CN103694999A - Europium ion activated phosphate red fluorescent powder and preparation method thereof - Google Patents
Europium ion activated phosphate red fluorescent powder and preparation method thereof Download PDFInfo
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- CN103694999A CN103694999A CN201410012061.XA CN201410012061A CN103694999A CN 103694999 A CN103694999 A CN 103694999A CN 201410012061 A CN201410012061 A CN 201410012061A CN 103694999 A CN103694999 A CN 103694999A
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Abstract
The invention belongs to the technical field of rare-earth luminous materials, and relates to europium ion activated phosphate red fluorescent powder and a preparation method thereof. The red fluorescent powder is sodium aluminum phosphate doped with rare-earth ion Eu<3+>, and the chemical composition is represented by the following chemical formula: Na3Al2(1-x)(PO4)3:2xEu<3+>, wherein 0.001<=x<=0.06, Na3Al2(1-x)(PO4)3 is a matrix, and Eu<3+> is the doping rare-earth ion. In the invention, the phosphate red fluorescent powder Na3Al2(1-x)(PO4)3:2xEu<3+> is synthesized by a combustion method; under the excitation of near ultraviolet, the red fluorescent powder has strong absorbability within the excitation wavelength of 220-300nm, and the main peak of the transmitted light is 575-625m; moreover, the red fluorescent powder has high luminous efficiency and stable chemical properties, is in an orange red band and can be applied to a high-color rendering white light LED (light emitting diode). The preparation method is simple and easy to operate, saves energy and time and has a great application prospect in the field of solid illumination.
Description
Technical field
The present invention relates to a kind of europium ion activated phosphate red fluorescence powder and preparation method thereof, particularly a kind of fluorescent material of launching red fluorescence under near ultraviolet excitation, it can be applicable to, in ultraviolet-near ultraviolet type white light LEDs, belong to fluorescent material technical field.
Background technology
White light emitting diode (LED) be called as the 4th generation lighting source, as solid light source of new generation, the shortcomings such as the energy consumption that traditional incandescent light and luminescent lamp exist is high, frangible except overcoming, pollution, also have that volume is little, environmental protection, speed of response is fast, the life-span is long, can planar package, luminous intensity high, efficient, energy-conservation, vibration resistance, low voltage drive and can not cause environmental pollution etc. to have advantage.Therefore in fields such as demonstration, background light source, signal lamp, illuminations, be widely used.Particularly in recent years, along with developing rapidly of blueness, purple and ultraviolet LED, make white light LEDs have very large application prospect at lighting field, be acknowledged as the green illumination light source of current replace fluorescent lamps and incandescent light.
At present, the form of acquisition white light LEDs mainly contains two kinds: a kind of is by three kinds of LED chip combination results white lights of red, green, blue; Another kind is to use UV-light, near-ultraviolet light or blue-light LED chip to add yellow fluorescent powder, and the two light sending is mixed to form white light, the blue-light excited YAG:Ce that wherein GaN base chip is launched
3+fluorescent material is with the fastest developing speed, has realized marketization application.This method is that application is also the most ripe at most at present, but shortcoming is fairly obvious, and major cause is the white light that blue chip and gold-tinted two primary colours are compounded to form, and has lacked red composition, so colour rendering index is on the low side.Current business is Y for the red fluorescence powder of GaN base ultraviolet or blue chip
2o
2s:Eu
3+yet 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 intensity.This external near ultraviolet or blue-light excited lower red fluorescence powder Y
2o
2s:Eu
3+chemical property is unstable, and sulfide easily decomposes.These deficiencies of red fluorescence powder have become the bottleneck that improves white light LEDs development.Therefore the red fluorescent powder for white radiation LED that exploitation can effectively be excited by near-ultraviolet light becomes the focus of current research and urgent task.
The advantages such as phosphoric acid salt is a kind of traditional phosphor host, and it has high stable performance, and the cheap and preparation technology of raw materials cost is simple, phosphate phosphor is one of fluorescent material of excellent property.Therefore, use phosphate radical is base starting material, development of new phosphate radical base red fluorescent powder become the focus of domestic and international research.But the material of preparing at present aluminum phosphate sodium salt red fluorescence powder is seldom reported.
