CN105838368A - Fluorescent material for white light LED and preparation method of fluorescent material - Google Patents
Fluorescent material for white light LED and preparation method of fluorescent material Download PDFInfo
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- CN105838368A CN105838368A CN201610356661.7A CN201610356661A CN105838368A CN 105838368 A CN105838368 A CN 105838368A CN 201610356661 A CN201610356661 A CN 201610356661A CN 105838368 A CN105838368 A CN 105838368A
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- 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
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Abstract
The invention relates to a fluorescent material for a white light LED and a preparation method of the fluorescent material. The chemical formula of the material is MgNb2O6:xEu, wherein x is the doping mole percent of Eu3+, and is greater than or equal to 0.0001 and smaller than or equal to 0.5. The method adopts a high temperature solid state method, and the material is prepared from the MgNb2O6 which is taken as a matrix. The fluorescent powder is high in luminescent intensity and good in stability, can absorb ultraviolet light about 250 to 480 nanometers, converts and emits red light about 615 nanometers, and can be applied to the preparation of LED; the preparation process is simple and flexible, the repeatability is good, and the whole process does not need reducing atmosphere protection, so that energy consumption is reduced, moreover, the requirement on equipment is not high, raw materials are cheap and easy to get, the production cost is further reduced, and compared with sulfide-based and halide-based fluorescent powder, the fluorescent material is more environment-friendly.
Description
Technical field
The present invention relates to a kind of fluorescent material for white light LED and preparation method thereof, belong to phosphor field.
Background technology
Along with Global Environmental Problems increases the weight of, energy shortage, energy-conserving and environment-protective become the important topic that current people face.Shine common
Bright illumination field, white light LEDs product becomes emphasis of concern.It is a kind of new green environment protection illuminating product, has relatively
The advantages such as high electrical efficiency, less volume, low-power, high life, it is considered to be a new generation's lighting source, have very well
Development trend.
White light LEDs produces white light mainly two approach: the first is that three kinds of LED combination of red, green, blue are produced white light；
The second is to deactivate luminous conversion phosphor with LED to be mixed to form white light, and this approach has two kinds of implementations, wherein compares
Ripe method is that blue-light LED chip realizes white light emission (United States Patent (USP) with the collocation of YAG:Ce yellow fluorescent powder
5998925), but owing to lacking red light, the compound white light obtained is cool white light, and therefore, the program still needs to add suitable red
Look fluorescent material improves its colour rendering index, and another kind of scheme is then by nearly purple LED chip (390-410nm) and red green blue
Three primary colors fluorescent powder combines, and therefore red fluorescence powder plays very important effect.And effectively the exciting of existing red fluorescence powder
Scope is most in shortwave UV region, and the launching efficiency under near ultraviolet and blue light is low.Therefore, the near ultraviolet of efficient stable is developed
Light, blue-ray LED red fluorescence powder are particularly important.At present, market still lacks excellent performance can by black light or
The red fluorescence powder that blue-light LED chip excites.
At present, it is possible to the red fluorescence powder all reaching application requirement in terms of luminous intensity and stability is the most rarely found.Such as: have
People attempts Y2O2S:Eu3+It is applied to WLED field, but, the most commercial red fluorescence powder Y2O2S:Eu3+Exist many
Shortcoming: luminous efficiency is low under near ultraviolet excitation, chemical property is unstable, easily decomposes, and the life-span is short, the precipitation of element sulphur
Chip can be caused corrosive effects, thus cause the inefficacy of whole device.It addition, relate in document and patent report is several
What class was main be expected also has for the red fluorescence powder of LED: Ca3(VO4)2:Eu3+、YVO4:Eu3+、Y2O3:Eu3+, Bi3+、
CaO:Eu3+、CaMoO4:Eu3+、(Gd,Y,Eu)2(MoO4)3:Sm3+、Ca5(SiO4)2Cl2:Eu2+、Sr2Si5N8:Eu2+Deng.Its
The stability high-luminous-efficiency of the nitrogen oxides that middle rare earth activates is good and comes into one's own, such as: Sr2Si5N8:Eu2+、
SrSi2O2N2:Eu2+, but the synthesis of the matrix of this kind of material needs in high temperature (1600-1700 DEG C) high nitrogen or ammonia pressure (10atm)
Under complete, to produce equipment requirement the harshest.
Summary of the invention
The problem existed for above-mentioned prior art, it is an object of the invention to provide that a kind of illumination effect is good, good stability, can
To be applied to fluorescent material prepared by LED illumination device；Another object of the present invention is to provide one to prepare simply, consume energy less,
The preparation method of the fluorescent material that production cost is low.
For achieving the above object, the technical solution used in the present invention is: a kind of fluorescent material for white light LED, the chemistry of material
Formula is MgNb2O6: xEu, wherein x is Eu3+The mole percent of doping, 0.0001≤x≤0.5.
