CN104877675B - A kind of mixed valence europium ion-doped single-matrix Color tunable fluorescent material and preparation method thereof - Google Patents
A kind of mixed valence europium ion-doped single-matrix Color tunable fluorescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of mixed valence europium ion-doped single-matrix Color tunable fluorescent material and preparation method thereof.The chemical composition expression of described fluorescent material is: Ca2‑xEuxSiO2F2；Wherein, Eu is active ions, for+2, and+3 mixed valences；X is the molar percentage coefficient that active ions Eu accounts for relative to alkaline-earth metal ions Ca, 0.001≤x≤0.10.Described fluorescent material is doped in substrate Ca by active ions Eu2SiO2F2In, effectively can be excited down by black light, and by changing the doping content of active ions Eu, the blue light of regulation divalent europium and the emission peak ratio of trivalent europium ion red light, and then it is adjustable from blue light to orange light emission to realize phosphor material powder.Concrete, along with the increase of Eu ion doping concentration, Eu3+The relative intensity of emitting red light increases, Ca2‑xEuxSiO2F2Glow color tapered to white by blueness, and continue to change to orange.
Description
Technical field
The present invention relates to luminescent material technical field, particularly relating to a kind of mixed valence europium ion-doped single-matrix color can
Adjust fluorescent material and preparation method thereof.
Background technology
Fluorescent material conversion type white light emitting diode (Phosphor-converted white light-emitting diodes, pc-LEDs)
Have that high brightness, volume be little, life-span length, design survivable, easy, conversion quickly and the distinguishing feature such as environmental friendliness, not
The lighting source of a new generation is become by replacing electric filament lamp, fluorescent lamp, sodium vapor lamp etc..Although existing several encapsulation WLEDs so far
Method, but use near ultraviolet (n-UV) InGaN base chip portfolio three primary colours (red, green and blue) fluorescent material be considered as most convenient
Approach.At present, main commercial near ultraviolet InGaN base LEDs fluorescent material is blue powder BaMgAl10O17:Eu2+, green powder
ZnS:(Cu+,Al3+) and Hydrargyri Oxydum Rubrum Y2O2S:Eu3+.But all there is certain shortcoming in these fluorescent material, the WLEDs finally encapsulated
There is the defect of the aspects such as colour temperature, display index, luminous efficiency and chemical stability.Wherein, blue colour fluorescent powder is luminous due to it
Efficiency is low, and blue light is prone to, by problems such as redness and green emitting phosphor absorptions, affect near ultraviolet excitated three primary colors fluorescent powder photism
Can, so that white light LEDs performance reduces.
The important directions of people's research it is always about the indigo plant that effectively can be excited by near ultraviolet, green, red fluorescence powder.Mesh
Before, had been reported that a kind of similar glow color adjustable fluorescent material LaGaO3:xTb3+, wherein Tb3+The doping of ion
For La3+The molal quantity of the 0.01-12% of ion, it is adjustable in a kind of glow color can realize from blueness to green fields
Fluorescent material.But, this fluorescent material needs to change wavelength and the Tb of excitation source3+The doping of ion realizes glow color
Adjustable.Therefore, it is necessary to seek the novel blueness that effectively can be excited by 350-410nm black light to cyan Color tunable
Fluorescent material.
Silicate substrate luminescent material has good chemical stability and heat stability due to it, becomes a class important
Phosphor material powder.It addition, silicate fluorescent material production cost is low, raw material high-purity silicon dioxide is cheap and easy to get, sintering temperature
Also lower than other systems such as phosphate, aluminate, advantageous to the reduction observable index during synthesis.High temperature solid-state method has
Preparation technology is simple, it is easy to operation, and equipment is easy to get, and operates safety, the advantage that condition is easily controlled.Therefore, design and synthesize
Can be used for the glow color adjustable fluorescent powder material that near ultraviolet InGaN chip excites to have broad application prospects.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of Color tunable fluorescent material, can be by regulation active ions
The doping content of Eu regulates mixed valence ion Eu3+And Eu2+Luminous strength ratio, it is achieved fluorescent material is from blue-white-orange
Color the most adjustable.
The present invention also provides for the preparation method of described fluorescent material.
The 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 characterised in that the change of described fluorescent material
Learning composition expression is: Ca2-xEuxSiO2F2；Wherein, Eu is active ions, for+2, and+3 mixed valences；X for activate from
The molar percentage coefficient that sub-Eu accounts for relative to alkaline-earth metal ions Ca, 0.001≤x≤0.10.