In addition, different preparation methods causes fluorescent material to have different performances, thereby can produce significantly impact to the luminescent properties of fluorescent material.For example, adopt the fluorescent material of the synthetic phosphate system of high temperature solid phase synthesis, its temperature of reaction is high, preparation time is grown, experimental installation is had relatively high expectations, because at high temperature reaction easily produces agglomeration, the particle size were obtaining is large, need ball milling, can have a strong impact on luminosity and the performance of fluorescent material.And coprecipitation method requires each component to have identical or close hydrolysis, deposition condition, condition is wayward and yield poorly, and luminous intensity and the efficiency of powder are lower.Therefore, selecting the suitable method of preparing fluorescent material is also urgent problem in the art.
Summary of the invention
The problem of technology to be solved by this invention is, this red fluorescence powder, under the exciting of near-ultraviolet light, has strong absorption within the scope of 220～300nm, and the main peak of launching that it excites is positioned at 575～625nm scope.
Further, another technical problem to be solved by this invention is that a kind of novel preparation method of above-mentioned red fluorescence powder is provided.The simple easy handling of the method, the reaction times is short, sintering temperature is low and the light-emitting phosphor intensity of preparation is high, stable chemical nature, and powder particle is evenly distributed, particle diameter is little etc.
The present invention gos deep into, at length research, by controlling the factors such as chemical constitution, proportioning raw materials, has solved above-mentioned technical problem.Concrete scheme is as follows:
A kind of europium ion activated phosphate red fluorescence powder provided by the invention and preparation method thereof, its chemical composition can be by following chemical formulation: Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+, 0.001≤x≤0.06 wherein, Na
3al
2 (1-x)(PO
4)
3matrix, Eu
3+it is the rare earth ion mixing.Comprise the following steps:
1. according to chemical general formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+calculate respectively, take reaction reagent Eu (NO
3)
3, A.R., A.R. represents analytical pure, Al
2(NO
3)
2, A.R., NaNO
3, A.R., NH
4h
2(PO
4), A.R., NH
4(NO
3), A.R.;
2. the Al 1. taking with deionized water dissolving step
2(NO
3)
2, NaNO
3and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
3. by Eu (NO
3)
3solion and above-mentioned steps 2. resulting solution phase are mixed, and stir about 30 minutes;
4. to the 3. resulting mixing solutions that contains rare earth ion of above-mentioned steps, then add therein urea, stir 30 minutes, obtain being mixed with the mixing solutions of urea, mixing solutions is placed in to crucible; The retort furnace that crucible is placed in, is warming up to 550-650 ℃, obtains the presoma of white loose porous;
The presoma of the white loose porous 5. above-mentioned steps being obtained in is 4. heat-treated 2～8 hours at 900 ℃ of left and right temperature, obtains phosphate red fluorescent powder.
The preparation method of described a kind of europium ion activated phosphate red fluorescence powder, is characterized in that: the step speed that 5. middle sintering temperature raises is 10 ℃/min.
The preparation method of described a kind of europium ion activated phosphate red fluorescence powder, is characterized in that: fluorescent material medium particle diameter is 0.1～0.5 micron.
The preparation method of described a kind of europium ion activated phosphate red fluorescence powder, is characterized in that: the solubility promoter of step described in is 2. NH
4(NO
3).
The invention has the beneficial effects as follows:
Compared with prior art, technical scheme advantage of the present invention is:
1, the substrate material that technical solution of the present invention provides, is easy to realize the reduction of trivalent rare earth ions, and trivalent rare earth ions can stable existence in this matrix, is difficult for deliquescence.
2, the phosphoric acid salt Na in technical solution of the present invention
3al
2 (1-x)(PO
4)
3: 2xEu
3+(wherein 0.001≤x≤0.05) red fluorescence material has wider excitation area, excites main peak at 243nm, the ruddiness that the main peak of launching under near ultraviolet excitation is 615nm.
