CN105255491A - Light color adjustable fluorescent material and preparation method thereof - Google Patents

Light color adjustable fluorescent material and preparation method thereof Download PDF

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CN105255491A
CN105255491A CN201510746251.9A CN201510746251A CN105255491A CN 105255491 A CN105255491 A CN 105255491A CN 201510746251 A CN201510746251 A CN 201510746251A CN 105255491 A CN105255491 A CN 105255491A
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fluorescent material
preparation
starting compound
photochromic adjustable
adjustable fluorescent
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CN105255491B (en
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冯垚淼
黄金萍
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Shanghai Normal University
University of Shanghai for Science and Technology
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Shanghai Normal University
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Abstract

The invention relates to a light color adjustable fluorescent material and a preparation method thereof. The chemical expression of the fluorescent material is as follows: A7-x-yB (PO4) 6: xTb<3+>, yEu<3+>, wherein A is selected from one of Ca, Sr or Ba, B is Zr or Ti, the value range of x is (0-0.05), the value range of y is (0-0.05), and the wavelength range of the excitation band of the fluorescent material is 295-500 nm. The preparation method comprises the following steps: (1) weighting raw material compounds respectively containing elements A, B, P, Tb and Eu, so that the molar ratio of A, B, P, Tb and Eu in each raw material compound is (7-x-y):1:6:x:y; and grinding and uniformly mixing the raw material compounds, so that a mixture sample is obtained; and (2) roasting the mixture sample, naturally cooling to room temperature, and grinding the obtained product again, so that the target product fluorescent material is obtained. Compared with the prior art, the light color of the fluorescent material disclosed by the invention can be adjusted from green, warm white to red under the excitation of near ultraviolet/purple light; and the fluorescent material is simple in process, cheap and easily-obtained in raw materials, green and environment-friendly.