The host material of fluorescent material of the present invention is Ca2SiO2F2, the Eu of mixed valence is active ions, and x is active ions
Eu is relative to alkaline-earth metal ions Ca2+The molar percentage coefficient accounted for.Host material Ca of the present invention2SiO2F2It is obtained in that near ultraviolet
Efficiently exciting of light, the centre of luminescence is bivalent rare earth europium ion (Eu2+) and trivalent rare earth europium ion (Eu3+), wherein, Eu2+
Turn blue coloured light, Eu3+Burn red.Under near ultraviolet excitation, along with the increase of Eu ion doping concentration, Eu3+And Eu2+
Luminous strength ratio increase, Ca2-xEuxSiO2F2Glow color tapered to white by blueness, and continue to change to orange.
Concrete, work as x=0.001, i.e. Eu is relative to Ca2+When the molar percentage coefficient accounted for is 0.01, fluorescent material consists of
Ca1.999Eu0.001SiO2F2, now Eu2+More, under near ultraviolet excitation, send more weak blue light；Work as x=0.01, i.e. Eu
Ca relatively2+When the molar percentage coefficient accounted for is 0.01, fluorescent material consists of Ca1.99Eu0.01SiO2F2, now Eu2+It is more,
Stronger blue light is sent under near ultraviolet excitation；When Eu ion doping concentration increases to x=0.05, and i.e. Eu is relative to Ca2+Account for
Molar percentage coefficient when being 0.05, fluorescent material consists of Ca1.95Eu0.05Si2O2F2, Eu2+/Eu3+Ratio reduce, closely
Stronger white light is sent under ultraviolet excitation；When Eu ion doping concentration is further increased to x=0.10, and i.e. Eu is relative to Ca2+
When the molar percentage coefficient accounted for is 0.10, fluorescent material consists of Ca1.90Eu0.10SiO2F2, Eu3+/Eu2+Ratio reduce, this
Time Eu3+More, under near ultraviolet excitation, send stronger orange red light.
Disclosing a kind of trivalent europium ion doped silicate fluorescent material in prior art, its chemical structure of general formula is
MLn2Si3O10: mBi3+, nEu3+.One or more during wherein M is Zn, Mg, Ca, Sr, Ba, Ln be La,
One or more in Y；0≤m≤0.1,0≤n≤0.22.Although, form the element type of this fluorescent material and class of the present invention
Seemingly, but, still there is some significant difference following: (1) this silicate fluorescent powder is different from the luminous host of the present invention, this
Bright luminous host is CaLa2Si3O10, and the substrate of the luminescent material of the present invention is Ca2SiO2F2, this be two kinds entirely different
Host material, and when host material difference, the crystal structure of material is different, and luminous host structure is again that impact is sent out
The key factor of light property, it follows that the luminescence mechanism of fluorescent material that different substrates material prepares cannot analogy.(2)
This invention is by regulation dopant ion Bi3+And Eu3+Relative concentration, and then regulation and control Bi3+Blue-light-emitting and Eu3+Redness send out
Light ratio, finally realizes glow color adjustable, and the present invention only adulterates a kind of light emitting ionic Eu, and component is relatively easy, synthesizes into
This is lower, passes through Eu2+Blue-light-emitting and Eu3+Emitting red light ratio to realize glow color adjustable.In sum, the present invention
Needing cooperates between described luminous host and mixed valence Eu could realize fluorescent material from blue-white-orange gradually may be used
Adjust.
It is a further object to provide the preparation method of above-mentioned fluorescent material, comprise the steps: according to described fluorescent material
The stoichiometric proportion of chemical composition expression weighs raw material, is fully ground mix homogeneously；Raw material roasting in reducing atmosphere will be mixed,
Then room temperature is naturally cooled to；Products therefrom is taken out, grinds and i.e. obtain final products.
Preferably, described raw material be one or more in europium oxide, europium oxalates, europium carbonate or europium nitrate,
In calcium carbonate, calcium nitrate or calcium fluoride one or more, silicon dioxide and ammonium fluoride.
In order to make above-mentioned raw materials the most fully react, generate fluorescent material of the present invention, it is preferred that described sintering temperature is
800～1000 DEG C, roasting time is 4～12 hours.
Preferably, described sintering temperature is 900 DEG C, the fluorescent material free from admixture prepared.