3, compare with commercial red fluorescence powder, the preparation process of substrate material of the present invention is simple, and product is easy to get, and without waste water and gas discharge, environmental protection, is applicable to serialization and produces.
4, the fluorescent material that the present invention obtains, in the very strong red light of near ultraviolet excitated lower transmitting, has good thermostability, color developing and granularity, and it can be satisfied with the application of near ultraviolet white light LEDs preferably.The invention provides the preparation method of this fluorescent material, its step is simple, easy handling simultaneously.
Accompanying drawing explanation
Fluorescent material sample prepared by Fig. 1 the present invention is the exciting light spectrogram that 615nm obtains at monitoring wavelength.
Fluorescent material sample prepared by Fig. 2 the present invention excites lower doping different concns Eu near ultraviolet 243nm
3+luminescent spectrum figure.
Fluorescent material sample doping different concns Eu prepared by Fig. 3 the present invention
3+luminous intensity figure.
Embodiment
Describe various preferred embodiment of the present invention below in detail.But the present invention is not limited to these concrete preferred embodiments.
According to the preferred embodiments of the invention, a kind of europium ion activated phosphate of the present invention red fluorescence powder, its chemical composition can be by following chemical formulation: Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+, 0.001≤x≤0.05 wherein, Na
3al
2 (1-x)(PO
4)
3matrix, Eu
3+it is the rare earth ion mixing.Further, the amount x of rare-earth metal doped europium ion can be 0.002,0.005,0.01,0.02.Described phosphate red fluorescent powder consists of Na
3al
1.996(PO
4)
3: 0.004Eu
3+, Na
3al
1.99(PO
4)
3: 0.01Eu
3+, Na
3al
1.98(PO
4)
3: 0.02Eu
3+na
3al
1.96(PO
4)
3: 0.04Eu
3+.
Specific embodiment of the invention scheme is described below with reference to accompanying drawings.It is evident that for the person of ordinary skill of the art: in the situation that not deviating from the spirit and scope of the invention, can therefrom carry out various modifications and variations.Thereby improvement of the present invention and the variation within the scope in claims and equivalent thereof contained in the present invention.
Embodiment 1:Na
3al
1.996(PO
4)
3: 0.004Eu
3+preparation
First, by chemical formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+stoichiometric ratio take reaction raw materials Eu (NO
3)
3, Al
2(NO
3)
2, NaNO
3, NH
4h
2(PO
4) mol ratio be 0.004: 0.998: 3: 3; Then with the above-mentioned Al taking of deionized water dissolving
2(NO
3)
2, NaNO
3and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
By Eu (NO
3)
3solution mixes mutually with mixed ion solutions, and induction stirring 5 minutes; Then add urea, continue electric stir about 5 minutes, obtain the mixing solutions containing rare earth metal europium ion.Mixing solutions containing rare earth metal europium ion is poured in crucible; Crucible is placed in to the retort furnace of 550～650 ℃, obtains the presoma of white loose porous; Presoma is heat-treated 2～4 hours at the temperature of 900 ℃ of left and right, obtain described phosphate red fluorescent powder.
Embodiment 2:Na
3al
1.99(PO
4)
3: 0.01Eu
3+preparation
First, by chemical formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+stoichiometric ratio take reaction raw materials Eu (NO
3)
3, Al
2(NO
3)
2, NaNO
3, NH
4h
2(PO
4) mol ratio be 0.01: 0.995: 3: 3; Then with the above-mentioned Al taking of deionized water dissolving
2(NO
3)
2, NaNO
3, and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
By Eu (NO
3)
3solution mixes mutually with mixed ion solutions, and induction stirring 5 minutes; Then add urea, continue electric stir about 5 minutes, obtain the mixing solutions containing rare earth metal europium ion.Mixing solutions containing rare earth metal europium ion is poured in crucible; Crucible is placed in to the retort furnace of 550～650 ℃, obtains the presoma of white loose porous; Presoma is heat-treated 2～4 hours at the temperature of 900 ℃ of left and right, obtain described phosphate red fluorescent powder.
