CN104877675A - Mixed-valence-state europium (Eu) ion doped single-matrix color-adjustable fluorescent powder and preparation method thereof - Google Patents
Mixed-valence-state europium (Eu) ion doped single-matrix color-adjustable fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses mixed-valence-state europium (Eu) ion doped single-matrix color-adjustable fluorescent powder and a preparation method thereof. An expression formula of the chemical composition of the fluorescent powder is Ca2-xEuxSiO2F2, wherein Eu is an active ion, and is in +2 and +3 mixed-valence state; x is a molar percentage coefficient accounted by the active ion Eu relative to an alkaline earth metal ion Ca, and x is more than or equal to 0.001 and less than or equal to 0.10; according to the fluorescent powder, the active ion Eu is doped into a matrix Ca2SiO2F2, and under the condition that the matrix Ca2SiO2F2 can be effectively activated by near-ultraviolet light, adjustable emission of a fluorescent powder material from blue light to orange red light can be achieved by changing the doping concentration of the active ion Eu and adjusting the emission peak ratio of the blue light of bivalent Eu ions to red light of trivalent Eu ions; and specifically, with the increase of Eu ion doping concentration, the relative strength of red light emission of Eu<3+> can be increased, and the light emitting color of Ca2-xEuxSiO2F2 is gradually changed from blue to white, and is continuously changed to orange.
Description
Technical field
The present invention relates to luminescent material technical field, particularly relate to a kind of mixed valence europium ion-doped single-matrix Color tunable fluorescent material and preparation method thereof.
Background technology
Fluorescent material conversion hysteria white light emitting diode (Phosphor-converted white light-emitting diodes, pc-LEDs) there is high brightness, volume be little, the life-span is long, survivable, easy design, conversion fast and the distinguishing feature such as environmental friendliness, followingly become the lighting source of a new generation by replacing incandescent light, luminescent lamp, sodium vapor lamp etc.Although the method for existing several encapsulation WLEDs so far, near ultraviolet (n-UV) InGaN base chip portfolio three primary colours (red, green and blue) fluorescent material is adopted to be considered to the approach of most convenient.At present, main commercial near ultraviolet InGaN base LEDs fluorescent material is blue powder BaMgAl
10o
17: Eu
2+, green powder ZnS:(Cu
+, Al
3+) and rouge and powder Y
2o
2s:Eu
3+.But these fluorescent material all exist certain shortcoming, there is the defect of the aspect such as colour temperature, display index, luminous efficiency and chemical stability in the WLEDs finally encapsulated.Wherein, blue colour fluorescent powder due to its luminous efficiency low, blue light is easy to, by problems such as red and green emitting phosphor absorptions, affect near ultraviolet excitated three primary colors fluorescent powder luminescent properties, thus white light LEDs performance is reduced.
About the indigo plant that effectively can be excited by near ultraviolet, green, red fluorescence powder are the important directions that people study always.At present, the fluorescent material LaGaO reporting that a kind of similar glow color was adjustable is had
3: xTb
3+, wherein Tb
3+the doping of ion is La
3+the mole number of the 0.01-12% of ion, it is that a kind of glow color can realize fluorescent material adjustable in from blueness to green fields.But this fluorescent material needs the wavelength and the Tb that change excitation light source
3+it is adjustable that the doping of ion realizes glow color.Therefore, be necessary to seek the fluorescent material of the novel blueness that effectively can be excited by 350-410nm near-ultraviolet light to cyan Color tunable.
Silicate substrate luminescent material has good chemical stability and thermostability due to it, becomes the phosphor material powder that a class is important.In addition, silicate fluorescent material production cost is low, and raw material high-purity silicon dioxide is cheap and easy to get, and sintering temperature is also low than other systems such as phosphoric acid salt, aluminate, more favourable to the reduction observable index in building-up process.It is simple that high temperature solid-state method has preparation technology, and easy handling, equipment is easy to get, operational safety, and condition holds manageable advantage.Therefore, design and synthesize and can be used for the glow color adjustable fluorescent powder material that near ultraviolet InGaN chip excites and have broad application prospects.