Preferably, described mixing raw material is at H2Or roasting in the reducing atmosphere of CO.
Compared with prior art, the present invention has the beneficial effects that: described fluorescent material is doped in substrate by active ions Eu
Ca2SiO2F2In, can effectively be excited down by black light, and by changing the doping content of active ions Eu, regulate bivalence
The blue light of europium ion and the emission peak ratio of trivalent europium ion red light, and then realize phosphor material powder from blue light to orange red
Light emission is adjustable.Concrete, along with the increase of Eu ion doping concentration, Eu3+The relative intensity of emitting red light increases, Ca2- xEuxSiO2F2Glow color tapered to white by blueness, and continue to change to orange.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction figure of embodiment 1 phosphor material powder.
Fig. 2 is embodiment 1 phosphor material powder excitation spectrum under monitoring 472nm launches.
Fig. 3 is embodiment 1-5 phosphor material powder emission spectrum 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-implements
Example 4 fluorescent material, e-embodiment 5 fluorescent material.
Detailed description of the invention
Below in conjunction with Figure of description and specific embodiment, the present invention is described in further details, but the present invention is not done by embodiment
Any type of restriction.Unless stated otherwise, the present invention use reagent, method and apparatus be the art conventional reagent,
Method and apparatus.
Embodiment 1
Weigh europium oxide (Eu2O3) 0.0176g, calcium carbonate (CaCO3) 1.9918g, silicon dioxide (SiO2) 0.6008g, fluorination
Ammonium (NH4F) 0.7408g is fully ground and after mix homogeneously in agate mortar, roasting in Carbon monoxide reduction atmosphere, 900 DEG C
Lower sintering 6 hours, naturally cools to room temperature.By sample take out grind, finally give product, phosphor material powder consist of:
Ca1.99Eu0.01SiO2F2。
The diffraction maximum position of gained phosphor material powder is consistent with crystallographic data storehouse PDF#19-1131, illustrative material structure and
Substrate Ca2SiO2F2Unanimously, Fig. 1 is seen.Fig. 2 is the excitation spectrum of the present embodiment material, figure it is seen that the present invention
Phosphor material powder effectively can be excited by 320nm-420nm black light.The present embodiment phosphor material powder is in 355nm near ultraviolet
Light excites down and sends stronger blue emission broadband (470nm) and weak red emission razor-edge (565-640nm), sees accompanying drawing 3-a；
Chromaticity coordinates is (0.182,0.160), sees accompanying drawing 4-a.
Embodiment 2
Weigh europium oxide (Eu2O3) 0.0528g, calcium carbonate (CaCO3) 1.9717g, silicon dioxide (SiO2) 0.6008g, fluorination
Ammonium (NH4F) 0.7408g is fully ground and after mix homogeneously in agate mortar, roasting in Carbon monoxide reduction atmosphere, 900 DEG C
Lower sintering 6 hours, naturally cools to room temperature.By sample take out grind, finally give product, phosphor material powder consist of:
Ca1.99Eu0.03SiO2F2。
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu3+Red emission razor-edge and bivalence Eu2+'s
Blue emission broadband strength ratio increases, and sees accompanying drawing 3-b；Chromaticity coordinates is (0.277,0.199), sees accompanying drawing 4-b.
Embodiment 3
Weigh europium oxide (Eu2O3) 0.0880g, calcium carbonate (CaCO3) 1.9518g, silicon dioxide (SiO2) 0.6008, fluorination
Ammonium (NH4F) 0.7408g is fully ground and after mix homogeneously in agate mortar, roasting in Carbon monoxide reduction atmosphere, 900 DEG C
Lower sintering 6 hours, naturally cools to room temperature.By sample take out grind, finally give product, phosphor material powder consist of:
Ca1.99Eu0.05SiO2F2。
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu3+Red emission razor-edge and bivalence Eu2+'s
Blue emission broadband strength ratio continues to increase, and sees accompanying drawing 3-c；Chromaticity coordinates is (0.337,0.235), sees accompanying drawing 4-c.
