CN105400512A - Red tungstate fluorescent powder as well as preparation method and application thereof - Google Patents

Red tungstate fluorescent powder as well as preparation method and application thereof Download PDF

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Publication number
CN105400512A
CN105400512A CN201510713761.6A CN201510713761A CN105400512A CN 105400512 A CN105400512 A CN 105400512A CN 201510713761 A CN201510713761 A CN 201510713761A CN 105400512 A CN105400512 A CN 105400512A
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red
fluorescent powder
preparation
tungstate
tungstate fluorescent
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Inventor
韦波
王旭红
游威
唐文涛
顾爱伟
孙立锋
张天宇
潘莹瑛
刘海燕
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Changshu Institute of Technology
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Changshu Institute of Technology
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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
    • C09K11/7736—Vanadates; Chromates; Molybdates; Tungstates
    • 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
    • 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 the field of optical technologies, and discloses near ultraviolet or blue light LED excited red tungstate fluorescent powder. The red tungstate fluorescent powder has a chemical formula of Li2Zn(2-3x)Eu2xW2O9, wherein x is the molar percentage coefficient of a doped activation ion Eu<3+> and is more than 0 and less than or equal to 1. The preparation method of the red tungstate fluorescent powder disclosed by the invention comprises the following steps: uniformly mixing and grinding compounds containing Li, Zn, Eu and W and used as raw materials, and then performing high-temperature sintering. The fluorescent powder disclosed by the invention can be effectively excited by a near ultraviolet or blue light LED to emit red light with high color purity; and the preparation method is simple, is easy to operate, and is energy-saving, time-saving and environmentally friendly.