Disclose a kind of trivalent europium ion doped silicate fluorescent material in prior art, its chemical structure of general formula is MLn
2si
3o
10: mBi
3+, nEu
3+.Wherein M is one or more in Zn, Mg, Ca, Sr, Ba, and Ln is one or more in La, Y; 0≤m≤0.1,0≤n≤0.22.Although element type and the present invention of forming this fluorescent material are similar, still have some significant difference following: (1) this silicate fluorescent powder is different from luminous host of the present invention, the luminous host of this invention is CaLa
2si
3o
10, and luminous host of the present invention is Ca
2siO
2f
7, this is two kinds of diverse substrate materials, and when substrate material is different, the crystalline structure of material is different, and luminous host structure is again the key factor affecting luminosity, learns thus, the luminescence mechanism of the fluorescent material that different substrates material obtains cannot analogy.(2) this invention is by regulating dopant ion Bi
3+and Eu
3+relative concentration, and then regulation and control Bi
3+blue-light-emitting and Eu
3+emitting red light ratio, finally realize glow color adjustable, and the present invention only adulterates a kind of light emitting ionic Eu, component is relatively simple, and synthesis cost is lower, passes through Eu
2+blue-light-emitting and Eu
3+emitting red light ratio to realize glow color adjustable.In sum, the present invention needs to cooperatively interact between described luminous host and mixed valence Eu and could realize adjustable gradually from blue-white-orange of fluorescent material.
Another object of the present invention is to provide the preparation method of above-mentioned fluorescent material, comprises the steps: to take raw material according to the stoichiometric ratio of described fluorescent material chemical constitution expression, and abundant ground and mixed is even; By mixing raw material roasting in reducing atmosphere, then naturally cool to room temperature; Taken out by products therefrom, namely grinding obtains the finished product.
Preferably, described raw material be in europium oxide compound, europium oxalate, europium carbonate or europium nitrate one or more, in calcium carbonate, nitrocalcite or Calcium Fluoride (Fluorspan) one or more, silicon-dioxide and Neutral ammonium fluoride.
In order to make above-mentioned raw materials mutually fully react, generate fluorescent material of the present invention, preferably, described maturing temperature is 800 ~ 1000 DEG C, and roasting time is 4-~ 12 hour.
Preferably, described maturing temperature is 900 DEG C, the fluorescent material inclusion-free prepared.
Preferably, described mixing raw material is at H
2or roasting in the reducing atmosphere of CO.
Compared with prior art, beneficial effect of the present invention is: described fluorescent material is doped in matrix Ca by active ions Eu
2siO
2f
2in, effectively can be excited down by near-ultraviolet light, and by changing the doping content of active ions Eu, regulate the blue light of divalent europium and the emission peak ratio of trivalent europium ion red light, and then it be adjustable from blue light to orange light emission to realize phosphor material powder.Concrete, along with the increase of Eu ion doping concentration, Eu
3+the relative intensity of emitting red light increases, Ca
2-
x eu
x siO
2f
2glow color taper to white by blueness, and continue to change to orange.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of Color tunable fluorescent material, mixed valence ion Eu can be regulated by regulating the doping content of active ions Eu
3+and Eu
2+luminous strength ratio, realize adjustable gradually from blue-white-orange of fluorescent material.
The present invention also provides the preparation method of described fluorescent material.
Above-mentioned purpose of the present invention is achieved by the following technical programs.
A kind of mixed valence europium ion-doped single-matrix Color tunable fluorescent material, it is characterized in that, the chemical constitution expression of described fluorescent material is: Ca
2-
x eu
x siO
2f
2; Wherein, Eu is active ions, is+2 ,+3 mixed valences;
xfor the molar percentage coefficient that the relative alkaline-earth metal ions Ca of active ions Eu accounts for, 0.001≤x≤0.10.