The present invention provides the preparation method of a kind of above-mentioned fluorescent material the most simultaneously, comprises the steps:
(1) chemical formula MgNb is pressed2O6: the stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing magnesium from
Sub-Mg2+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, grind and mix,
Obtain mixture；
(2) mixture that step (1) obtains being carried out precalcining in air atmosphere, precalcining temperature is 500～900 DEG C,
The precalcining time is 2～16 hours；
(3) mixture that step (2) obtains is cooled down naturally, after grinding and mixing, calcine in air atmosphere, forge
Burning temperature is 900～1500 DEG C, and calcination time is 2～16 hours, naturally cools to room temperature, i.e. obtains fluorescent material.
As the preferred version of said method, the precalcining temperature of step (2) is 550～850 DEG C, and the precalcining time is 3～12
Hour.
As the preferred version of said method, the calcining heat of step (3) is 950～1400 DEG C, and calcination time is 2～9 hours.
Above-mentioned containing magnesium ion Mg2+Compound be the one in magnesia, magnesium chloride, magnesium nitrate, basic magnesium carbonate；Institute
State containing niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In
A kind of；Described containing europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3·6H2O, europium carbonate
Eu2(CO3)3In one..
Technical solution of the present invention advantage is: the fluorescent material luminous intensity of the present invention is high, good stability, can inhale by 250～
The ultraviolet light of 480 nm, switching emission goes out the ruddiness of 615 nm, it is possible to be applied to the preparation of LED；Prepared
Journey simple and flexible, favorable repeatability, and whole during be not required to reducing atmosphere protection, therefore reduce energy consumption, and for setting
Standby is less demanding, and cheaper starting materials is easy to get, and has been greatly reduced the cost produced, relative to fluorescence such as sulfide, halide bases
Powder, more environmentally-friendly.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 prepares sample exciting light spectrogram under 615 nano wave length monitoring；
Fig. 2 is that the embodiment of the present invention 1 prepares sample luminescent spectrum figure under 390 nano wave lengths excite；
Fig. 3 is the decay of luminescence curve that the embodiment of the present invention 1 prepares sample；
Fig. 4 is the ESEM microphoto that the embodiment of the present invention 1 prepares sample；
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
According to chemical formula MgNb2O6: 0.0001Eu weighs MgO:1.400 gram of magnesia, europium oxide Eu2O3: 0.001 gram, five
Aoxidize two niobium Nb2O5: 9.580 grams, add in agate mortar appropriate acetone mixed grinding uniformly after, at air
Atmosphere carries out precalcining, calcines at 500 DEG C 2 hours after cooling down with stove, take out sample by the raw material of precalcining
Again it is sufficiently mixed grinding uniformly by identical method, again calcines in air atmosphere, calcine 2 at 900 DEG C little
Time, it is cooled to room temperature, is fully ground after taking-up and i.e. obtains sample.
Fig. 1 is the sample prepared by the present embodiment technical scheme excitation spectrum under 615 nano wave length light monitoring, as seen from the figure,
This material can be excited by wavelength light in 250～480 nanometer range；
Fig. 2 is the sample prepared by the present embodiment technical scheme emission spectrum figure under 390 nano wave length light excite, test knot
Fruit display, electromagnetic radiation goes out the centre wavelength light in 615 nanometers, and obtained material can effectively convert ultraviolet light into transmitting
Ruddiness.
Fig. 3 is that to prepare sample in excitation wavelength be 390 nanometers to the embodiment of the present invention 1, and monitoring wavelength is that the luminescence of 615 nanometers declines
Subtracting curve, can be calculated die-away time is 1.400 milliseconds.
Fig. 4 is the scanning electron microscope diagram spectrum of sample as prepared by the present embodiment technical scheme, it can be seen that gained
Sample particle is uniformly dispersed, and its average grain diameter is 1.45 microns.
Embodiment 2
According to chemical formula MgNb2O6: 0.01Eu weighs basic magnesium carbonate 4MgCO3·Mg(OH)2·5H2O:4.080 gram, europium carbonate
Eu2(CO3)3: 0.004 gram, niobium hydroxide Nb (OH)5: 5.150 grams, agate mortar adds appropriate acetone mixing
After grinding uniformly, air atmosphere carries out precalcining, after precalcining cools down with stove for 16 hours at 900 DEG C, take
Go out sample and the raw material of precalcining is sufficiently mixed grinding uniformly, by identical method again in air atmosphere again
Secondary calcining, calcines 10 hours at 1500 DEG C, is cooled to room temperature, is fully ground and i.e. obtains sample after taking-up.
It is micro-that the present embodiment technical scheme prepares the exciting light spectrogram of sample, fluorescence spectrum figure, decay of luminescence curve, ESEM
Photo is consistent with the sample of preparation in embodiment 1.