Description

A kind of red Tungstate fluorescent powder and its production and use
Technical field
The present invention relates to optical technical field, be specifically related to a kind of rare earth luminescent material, particularly a kind of what effectively can be excited by near-ultraviolet light or blue-ray LED take tungstate as the red fluorescence powder of matrix, and relates to preparation method and the application thereof of this fluorescent material.
Background technology
LED (LightEmittingDiode) is a kind of semiconductor energy switching device that electric energy efficiently can be converted to luminous energy, and it has, and volume is little, the life-span is long, antidetonation is not fragile, operating voltage is low, the starting-up response time is fast, energy-conservation, pollution-free and the feature such as reduce power consumption.Therefore be widely used in fields such as display, background light source, signal lamp, illuminations.Particularly in recent years, along with developing rapidly of blue, purple and ultraviolet LED, make white light LEDs have very large application prospect at lighting field, be acknowledged as the green illumination light source substituting luminescent lamp and incandescent light at present.
At present, the principal mode obtaining white light LEDs is by Phosphor-conversion, is namely mixed to form white light with other luminescent materials of LED de-excitation.Such as coordinate the jaundice fluorescent material of coloured light and red light fluorescent material with blue-ray LED, or coordinate the fluorescent material of glow green and burn red with blue-ray LED, or with purple light or ultraviolet LED de-excitation red, green, blue three kinds of fluorescent material etc.Because fluorescent material can determine key property and the parameters such as the light conversion efficiency of white light LEDs, luminous efficiency, colour temperature, chromaticity coordinates value and colour rendering index, so development white light LEDs high-efficiency fluorescence powder is significant.The red fluorescence powder that Current commercial is used for GaN base ultraviolet or blue chip is Y 2o 2s:Eu 3+, but this red fluorescence powder can not effectively absorb to blue light range near ultraviolet, its luminous intensity only has 1/8th of blue colour fluorescent powder and green emitting phosphor brightness.In addition, red fluorescence powder Y under the exciting of near-ultraviolet light or blue light 2o 2s:Eu 3+chemical property is unstable, easily decompose and produce harmful SO 2gas.These deficiencies of red fluorescence powder have become the bottleneck improving white light LEDs development.Research for red fluorescent powder for white LED makes some progress, and its kind is a lot, has their own characteristics each, also respectively has shortcoming, in general, can't reach the target that current LED technology is expected red fluorescence powder.Therefore, exploitation can be become a urgent task by the red fluorescent powder for white radiation LED that near-ultraviolet light and blue light effectively excite.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of that effectively can be excited by near-ultraviolet light or blue light, good luminous performance and stable chemical performance and the red fluorescence powder of ruddiness ideal color purity.
The preparation method being to provide above-mentioned red fluorescence powder of a second aspect of the present invention.The method preparation method technological process is simple, energy-and time-economizing, and easy handling, pollution-free, cost is low.
For solving the problems of the technologies described above, technical scheme of the present invention is: the red Tungstate fluorescent powder that a kind of near ultraviolet or blue-ray LED excite, and its chemical formula is: Li 2zn 2-3xeu 2xw 2o 9, wherein x is doping active ions Eu 3+molar percentage coefficient, 0<x≤1; Preferably, described 0<x≤0.5; More preferably, described 0<x≤0.1.
Present invention also offers the preparation method of a kind of white light LEDs by red Tungstate fluorescent powder, the method comprises the following steps:
(1) compound containing Li, Zn, Eu, W is chosen as raw material, according to chemical formula Li 2zn 2-3xeu 2xw 2o 9choose, wherein x is doping active ions Eu 3+molar percentage coefficient, 0<x≤1, accurately takes corresponding raw material respectively, desired raw material is placed in baking oven fully dry, and grinding raw material also mixes;
(2) mixture that step (1) obtains is placed in retort furnace, carries out high-temperature roasting in air atmosphere;
(3) repeating step (2) several times, as 1-2 time, obtain red Tungstate fluorescent powder of the present invention.
In above-mentioned steps (1), the compound containing Li is selected from one or two or more kinds combination in Lithium Oxide 98min, lithium nitrate, Quilonum Retard or lithium hydroxide; Compound containing Zn is selected from one or two or more kinds combination in zinc oxide, zinc nitrate, zinc carbonate; Containing Eu compound be selected from europium sesquioxide, nitrate or containing europium organic acid salt in one or two or more kinds combination; Compound containing W is selected from one or two or more kinds combination in Tungsten oxide 99.999 or ammonium tungstate.
In above-mentioned steps (1), during mixed grinding, distilled water or volatile solvent can be added, or grind when not solubilizing agent.
Volatile solvent in described step (1) is ethanol or acetone.
In above-mentioned steps (2), its high-temperature roasting temperature is 500 DEG C ~ 1000 DEG C, and sintering time is 1 hour ~ 12 hours.
Third aspect present invention provides the application of red Tungstate fluorescent powder, uses it for the white light LEDs excited by near ultraviolet or blue-ray LED.
" near ultraviolet " in the present invention refers to the spectral band of 200-400nm, is preferably the spectrum of 390-400nm wavelength.Described " blue light " spectrum refers to the spectrum of the wavelength of 420-470nm.