Embodiment 4
Weigh europium oxide (Eu2O3) 0.1231g, calcium carbonate (CaCO3) 1.9317g, silicon dioxide (SiO2) 0.6008g, fluorination
Ammonium (NH4F) 0.7408g is fully ground and after mix homogeneously in agate mortar, roasting in Carbon monoxide reduction atmosphere, 900 DEG C
Lower sintering 6 hours, naturally cools to room temperature.By sample take out grind, finally give product, phosphor material powder consist of:
Ca1.99Eu0.07SiO2F2。
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu3+Red emission razor-edge and bivalence Eu2+'s
Blue emission broadband strength ratio continues to increase, and sees accompanying drawing 3-d.Chromaticity coordinates is (0.414,0.281), sees accompanying drawing 4-d.
Embodiment 5
Weigh europium oxide (Eu2O3) 0.1760g, calcium carbonate (CaCO3) 1.9017g, silicon dioxide (SiO2) 0.6008g, fluorination
Ammonium (NH4F) 0.7408g is fully ground and after mix homogeneously in agate mortar, roasting in Carbon monoxide reduction atmosphere, 900 DEG C
Lower sintering 6 hours, naturally cools to room temperature.By sample take out grind, finally give product, phosphor material powder consist of:
Ca1.99Eu0.10SiO2F2。
Phosphor material powder of the present invention under 355nm near ultraviolet excitation, trivalent Eu3+Red emission razor-edge and bivalence Eu2+'s
Blue emission broadband strength ratio continues to increase, and sees accompanying drawing 3-e.Chromaticity coordinates is (0.474,0.318), sees accompanying drawing 4-e.
Summary embodiment result is visible, under near ultraviolet excitation, along with the increase of Eu ion doping concentration, trivalent
Eu3+Red emission razor-edge and bivalence Eu2+Blue emission width strength ratio be gradually increased, Ca2-xEuxSiO2F2Glow color by
Blueness gradually changes white, finally changes to orange.
Claims (5)
1. a mixed valence europium ion-doped single-matrix Color tunable fluorescent material, it is characterised in that the chemical composition expression of described fluorescent material is: Ca2-xEuxSiO2F2；Wherein, Eu is active ions, for+2 ,+3 mixed valences；X is the molar percentage coefficient that active ions Eu accounts for relative to alkaline-earth metal ions Ca,
0.001≤x≤0.10。
2. the preparation method of fluorescent material described in a claim 1, it is characterised in that comprise the steps: to weigh raw material according to the stoichiometric proportion of described fluorescent material chemical composition expression, be fully ground mix homogeneously；Raw material roasting in reducing atmosphere will be mixed, then naturally cool to room temperature；Products therefrom is taken out, grinds and i.e. obtain final products.
Preparation method the most according to claim 2, it is characterised in that described raw material is one or more in europium oxide, europium oxalates, europium carbonate or europium nitrate, one or more in calcium carbonate, calcium nitrate or calcium fluoride, silicon dioxide and ammonium fluoride.
Preparation method the most according to claim 2, it is characterised in that described sintering temperature is 800～1000 DEG C, roasting time is 4～12 hours.
Preparation method the most according to claim 3, it is characterised in that described sintering 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 |
| CN105950139A (en) * | 2016-06-29 | 2016-09-21 | 东台市天源荧光材料有限公司 | Manganese ion activated fluorosilicate red fluorescent powder and preparation method thereof |
| CN109609128A (en) * | 2018-12-29 | 2019-04-12 | 上海应用技术大学 | A kind of green emitting phosphor and preparation method thereof |
| CN109628084A (en) * | 2018-12-29 | 2019-04-16 | 上海应用技术大学 | A kind of blue colour fluorescent powder and its fast preparation method |
| CN111088048B (en) * | 2019-12-27 | 2022-06-14 | 江苏师范大学 | Eu (Eu)3+Doped fluorotantalate fluorescent ceramic and synthetic method and application thereof |
| 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 |
| CN113174254B (en) * | 2021-04-23 | 2023-02-17 | 宁波萃英化学技术有限公司 | Blue-red light dual-waveband emission fluorescent powder for LED plant light supplementing lamp |
| CN113416543A (en) * | 2021-07-27 | 2021-09-21 | 上海工程技术大学 | Mixed-state europium-activated single-matrix white-light LED fluorescent powder and preparation method thereof |
| CN113773832A (en) * | 2021-10-15 | 2021-12-10 | 烟台布莱特光电材料有限公司 | Fluosilicate red fluorescent powder and preparation method thereof |
| CN115926792B (en) * | 2022-12-12 | 2023-11-10 | 淮北师范大学 | Trivalent europium ion doped fluorescent powder with single matrix and preparation method and application thereof |
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