The substrate material of fluorescent material of the present invention is Ca
2siO
2f
2, the Eu of mixed valence is active ions,
xfor the relative alkaline-earth metal ions Ca of active ions Eu
2+the molar percentage coefficient accounted for.Substrate material Ca of the present invention
2siO
2f
2can obtain efficiently exciting of near-ultraviolet light, luminescence center is bivalent rare earth europium ion (Eu
2+) and trivalent rare earth europium ion (Eu
3+), wherein, Eu
2+turn blue coloured light, Eu
3+burn red.Under near ultraviolet excitation, along with the increase of Eu ion doping concentration, Eu
3+and Eu
2+luminous strength ratio increase, Ca
2-
x eu
x siO
2f
2glow color taper to white by blueness, and continue to change to orange.Concrete, work as x=0.001, i.e. the relative Ca of Eu
2+when the molar percentage coefficient accounted for is 0.01, fluorescent material consists of Ca
1.999eu
0.001siO
2f
2, now Eu
2+more, under near ultraviolet excitation, send more weak blue light; When x=0.01, i.e. the relative Ca of Eu
2+when the molar percentage coefficient accounted for is 0.01, fluorescent material consists of Ca
1.99eu
0.01siO
2f
2, now Eu
2+more, under near ultraviolet excitation, send stronger blue light; When Eu ion doping concentration is increased to x=0.05, i.e. the relative Ca of Eu
2+when the molar percentage coefficient accounted for is 0.05, fluorescent material consists of Ca
1.95eu
0.05si
2o
2f
2, Eu
2+/ Eu
3+ratio reduce, under near ultraviolet excitation, send stronger white light; When Eu ion doping concentration is increased to x=0.10 further, i.e. the relative Ca of Eu
2+when the molar percentage coefficient accounted for is 0.10, fluorescent material consists of Ca
1.90eu
0.10siO
2f
2, Eu
3+/ Eu
2+ratio reduce, now Eu
3+more, under near ultraviolet excitation, send stronger orange red light.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction figure of embodiment 1 phosphor material powder.
Fig. 2 is the excitation spectrum of embodiment 1 phosphor material powder under monitoring 472nm launches.
Fig. 3 is the emmission spectrum of embodiment 1-5 phosphor material powder under 355nm near ultraviolet excitation.
Fig. 4 is the chromaticity coordinates figure of embodiment 1-5 phosphor material powder.
Caption (Fig. 3-4): a-embodiment 1 fluorescent material, b-embodiment 2 fluorescent material, c-embodiment 3 fluorescent material, d-embodiment 4 fluorescent material, e-embodiment 5 fluorescent material.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the present invention is described in further details, but embodiment does not limit in any form the present invention.Unless stated otherwise, the present invention adopts reagent, method and apparatus are the art conventional reagent, method and apparatus.
embodiment 1
Take europium sesquioxide (Eu
2o
3) 0.0176g, calcium carbonate (CaCO
3) 1.9918g, silicon-dioxide (SiO
2) 0.6008g, Neutral ammonium fluoride (NH
4f) 0.7408g fully grind and after mixing, roasting in Carbon monoxide reduction atmosphere, at 900 DEG C, sintering 6 hours, naturally cools to room temperature in agate mortar.By sample take out grinding, finally obtain product, phosphor material powder consist of: Ca
1.99eu
0.01siO
2f
2.
The diffraction peak position of gained phosphor material powder is consistent with crystallographic data storehouse PDF#19-1131, illustrative material structure and matrix Ca
2siO
2f
2unanimously, Fig. 1 is seen.Fig. 2 is the excitation spectrum of the present embodiment material, and as can be seen from Figure 2, phosphor material powder of the present invention effectively can be excited by 320nm-420nm near-ultraviolet light.The present embodiment phosphor material powder sends stronger blue emission broadband (470 nm) and weak red emission razor-edge (565-640 nm) under 355nm near ultraviolet excitation, sees accompanying drawing 3-a; Chromaticity coordinates is (0.182,0.160), sees accompanying drawing 4-a.
embodiment 2
Take europium sesquioxide (Eu
2o
3) 0.0528g, calcium carbonate (CaCO
3) 1.9717g, silicon-dioxide (SiO
2) 0.6008g, Neutral ammonium fluoride (NH
4f) 0.7408g fully grind and after mixing, roasting in Carbon monoxide reduction atmosphere, at 900 DEG C, sintering 6 hours, naturally cools to room temperature in agate mortar.By sample take out grinding, finally obtain product, phosphor material powder consist of: Ca
1.99eu
0.03siO
2f
2.
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu
3+red emission razor-edge and divalence Eu
2+blue emission broadband strength ratio increase, see accompanying drawing 3-b; Chromaticity coordinates is (0.277,0.199), sees accompanying drawing 4-b.
embodiment 3
Take europium sesquioxide (Eu
2o
3) 0.0880g, calcium carbonate (CaCO
3) 1.9518g, silicon-dioxide (SiO
2) 0.6008, Neutral ammonium fluoride (NH
4f) 0.7408g fully grind and after mixing, roasting in Carbon monoxide reduction atmosphere, at 900 DEG C, sintering 6 hours, naturally cools to room temperature in agate mortar.By sample take out grinding, finally obtain product, phosphor material powder consist of: Ca
1.99eu
0.05siO
2f
2.