The positively effect that the present invention has: 1. red fluorescence powder physicochemical property of the present invention are stablized, nontoxic, nuisanceless, do not react with the oxygen in environment, carbonic acid gas and steam.2. red fluorescence powder of the present invention can the near-ultraviolet light of about 396nm and about 467nm blue-light excited under launch the good red light of purity of color of about 617nm, its excitation wavelength is mated with the output wavelength of near ultraviolet LED chip or blue-light LED chip, meets the requirement of white light LEDs solid-state photo device powder.3. preparation method's technological process of red fluorescence powder of the present invention is simple, energy-and time-economizing, and aftertreatment is simple, and preparation cost is low, and can not produce pollution.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the red fluorescence powder that the present invention is prepared by embodiment 1;
Fig. 2 is the excitation spectrum of the red fluorescence powder that the present invention is prepared by embodiment 1;
Fig. 3 is the emmission spectrum of the red fluorescence powder that the present invention is prepared by embodiment 1.
Embodiment:
For understanding the present invention further, below in conjunction with specific embodiment, preferred version of the present invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
The tungstate red fluorescent powder that a kind of near ultraviolet of the present embodiment or blue-ray LED excite, the chemical formula of this red fluorescence powder is: Li 2zn 1.82eu 0.12w 2o 9.
The present embodiment prepares Li 2zn 1.82eu 0.12w 2o 9the concrete steps of red fluorescence powder are:
Desired raw material is placed in baking oven fully dry, then takes Eu 2o 30.1609 weight part, ZnO1.1283 weight part, Li 2cO 30.5629 weight part, WO 33.5325 weight parts, Eu in above raw material 2o 3purity is 99.99% (quality), and remaining is all analytical pure.After even for above-mentioned raw materials mixed grinding in agate mortar, be placed in retort furnace, pre-burning is carried out 5 hours in atmosphere in 600 DEG C, powder after pre-burning is ground to again evenly, 6 hours are sintered in atmosphere under 800 DEG C of conditions, be cooled to room temperature, namely obtain the red fluorescence powder of above-mentioned chemical expression.
The tungstate matrix red fluorescence powder that the present embodiment prepares, its XRD spectra is see Fig. 1.As seen from Figure 1, the diffraction peak intensity of red fluorescence powder is high and comparatively sharp-pointed, illustrates that red fluorescence powder crystal property well, illustrates that red fluorescence powder that this enforcement synthesizes is without dephasign.
The excitation spectrum of the tungstate red fluorescent powder that the present embodiment obtains and emmission spectrum are respectively by shown in Fig. 2 and Fig. 3, wherein: two main excitation peaks are respectively near 396nm and 467nm, its main emission peak is near 617nm ruddiness, and can calculate its chromaticity coordinates by spectrogram is x=0.675, y=0.325.It can thus be appreciated that this fluorescent material can effectively be excited by near-ultraviolet light and blue light and send comparatively pure ruddiness, can be used for white light LEDs.
Embodiment 2
The present embodiment preparative chemistry formula is Li 2zn 1.88eu 0.08w 2o 9red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Desired raw material is placed in baking oven fully dry, then takes Eu 2o 30.1287 weight part, ZnO1.3986 weight part, Li 2cO 30.6755 weight part, WO 34.2390 weight parts, Eu in above raw material 2o 3purity is 99.99% (quality), and remaining is all analytical pure.By above-mentioned raw materials mixed grinding in agate mortar, volatile solvent ethanol is added in process of lapping, Deng grinding after 1 hour, be positioned in corundum crucible, carry out pre-burning 5 hours in 600 DEG C in atmosphere, the powder after pre-burning is ground to again evenly, sinter 6 hours under 800 DEG C of conditions in atmosphere, be cooled to room temperature, namely obtain the red fluorescence powder of above-mentioned chemical expression.
Embodiment 3
The present embodiment preparative chemistry formula is Li 2zn 1.7eu 0.2w 2o 9red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Desired raw material is placed in baking oven fully dry, then takes Eu 2o 31.0558 weight part, Y 2o 30.4516 weight part, Na 2cO 30.2650 weight part, WO 34.0571 weight parts, Eu in above raw material 2o 3purity is 99.99% (quality), and remaining is all analytical pure.Above-mentioned raw materials is ground 3 hours with the speed of 300 revs/min in ball mill, after mixed grinding is even, be positioned in corundum crucible, carry out once sintered in atmosphere, sintering temperature is 850 DEG C, sintering time is 8 hours, sinters completely to be cooled to room temperature, namely obtains the red fluorescence powder of above-mentioned chemical expression.
Embodiment 4
The present embodiment preparative chemistry formula is Li 2zn 1.76eu 0.16w 2o 9red fluorescence powder, preparation method and the red fluorescence powder performance for preparing, substantially with embodiment 1, to be now summarized as follows preparation process:
Desired raw material is placed in baking oven fully dry, then takes Eu 2o 30.2145 weight part, ZnO1.0911 weight part, Li 2o0.2276 weight part, H 8n 2o 44.3258 weight parts, Eu in above raw material 2o 3purity is 99.99% (quality), and remaining is all analytical pure.By above-mentioned raw materials mixed grinding in agate mortar, volatile solvent acetone is added in process of lapping, Deng grinding after 1.5 hours, be positioned in corundum crucible, carry out pre-burning 5 hours in 500 DEG C in atmosphere, the powder after pre-burning is ground to again evenly, sinter 5 hours under 850 DEG C of conditions in atmosphere, be cooled to room temperature, namely obtain the red fluorescence powder of above-mentioned chemical expression.
Technology contents of the present invention and technical characteristic have disclosed as above; but those of ordinary skill in the art still may do all replacement and the modification that do not deviate from spirit of the present invention based on teaching of the present invention and announcement; therefore; scope should be not limited to the content that embodiment discloses; and various do not deviate from replacement of the present invention and modification should be comprised, and contained by present patent application claim.

