue light emitting material.The system
Preparation Method is simple, easily operated, equipment cost is low and pollution-free.
The three of the object of the invention are to provide that a kind of color temperature uniformity is good, transmitting band is narrow, and are not susceptible to the white light of light decay
LED light emission device.
To realize that upper partially substituted alkaline-earth silicate is matrix, using divalent Eu as activator, a kind of luminous intensity is obtained
High, chemical stability and the white light LEDs narrow-band blue light fluorescent powder that temperature quenching characteristic is good, excites scope is wider.
White light LEDs are Rb with the chemical constitution formula of narrow-band blue light fluorescent powder1-x-yNaxLi3SiO4:yEu2+, wherein 0.70≤x
≤ 0.80,0.03≤y≤0.05.Preferably, the chemical constitution formula of white light LEDs of the invention blue light fluorescent powder is Rb1-x- yNaxLi3SiO4:yEu2+, wherein x=0.75, y=0.03, that is, Rb0.22Na0.75Li3SiO4:0.03Eu2+。
On the other hand, the present invention provides a kind of method preparing above-mentioned white light LEDs narrow-band blue light fluorescent powder, this method
Include the following steps：
1) general formula R b is pressed1-x-yNaxLi3SiO4:yEu2+, wherein 0.70≤x≤0.80,0.03≤y≤0.05, weigh the hair
Corresponding raw material in luminescent material；
2) the solid mixture grind into powder for obtaining step 1), at a temperature of 500-700 DEG C and under oxidizing atmosphere
Calcining 6-15 hours obtains presoma；
3) the presoma grinding that step 2) obtains is placed in alumina crucible, then alumina crucible is placed in tube furnace
In, it at a temperature of 600-900 DEG C and calcines 2-6 hours under reducing atmosphere, after cooling, and grind into powder is to get the hair
Luminescent material.
In step 1), raw material can come from the simple substance of sodium, rubidium, silicon, lithium and europium, oxide, chloride, sulfide,
Carbonate, sulfate, phosphate, nitrate and other suitable raw materials.In one preferred embodiment, raw material comes
From the chloride, carbonate, nitrate of sodium, rubidium, silicon, lithium and europium.In a preferred embodiment, raw material comes from
The carbonate and oxide of sodium, rubidium, silicon, lithium and europium.
In one preferred embodiment, by general formula R b1-x-yNaxLi3SiO4:yEu2+Stoichiometric ratio weigh carbonic acid
Sodium, rubidium carbonate, lithium carbonate, silica and europium oxide, wherein 0.70≤x≤0.80,0.03≤y≤0.05；It is preferred that x=
0.75, y=0.03.
The temperature and time described in step 2) refers to calcining 6-15 hours at a temperature of 500-750 DEG C, preferably 550-
It is calcined 12 hours at a temperature of being calcined at a temperature of 700 DEG C 9-12 hours, most preferably 650 DEG C.
Temperature and time described in step 3) is calcined 2-6 hours at a temperature of referring to 600-900 DEG C, preferably 700-800
It is calcined 4 hours at a temperature of being calcined at a temperature of DEG C 3-5 hours, most preferably 750 DEG C.The reducing atmosphere is selected from H2Atmosphere, H2/
N2Atmosphere and CO atmosphere.In one preferred embodiment, the reducing atmosphere is selected from H2/N2Atmosphere, the atmosphere is to this hair
The synthesis of bright white light LEDs blue light fluorescent powder and performance improvement are beneficial.
Above-mentioned preparation method is simple, easily operated, equipment cost is low and pollution-free.Preparation-obtained white light LEDs are blue
Emitting phosphor luminous intensity is high, chemical stability and temperature quenching characteristic are good, excites scope is wider, in ultraviolet and purple light wave band
There is wider strong excitation, and white light LED part can be assembled into near ultraviolet chip, green and red fluorescence powder, it can be larger
Meet industry demand in degree.
Another aspect, that the present invention provides a kind of color developings is good, 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, black light LED chip and can effectively absorb LED core
Piece shines and discharges the three primary colors fluorescent powder of redgreenblue light；Wherein, blue light fluorescent powder is that the white light LEDs of aforementioned present invention are used
Narrow-band blue light fluorescent powder, chemical constitution formula Rb1-x-yNaxLi3SiO4:yEu2+, wherein 0.70≤x≤0.80,0.03≤y≤
0.05.Preferably, chemical constitution formula Rb0.22Na0.75Li3SiO4:0.03Eu2+。
Wherein, near ultraviolet LED chip is GaN semiconductor chips, peak luminous wavelength 395nm.Red light fluorescent powder is
K2SiF6:Mn4+, green light fluorescent powder is β-SiAlON:Eu2+。
LED light emission device generates white light by following principle, i.e., LED chip is fixed on package substrate, is connected to electrode
And three primary colors fluorescent powder is directly or indirectly applied to near ultraviolet LED chip (GaN semiconductor chips) in a manner of coating or is for dispensing glue
Surface generates three primary colours light using near ultraviolet excitation fluorescent powder, and colour mixture obtains white light.