Embodiment 3:Na
3al
1.98(PO
4)
3: 0.02Eu
3+preparation
First, by chemical formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+stoichiometric ratio take reaction raw materials Eu (NO
3)
3, Al
2(NO
3)
2, NaNO
3, NH
4h
2(PO
4) mol ratio be 0.02: 0.99: 3: 3; Then with the above-mentioned Al taking of deionized water dissolving
2(NO
3)
2, NaNO
3, and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
By Eu (NO
3)
3solution mixes mutually with mixed ion solutions, and induction stirring 5 minutes; Then add urea, continue electric stir about 5 minutes, obtain the mixing solutions containing rare earth metal europium ion.Mixing solutions containing rare earth metal europium ion is poured in crucible; Crucible is placed in to the retort furnace of 550～650 ℃, obtains the presoma of white loose porous; Presoma is heat-treated 2～4 hours at the temperature of 900 ℃ of left and right, obtain described phosphate red fluorescent powder.
Referring to accompanying drawing 1, it be the fluorescent material sample prepared of the present invention is the ultraviolet that obtains of 482nm and the exciting light spectrogram of near ultraviolet region at monitoring wavelength.
Embodiment 4:Na
3al
1.96(PO
4)
3: 0.04Eu
3+preparation
First, by chemical formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+stoichiometric ratio take reaction raw materials Eu (NO
3)
3, Al
2(NO
3)
2, NaNO
3, NH
4h
2(PO
4) mol ratio be 0.04: 0.98: 3: 3; Then with the above-mentioned Al taking of deionized water dissolving
2(NO
3)
2, NaNO
3, and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
By Eu (NO
3)
3solution mixes mutually with mixed ion solutions, and induction stirring 5 minutes; Then add urea, continue electric stir about 5 minutes, obtain the mixing solutions containing rare earth metal europium ion.Mixing solutions containing rare earth metal europium ion is poured in crucible; Crucible is placed in to the retort furnace of 550～650 ℃, obtains the presoma of white loose porous; Presoma is heat-treated 2～4 hours at the temperature of 900 ℃ of left and right, obtain described phosphate red fluorescent powder.
Referring to accompanying drawing 1, it is the fluorescent material sample prepared of the present invention is the ultraviolet that obtains of 615nm and the exciting light spectrogram of near ultraviolet region at monitoring wavelength.
Referring to accompanying drawing 2, it is the trivalent europium ion Eu of the different concns of the embodiment of the present invention 1,2,3 and 4 preparations
3+at Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+in fluorescent material, with UV-light 243nm, excite the luminescent spectrum figure obtaining.By Fig. 2, can be seen, the present invention each different fluorescent powder that provide are provided, and their main center emission wavelengths are about the emitting red light wave band of 615nm, are applicable to the white light LEDs that UV-light is excitation light source.In Fig. 2, curve (1), (2), (3), (4) are respectively the spectral radiation curves of the fluorescent material sample prepared by embodiment 1,2,3 and 4 technical schemes, as seen from Figure 2, along with the energy of trivalent europium ion concentration is large, the luminous intensity of fluorescent material strengthens gradually, work as x=0.01, it is the strongest that luminous intensity reaches substantially, continues to increase trivalent europium ion Eu
3+concentration, luminous intensity keeps faint reducing, this is the result of concentration quenching
Referring to accompanying drawing 3, it is fluorescent material sample doping different concns Eu prepared by the present invention
3+luminous intensity figure, can see more clearly the Strength Changes of accompanying drawing 2.
Claims (5)
1. an europium ion activated phosphate red fluorescence powder, is characterized in that: its moiety is by following chemical formulation: Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+, x span is 0.001～0.06.