Claims (10)

1. a red Tungstate fluorescent powder, is characterized in that, its chemical formula is: Li 2zn 2-3xeu 2xw 2o 9, wherein x is doping active ions Eu 3+molar percentage coefficient, 0<x≤1.
2. a preparation method for red Tungstate fluorescent powder as claimed in claim 1, it is characterized in that, it comprises the steps:
(1) compound containing Li, Zn, Eu, W is chosen as raw material, according to chemical formula Li 2zn 2-3xeu 2xw 2o 9choose, wherein x is doping active ions Eu 3+molar percentage coefficient, 0<x≤1, accurately takes corresponding raw material respectively, desired raw material is placed in baking oven fully dry, and grinding raw material also mixes;
(2) mixture that step (1) obtains is placed in retort furnace, carries out high-temperature roasting in air atmosphere, temperature is 500 DEG C ~ 1000 DEG C, and sintering time is 1 hour ~ 12 hours;
(3) repeating step (2) several times obtain red Tungstate fluorescent powder of the present invention.
3. the preparation method of red Tungstate fluorescent powder according to claim 2, is characterized in that, in above-mentioned steps (1), the compound containing Li is selected from one or two or more kinds combination in Lithium Oxide 98min, lithium nitrate, Quilonum Retard or lithium hydroxide; Compound containing Zn is selected from one or two or more kinds combination in zinc oxide, zinc nitrate, zinc carbonate.
4. the preparation method of red Tungstate fluorescent powder according to claim 2, is characterized in that, the described compound containing Eu is selected from europium sesquioxide, nitrate or combines containing one or two or more kinds in the organic acid salt of europium; Compound containing W is selected from one or two or more kinds combination in Tungsten oxide 99.999 or ammonium tungstate.
5. the preparation method of red Tungstate fluorescent powder according to claim 2, is characterized in that, in above-mentioned steps (1), can add distilled water or volatile solvent during mixed grinding.
6. the preparation method of red Tungstate fluorescent powder according to claim 2, is characterized in that, in above-mentioned steps (1), and not solubilizing agent during mixed grinding.
7. an application for red Tungstate fluorescent powder as claimed in claim 1, is characterized in that, uses it for the white light LEDs excited by near ultraviolet LED.
8. purposes according to claim 7, is characterized in that, described " near ultraviolet " refers to the spectrum of 200-400nm wavelength.
9. an application for red Tungstate fluorescent powder as claimed in claim 1, is characterized in that, uses it for the white light LEDs excited by blue-ray LED.
10. purposes according to claim 9, is characterized in that, described " blue light " refers to the spectrum of the wavelength of 420-470nm.
CN201510713761.6A 2015-10-28 2015-10-28 Red tungstate fluorescent powder as well as preparation method and application thereof Pending CN105400512A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105969352A (en) * 2016-06-04 2016-09-28 王颖畅 Red phosphor for LED light source and preparation method of red phosphor
CN110896086A (en) * 2018-09-13 2020-03-20 群创光电股份有限公司 Electronic device
CN114479854A (en) * 2021-12-28 2022-05-13 吉林化工学院 Charge compensation type molybdenum tungstate red luminescent material and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN101157853A (en) * 2007-11-12 2008-04-09 中国科学院长春光学精密机械与物理研究所 Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof
CN102533266A (en) * 2011-12-15 2012-07-04 常熟理工学院 Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder
CN103396794A (en) * 2013-07-30 2013-11-20 苏州大学 Eu<3+> activated sodium barium tungstate fluorescent powder, preparation method and application thereof
CN103881712A (en) * 2014-02-28 2014-06-25 淮南师范学院 Tungstate-matrix red fluorescent powder for white light LED (Light Emitting diode) and preparation method of powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157853A (en) * 2007-11-12 2008-04-09 中国科学院长春光学精密机械与物理研究所 Near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof
CN102533266A (en) * 2011-12-15 2012-07-04 常熟理工学院 Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder
CN103396794A (en) * 2013-07-30 2013-11-20 苏州大学 Eu<3+> activated sodium barium tungstate fluorescent powder, preparation method and application thereof
CN103881712A (en) * 2014-02-28 2014-06-25 淮南师范学院 Tungstate-matrix red fluorescent powder for white light LED (Light Emitting diode) and preparation method of powder

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105969352A (en) * 2016-06-04 2016-09-28 王颖畅 Red phosphor for LED light source and preparation method of red phosphor
CN110896086A (en) * 2018-09-13 2020-03-20 群创光电股份有限公司 Electronic device
CN110896086B (en) * 2018-09-13 2022-02-11 群创光电股份有限公司 Electronic device
CN114479854A (en) * 2021-12-28 2022-05-13 吉林化工学院 Charge compensation type molybdenum tungstate red luminescent material and preparation method and application thereof
CN114479854B (en) * 2021-12-28 2023-11-21 吉林化工学院 Charge compensation type molybdenum tungstate red luminescent material and preparation method and application thereof

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Application publication date: 20160316