Embodiment 3
According to chemical formula MgNb2O6: 0.01Eu weighs MgO:0.830 gram of magnesia, europium nitrate Eu (NO3)3·6H2O:0.089
Gram, niobium chloride NbCl5: 1.780 grams, add in agate mortar appropriate acetone mixed grinding uniformly after, at sky
Gas atmosphere carries out precalcining, after precalcining cools down with stove for 3 hours at 550 DEG C, takes out sample by precalcining
Raw material is sufficiently mixed grinding uniformly by identical method again, again calcines in air atmosphere, calcines at 950 DEG C
2 hours, it is cooled to room temperature, is fully ground after taking-up and i.e. obtains sample.
It is micro-that the present embodiment technical scheme prepares the exciting light spectrogram of sample, fluorescence spectrum figure, decay of luminescence curve, ESEM
Photo is consistent with the sample of preparation in embodiment 1.
Embodiment 4
According to chemical formula MgNb2O6: 0.1Eu weighs basic magnesium carbonate 4MgCO3·Mg(OH)2·5H2O:3.480 gram, europium oxide
Eu2O3: 0., 252 gram, niobium pentaoxide Nb2O5: 0.895 gram, agate mortar adds appropriate acetone mixing and grinds
After mill is uniform, air atmosphere carries out precalcining, after precalcining cools down with stove for 12 hours at 850 DEG C, take out
The raw material of precalcining is sufficiently mixed grinding uniformly, by identical method by sample again in air atmosphere again
Calcining, calcines 9 hours at 1400 DEG C, is cooled to room temperature, is fully ground and i.e. obtains sample after taking-up.
It is micro-that the present embodiment technical scheme prepares the exciting light spectrogram of sample, fluorescence spectrum figure, decay of luminescence curve, ESEM
Photo is consistent with the sample of preparation in embodiment 1.
Claims (5)
1. a fluorescent material for white light LED, it is characterised in that: the chemical formula of described material is MgNb2O6: xEu, wherein
X is Eu3+The mole percent of doping, 0.0001≤x≤0.5.
2. the preparation method of a red fluorescence material as claimed in claim 1, it is characterised in that use high temperature solid-state method,
Comprise the steps:
(1) chemical formula MgNb is pressed2O6: the stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing magnesium from
Sub-Mg2+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, grind and mix,
Obtain mixture；
(2) mixture that step (1) obtains being carried out precalcining in air atmosphere, precalcining temperature is 500～900 DEG C, in advance
Calcination time is 2～16 hours；
(3) mixture that step (2) obtains is cooled down naturally, after grinding and mixing, calcine in air atmosphere, forge
Burning temperature is 900～1500 DEG C, and calcination time is 2～16 hours, naturally cools to room temperature, i.e. obtains fluorescent material.
The preparation method of fluorescent material for white light LED the most according to claim 2, it is characterised in that: step (2)
Precalcining temperature be 550～850 DEG C, the precalcining time is 3～12 hours.
The preparation method of fluorescent material for white light LED the most according to claim 2, it is characterised in that: step (3)
Calcining heat be 950～1400 DEG C, calcination time is 2～9 hours.
The preparation method of fluorescent material for white light LED the most according to claim 2, it is characterised in that: described contains
Magnesium ion Mg2+Compound be the one in magnesia, magnesium chloride, magnesium nitrate, basic magnesium carbonate；Described containing niobium ion
Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one；Described contains
There is europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3·6H2O, europium carbonate Eu2(CO3)3In one.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910908A (en) * | 2015-05-08 | 2015-09-16 | 江苏师范大学 | Red fluorescent material for white light LED and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910908A (en) * | 2015-05-08 | 2015-09-16 | 江苏师范大学 | Red fluorescent material for white light LED and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| LI YA ZHOU ET AL.: "Preparation and photoluminescence properties of MgNb2O6:Eu3+, Bi3+ red-emitting phosphor", 《MATERIALS SCIENCE-POLAND》 * |
| 김지선: "다양한 활성제 이온이 치환 고용된 MgNb2O6 형광체의 특성", 《PROCEEDINGS OF THE KOREAN VACUUM SOCIETY CONFERENCE》 * |
| 刘娟 等: "Eu3+，Bi3+共掺杂铌酸镁荧光粉的发光性质", 《广西师范大学学报：自然科学版》 * |
| 周静: "高压下A2+Nb2O6（A2+=Ca、Zn、Mg）的结构转变研究", 《中国博士学位论文全文数据库基础科学辑》 * |
| 莫福旺: "白光LED用Eu3+掺杂红色荧光粉的合成及其发光性质研究", 《中国博士学位论文全文数据库基础科学辑》 * |
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Application publication date: 20160810 |