2. a kind of europium ion Eu according to claim 1
3+the preparation method of activated phosphate red fluorescence powder, is characterized in that comprising the following steps:
1. according to chemical general formula Na
3al
2 (1-x)(PO
4)
3: 2xEu
3+calculate respectively, take reaction reagent Eu (NO
3)
3, A.R., A.R. represents analytical pure, Al
2(NO
3)
2, A.R., NaNO
3, A.R., NH
4h
2(PO
4), A.R., NH
4(NO
3), A.R.;
2. the Al 1. taking with deionized water dissolving step
2(NO
3)
2, NaNO
3and NH
4h
2(PO
4), and add solubility promoter, obtain the mixing solutions that contains corresponding ion;
3. by Eu (NO
3)
3solion and above-mentioned steps 2. resulting solution phase are mixed, and stir about 30 minutes;
4. to the 3. resulting mixing solutions that contains rare earth ion of above-mentioned steps, then add therein urea, stir 30 minutes, obtain being mixed with the mixing solutions of urea, mixing solutions is placed in to crucible; The retort furnace that crucible is placed in, is warming up to 550-650 ℃, obtains the presoma of white loose porous;
The presoma of the white loose porous 5. above-mentioned steps being obtained in is 4. heat-treated 2～8 hours at 900 ℃ of left and right temperature, obtains phosphate red fluorescent powder.
3. the preparation method of a kind of europium ion activated phosphate red fluorescence powder according to claim 2, is characterized in that: the step speed that 5. middle sintering temperature raises is 10 ℃/min.
4. the preparation method of a kind of europium ion activated phosphate red fluorescence powder according to claim 2, is characterized in that: fluorescent material medium particle diameter is 0.1～0.5 micron.
5. the preparation method of a kind of europium ion activated phosphate red fluorescence powder according to claim 2, is characterized in that: the solubility promoter of step described in is 2. NH
4(NO
3).
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640505A (en) * | 2018-08-22 | 2018-10-12 | 大连工业大学 | Europium adulterates the preparation method of fluorophosphate red fluorescence glass |
| CN109266345A (en) * | 2018-10-29 | 2019-01-25 | 江苏师范大学 | A kind of single matrix phosphate white emitting fluorescent powder of rare earth ion codope and preparation method thereof |
| CN110615613A (en) * | 2019-07-01 | 2019-12-27 | 上海大学 | Red light compensation fluorescent glass ceramic, preparation method thereof and application thereof in white light LED device |
| CN111138185A (en) * | 2019-12-27 | 2020-05-12 | 江苏师范大学 | Eu (Eu)3+Ion activated aluminum phosphate fluorescent ceramic and preparation method and application thereof |
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|---|---|---|---|---|
| CN101768444A (en) * | 2008-12-31 | 2010-07-07 | 北京有色金属研究总院 | Phosphate green emitting phosphor and preparation method thereof |
| JP2013177523A (en) * | 2012-02-29 | 2013-09-09 | Niigata Univ | Phosphate fluorescent substance |
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2014
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| CN101768444A (en) * | 2008-12-31 | 2010-07-07 | 北京有色金属研究总院 | Phosphate green emitting phosphor and preparation method thereof |
| JP2013177523A (en) * | 2012-02-29 | 2013-09-09 | Niigata Univ | Phosphate fluorescent substance |
Non-Patent Citations (2)
| Title |
|---|
| I.M. NAGPURE等: "Combustion synthesis and luminescence investigation of Na3Al2(PO4)3:RE(RE=Ce3+, Eu3+ and Mn2+) phosphor", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640505A (en) * | 2018-08-22 | 2018-10-12 | 大连工业大学 | Europium adulterates the preparation method of fluorophosphate red fluorescence glass |
| CN109266345A (en) * | 2018-10-29 | 2019-01-25 | 江苏师范大学 | A kind of single matrix phosphate white emitting fluorescent powder of rare earth ion codope and preparation method thereof |
| CN110615613A (en) * | 2019-07-01 | 2019-12-27 | 上海大学 | Red light compensation fluorescent glass ceramic, preparation method thereof and application thereof in white light LED device |
| CN111138185A (en) * | 2019-12-27 | 2020-05-12 | 江苏师范大学 | Eu (Eu)3+Ion activated aluminum phosphate fluorescent ceramic and preparation method and application thereof |
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Application publication date: 20140402 |