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu
3+red emission razor-edge and divalence Eu
2+blue emission broadband strength ratio continue to increase, see accompanying drawing 3-c; Chromaticity coordinates is (0.337,0.235), sees accompanying drawing 4-c.
embodiment 4
Take europium sesquioxide (Eu
2o
3) 0.1231g, calcium carbonate (CaCO
3) 1.9317g, silicon-dioxide (SiO
2) 0.6008g, Neutral ammonium fluoride (NH
4f) 0.7408g fully grind and after mixing, roasting in Carbon monoxide reduction atmosphere, at 900 DEG C, sintering 6 hours, naturally cools to room temperature in agate mortar.By sample take out grinding, finally obtain product, phosphor material powder consist of: Ca
1.99eu
0.07siO
2f
2.
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu
3+red emission razor-edge and divalence Eu
2+blue emission broadband strength ratio continue to increase, see accompanying drawing 3-d.Chromaticity coordinates is (0.414,0.281), sees accompanying drawing 4-d.
embodiment 5
Take europium sesquioxide (Eu
2o
3) 0.1760g, calcium carbonate (CaCO
3) 1.9017g, silicon-dioxide (SiO
2) 0.6008g, Neutral ammonium fluoride (NH
4f) 0.7408g fully grind and after mixing, roasting in Carbon monoxide reduction atmosphere, at 900 DEG C, sintering 6 hours, naturally cools to room temperature in agate mortar.By sample take out grinding, finally obtain product, phosphor material powder consist of: Ca
1.99eu
0.10siO
2f
2.
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu
3+red emission razor-edge and divalence Eu
2+blue emission broadband strength ratio continue to increase, see accompanying drawing 3-e.Chromaticity coordinates is (0.474,0.318), sees accompanying drawing 4-e.
Comprehensive above-described embodiment result is visible, under near ultraviolet excitation, along with the increase of Eu ion doping concentration, and trivalent Eu
3+red emission razor-edge and divalence Eu
2+the wide strength ratio of blue emission increase gradually, Ca
2-xeu
x siO
2f
2glow color to be gradually changed white by blueness, finally change to orange.
Claims (5)
1. a mixed valence europium ion-doped single-matrix Color tunable fluorescent material, is characterized in that, the chemical constitution expression of described fluorescent material is: Ca
2-
x eu
x siO
2f
2; Wherein, Eu is active ions, is+2 ,+3 mixed valences;
xfor the molar percentage coefficient that the relative alkaline-earth metal ions Ca of active ions Eu accounts for, 0.001≤x≤0.10.
2. a preparation method for fluorescent material described in claim 1, is characterized in that, comprises the steps: to take raw material according to the stoichiometric ratio of described fluorescent material chemical constitution expression, and abundant ground and mixed is even; By mixing raw material roasting in reducing atmosphere, then naturally cool to room temperature; Taken out by products therefrom, namely grinding obtains the finished product.
3. preparation method according to claim 2, it is characterized in that, described raw material be in europium oxide compound, europium oxalate, europium carbonate or europium nitrate one or more, in calcium carbonate, nitrocalcite or Calcium Fluoride (Fluorspan) one or more, silicon-dioxide and Neutral ammonium fluoride.
4. preparation method according to claim 2, is characterized in that, described maturing temperature is 800 ~ 1000 DEG C, and roasting time is 4-~ 12 hour.
5. preparation method according to claim 3, is characterized in that, described maturing temperature is 900 DEG C.
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| CN106118637A (en) * | 2016-06-27 | 2016-11-16 | 东台市天源荧光材料有限公司 | A kind of fluosilicate red fluorescence powder and preparation method thereof |
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| CN111088048A (en) * | 2019-12-27 | 2020-05-01 | 江苏师范大学 | Eu (Eu)3+Doped fluorotantalate fluorescent ceramic and synthetic method and application thereof |
| CN111607397A (en) * | 2020-05-27 | 2020-09-01 | 杭州电子科技大学 | Eu (Eu)2+-Eu3+Co-doped silicate fluorescent powder and preparation method and application thereof |
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| CN111607397B (en) * | 2020-05-27 | 2023-03-21 | 杭州电子科技大学 | Eu (Eu) 2+ -Eu 3+ Co-doped silicate fluorescent powder and preparation method and application thereof |
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