The White LED light-emitting device of the present invention is with color developing is good, color temperature uniformity is good and is not susceptible to light decay
Advantage.
Compared with prior art, the present invention has following advantage：
1) white light LEDs of the invention narrow-band blue light light-emitting phosphor intensity height, chemical stability and temperature quenching characteristic
Well, excites scope is wider, has wider strong excitation near ultraviolet band, and can be near ultraviolet chip and feux rouges, blue phosphor
Powder is assembled into white light LED part, can largely meet industry demand.
2) preparation method of the invention is simple, easily operated, equipment cost is low and pollution-free；Huge society's effect can be generated
Benefit and economic benefit are suitble to popularity to use.
3) white light LEDs of the invention are combined with narrow-band blue light fluorescent powder with feux rouges in the prior art and green light fluorescent powder,
It can get a series of efficient white light under near ultraviolet excitation, disclosure satisfy that general illumination field for different type light source
Demand, while having the advantages that color developing is good, color temperature uniformity is good and is not susceptible to light decay.
Description of the drawings
Fig. 1 is X-ray powder (XRD) figure of the fluorescent material prepared by embodiment 1.Rb0.22Na0.75Li3SiO4Reference substance
The XRD diagram of matter is also given at Fig. 1 as reference.
Fig. 2 be and embodiment 1 prepared by fluorescent material excitation spectrum (monitoring wavelength XemFor 471nm) and emission spectrum
(excitation wavelength lambdaexFor 365nm) curve synoptic diagram.
Specific implementation mode
Embodiment 1：
The chemical constitution formula of the white light LEDs of embodiment blue light fluorescent powder is Rb1-x-yNaxLi3SiO4:yEu2+, wherein x
=0.75, y=0.03, expression Rb0.22Na0.75Li3SiO4:0.03Eu2+。
By Rb0.22Na0.75Li3SiO4:0.03Eu2+Middle each element measures ratio, weighs Rb2CO3,Na2CO3,Li2CO3,SiO2
And Eu2O3, by Rb2CO3,Na2CO3,Li2CO3,SiO2And Eu2O3It is fully ground, then forges the powder after grinding at 650 DEG C
In H after being regrind after burning 12 hours2/N24 hours are calcined to get single-phase phosphor at 750 DEG C under atmosphere
Rb0.22Na0.75Li3SiO4:0.03Eu2+。
White LED light-emitting device Application Example
The White LED light-emitting device of the present invention is prepared in following manner.The White LED light-emitting device includes encapsulation base
Plate, black light LED chip and it can effectively absorb the three primary colours fluorescence that LED chip shines and discharges redgreenblue light
Powder；Wherein, blue light fluorescent powder is the white light LEDs blue light fluorescent powder of above-described embodiment 1, and chemical constitution formula is
Rb0.22Na0.75Li3SiO4:0.03Eu2+.Wherein, near ultraviolet LED chip is GaN semiconductor chips, and peak luminous wavelength is
395nm.Red light fluorescent powder is that red light fluorescent powder is K2SiF6:Mn4+, green light fluorescent powder is β-SiAlON:Eu2+.Three primary colours are glimmering
Light powder is dispersed in silica gel, is covered on chip in a manner of coating or is for dispensing glue, circuit is welded, obtain the white of the present invention
Light LED light emission device.
Light efficiency of the white light LEDs encapsulated with blue light fluorescent powder using the white light LEDs of embodiment 1 under different electric currents and photochromic
Data.Referring specifically to table 1.
Table 1
As it can be seen from table 1 the white light LEDs blue light fluorescent powder of the present invention and feux rouges in the prior art and green-emitting fluorescent
Powder combines, and a series of efficient white light is can get under near ultraviolet excitation, disclosure satisfy that general illumination field for inhomogeneity
The demand of type light source.In a large number of experiments, the white light LEDs prepared by white light LEDs blue light fluorescent powder by the present invention, which shine, to be filled
It is good to set color developing, color temperature uniformity is good and the advantages of being not susceptible to light decay.
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, any made by repair
Change, equivalent replacement, improvement etc., be all included in the scope of protection of the present invention.
Claims (10)
1. a kind of white light LEDs narrow-band blue light fluorescent powder, which is characterized in that its chemical constitution formula is Rb1-x-yNaxLi3SiO4:
yEu2+, wherein 0.70≤x≤0.80,0.03≤y≤0.05.
2. white light LEDs according to claim 1 narrow-band blue light fluorescent powder, which is characterized in that wherein x=0.75, y=
0.03。
3. a kind of preparing the method such as claim 1-2 any one of them white light LEDs blue light fluorescent powders, it is characterised in that packet
Include the following steps：
1) general formula R b is pressed1-x-yNaxLi3SiO4:yEu2+Stoichiometric ratio accurately weigh raw material, and fully finely ground mixing obtains original
Expect mixture；
2) raw mixture that step 1) obtains is calcined in oxidizing atmosphere, to obtain presoma；
3) the presoma grind into powder that step 2) obtains is calcined in a reducing atmosphere, to obtain sintered body；
4) the sintered body grind into powder for obtaining step 3) is to get the luminescent material.
4. the preparation method of white light LEDs blue light fluorescent powder as claimed in claim 3, it is characterised in that
Temperature and time described in step 2) is calcined 6-15 hours at a temperature of referring to 500-750 DEG C.
5. the preparation method of white light LEDs blue light fluorescent powder as described in claim 3 or 4, it is characterised in that institute in step 2)
It states and is calcined 9-12 hours at a temperature of temperature and time refers to 550-700 DEG C.
6. the preparation method of white light LEDs blue light fluorescent powder as claimed in claim 3, it is characterised in that warm described in step 3)
Degree and time calcine 2-6 hours at a temperature of referring to 600-900 DEG C.
7. the preparation method of the white light LEDs blue light fluorescent powder as described in claim 3 or 6, it is characterised in that institute in step 3)
It states and is calcined 3-5 hours at a temperature of temperature and time refers to 700-800 DEG C.
8. the preparation method of white light LEDs blue light fluorescent powder as claimed in claim 3, it is characterised in that described in step 3) also
Primordial Qi atmosphere is selected from H2Atmosphere, H2/N2Atmosphere and CO atmosphere.
9. a kind of White LED light-emitting device, including package substrate, near ultraviolet LED chip and it can effectively absorb LED chip hair
Light and the three primary colors fluorescent powder for discharging redgreenblue light, which is characterized in that blue light fluorescent powder is any one of claim 1-2 institutes
The white light LEDs blue light fluorescent powder stated.
10. White LED light-emitting device according to claim 9, wherein the near ultraviolet LED chip is GaN semiconductor cores
Piece；The red light fluorescent powder is K2SiF6:Mn4+, green light fluorescent powder is β-SiAlON:Eu2+。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810748705.XA CN108753277A (en) | 2018-07-10 | 2018-07-10 | White light LEDs narrow-band blue light fluorescent powder and preparation method and White LED light-emitting device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810748705.XA CN108753277A (en) | 2018-07-10 | 2018-07-10 | White light LEDs narrow-band blue light fluorescent powder and preparation method and White LED light-emitting device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593521A (en) * | 2018-11-19 | 2019-04-09 | 广东晶科电子股份有限公司 | A kind of blue green light illuminator, LED component and preparation method thereof |
| 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 |
| CN112457848A (en) * | 2020-12-09 | 2021-03-09 | 江苏科技大学 | Narrow-band blue-light fluorescent powder and preparation method and application thereof |
| CN112812775A (en) * | 2019-11-18 | 2021-05-18 | 富源磁器股份有限公司 | Fluorescent material |
| CN113031380A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | RGB fluorescent wheel with narrow-band luminescent spectrum for laser projector |
| CN115232619A (en) * | 2022-08-10 | 2022-10-25 | 江苏博睿光电股份有限公司 | Green phosphor and preparation method and application thereof |
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| CN104781369A (en) * | 2012-05-22 | 2015-07-15 | 皇家飞利浦有限公司 | New phosphors, such as new narrow-band red emitting phosphors, for solid state lighting |
| WO2018029299A1 (en) * | 2016-08-12 | 2018-02-15 | Osram Gmbh | Luminophore and process for producing a luminophore |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104781369A (en) * | 2012-05-22 | 2015-07-15 | 皇家飞利浦有限公司 | New phosphors, such as new narrow-band red emitting phosphors, for solid state lighting |
| WO2018029299A1 (en) * | 2016-08-12 | 2018-02-15 | Osram Gmbh | Luminophore and process for producing a luminophore |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593521A (en) * | 2018-11-19 | 2019-04-09 | 广东晶科电子股份有限公司 | A kind of blue green light illuminator, LED component and preparation method thereof |
| 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 |
| CN112812775A (en) * | 2019-11-18 | 2021-05-18 | 富源磁器股份有限公司 | Fluorescent material |
| CN113031380A (en) * | 2019-12-09 | 2021-06-25 | 上海航空电器有限公司 | RGB fluorescent wheel with narrow-band luminescent spectrum for laser projector |
| CN112457848A (en) * | 2020-12-09 | 2021-03-09 | 江苏科技大学 | Narrow-band blue-light fluorescent powder and preparation method and application thereof |
| CN115232619A (en) * | 2022-08-10 | 2022-10-25 | 江苏博睿光电股份有限公司 | Green phosphor and preparation method and application thereof |
| CN115232619B (en) * | 2022-08-10 | 2023-09-19 | 江苏博睿光电股份有限公司 | Green fluorescent powder and preparation method and application thereof |
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Application publication date: 20181106 |