Description

A kind of photochromic adjustable fluorescent material and preparation method thereof
Technical field
The present invention relates to rare-earth luminescent material field, especially relate to photochromic adjustable fluorescent material that a kind of near ultraviolet excites to purple LED chip and preparation method thereof.
Background technology
White light LEDs is as the novel all solid state lighting source of one, and due to it, to have the life-span long, and efficiency is high, energy-conservation, environment friendly and pollution-free, the dark attention by people and obtained the support energetically of national governments.Obtain the mode of white light in the market for be combined as master with blue-light LED chip and YAG:Ce.It achieves outstanding progress in Application Areas, but exposes the problem of some keys simultaneously.The maximum deficiency of this combination is that color developing is on the low side, is maximumly only about 85, higher owing to lacking the white light colour temperature that red color components causes being combined into, and makes the LED light colour cast that is assembled into cold, dazzling.
In recent years for current business white light Problems existing, researchist starts fluorescent material sight being turned near ultraviolet or UV LED chip to excite.Near ultraviolet or UV LED chip have higher energy than blue-light LED chip, are more conducive to excitated fluorescent powder; Although good colour rendering index can be reached by the compound of three primary colours, owing to there is " look declines " degree varies between various fluorescent material, cause the photochromic imbalance of compound.Therefore develop a kind of near ultraviolet excitated single-matrix white and photochromic adjustable masstone fluorescent material particularly important.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and the single-matrix white and photochromic adjustable masstone fluorescent material and preparation method thereof that a kind of near ultraviolet excites to purple LED chip is provided.
Object of the present invention can be achieved through the following technical solutions:
A photochromic adjustable fluorescent material, its chemical expression is as follows: A 7-x-yb (PO 4) 6: xTb 3+, yEu 3+; Wherein, A is selected from Ca, the one in Sr or Ba, and B is the span of Zr or Ti, x is (0 ~ 0.05), and the span of y is (0 ~ 0.05), and the excitation band wavelength region of described fluorescent material is 295 ~ 500nm.
A preparation method for photochromic adjustable fluorescent material, comprises the following steps:
(1) starting compound of containing element A, B, P, Tb and Eu is respectively taken, make the elements A in each starting compound: the mol ratio of B:P:Tb:Eu is (7-x-y): 1:6:x:y, and each starting compound ground and mixed is even, obtain blend sample;
(2) by blend sample roasting, be then naturally down to room temperature, again grind and obtain object product fluorescent material.
The starting compound comprising element A is selected from one or more in the carbonate of element A, nitrate, acetate, fluorochemical, muriate or oxide compound, wherein,
When A is Ca, its starting compound be selected from calcium carbonate, Calcium Fluoride (Fluorspan), calcium chloride, calcium oxide, nitrocalcite or calcium acetate one or more;
When A is Sr, its starting compound be selected from Strontium carbonate powder, strontium fluoride, strontium chloride, strontium oxide, strontium nitrate or strontium acetate one or more;
When A is Ba, its starting compound is selected from barium carbonate, barium fluoride, bariumchloride, barium oxide, nitrate of baryta, one or more in barium acetate.
The starting compound comprising B element is selected from oxide compound or the muriate of B element, wherein,
When B is Zr, its compound is zirconium white or zirconium chloride;
When B is Ti, its compound is titanium oxide or titanium tetrachloride.
The starting compound of containing element Tb be selected from Terbium trinitrate, terbium carbonate, terbium sesquioxide, terbium chloride or fluoridize in terbium one or more.
The starting compound of containing element Eu be selected from europium nitrate, Europium trichloride, acetic acid europium, europium carbonate, europium, europium sulfate or europium sesquioxide one or more.
The starting compound of containing element P be selected from Secondary ammonium phosphate or primary ammonium phosphate one or both.
In step (1) during each starting compound grinding, also add dehydrated alcohol and assist grinding, after having ground, dry and obtain blend sample.
The addition of described dehydrated alcohol is 25 ~ 40% of blend sample quality.
In step (2), the maturing temperature of blend sample is more than 1000 DEG C, and roasting time is 2 ~ 4h; Preferably, maturing temperature is 1000 ~ 1300 DEG C.
In fluorescent material of the present invention, A 7b (PO 4) 6as matrix, Tb 3+for sensitizing agent, Eu 3+for activator, by raw material according to a certain ratio, mix.Under hot conditions, through contact between solid phase interface, reaction, nucleation, thus form new crystalline compounds.In synthesis fluorescent material process, under certain temperature of reaction, the proper extension reaction times is conducive to the fluorescence intensity that crystal nucleation is conducive to improving fluorescent material.And the too high quenching of fluorescence that will cause of temperature of reaction, temperature is too low, cannot obtain target product.In the present invention, when singly mixing Eu in matrix 3+or Tb 3+time, fluorescent material, under near ultraviolet excitation, can obtain feature ruddiness or green glow, respectively when mixing Eu altogether in matrix 3+and Tb 3+time, under ultraviolet excitation, due to Eu 3+and Tb 3+between there is transmission ofenergy, Eu 3+and Tb 3+all launch the fluorescence spectrum of its feature, by improving Eu 3+/ Tb 3+ratio, photochromicly can be changed by green glow-warm white-ruddiness, realize photochromic adjustable.
Compared with prior art, the present invention has the following advantages:
1) photochromic regulation range is large: the chemical expression that the present invention obtains is A 7-x-yb (PO 4) 6: xTb 3+, yEu 3+photochromic adjustable fluorescent material, its excitation band wavelength region, at the 290 ~ 500nm of near ultraviolet to purple light, has good matching degree with the near ultraviolet chip on market, meanwhile, by adjusting the doping ratio of rare earth, fixing Tb 3+concentration, increase Eu 3+concentration, the photochromic transformation by green glow-warm white-ruddiness can be obtained, thus the LED light colour cast that is assembled into is warmed up, can not be dazzling;
2) preparation technology of the present invention is simple, and raw material is cheap and easy to get, and reaction process does not have three industrial wastes, has the features such as environmental protection, less energy-consumption, high benefit, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the fluorescent material of embodiments of the invention 1 ~ 4 and embodiment 7;
Fig. 2 is fluorescence excitation and the emmission spectrum of the fluorescent material of embodiments of the invention 5;
Fig. 3 is fluorescence excitation and the emmission spectrum of the fluorescent material of embodiments of the invention 6;
Fig. 4 is fluorescence excitation and the emmission spectrum of the fluorescent material of embodiments of the invention 1;
Fig. 5 is fluorescence excitation and the emmission spectrum of the fluorescent material of embodiments of the invention 1 ~ 5.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.01, y=0.005); The excitation band wavelength region of this fluorescent material is 295 ~ 500nm.
The preparation method of above-mentioned photochromic adjustable fluorescent material, comprises the following steps:
(1) 6.985molSrCO is taken respectively 3, 1molZrO 2, 6mol (NH 4) 2hPO 4, 0.0025molEu 2o 3, 0.005molTb 2o 3, and by after each starting compound mixing, add the dehydrated alcohol of mixture total mass 40%, ground and mixed is even, obtains blend sample;
(2) by blend sample roasting 4h at 1000 DEG C, be then naturally down to room temperature, again grind and obtain object product fluorescent material.
Embodiment 2
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.01, y=0.01); The excitation band wavelength region of this fluorescent material is 295 ~ 500nm.
Its preparation method compared with described in embodiment 1, except Eu 2o 3addition be 0.005mol, SrCO 3addition be outside 6.98mol, all the other are all identical.
Embodiment 3
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.01, y=0.015); The excitation band wavelength region of this fluorescent material is 295 ~ 500nm.
Its preparation method compared with described in embodiment 1, except Eu 2o 3addition be 0.0075mol, SrCO 3addition be outside 6.975mol, all the other are all identical.
Embodiment 4
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.01, y=0.02); The excitation band wavelength region of this fluorescent material is 295 ~ 500nm.
Its preparation method compared with described in embodiment 1, except Eu 2o 3addition be 0.01mol, SrCO 3addition be outside 6.97mol, all the other are all identical.
Embodiment 5
A kind of fluorescent material, its chemical expression is Sr 7-xzr (PO 4) 6: xTb 3+(x=0.01); Its preparation method compared with described in embodiment 1, except not adding Eu 2o 3outward, all the other are all identical.
Embodiment 6
A kind of fluorescent material, its chemical expression is Sr 7-yzr (PO 4) 6: yEu 3+((y=0.01)); Its preparation method compared with described in embodiment 2, except not adding Tb 2o 3outward, all the other are all identical.
Embodiment 7
A kind of fluorescent material, its chemical expression is Sr 7zr (PO 4) 6; Its preparation method compared with described in embodiment 1, except not adding Tb 2o 3and Eu 2o 3outward, all the other are all identical.
The performance of the fluorescent material obtained by embodiment 1 ~ 7 is tested, and carries out Integrated comparative, can draw:
Fig. 1 shows embodiment 1 ~ 4 and the fluorescent material obtained by embodiment 7, with Sr 7zr (PO 4) 6the X-ray diffractogram of standard card PDF#34-0065, in figure, a represents embodiment 7, b and represents embodiment 1, c and represent embodiment 2, d represents embodiment 3, e represents embodiment 4, by X-ray diffraction analysis, can find out, do not changed the phase structure of matrix by doped with rare-earth elements, what this explanation was obtained is pure phase fluorescent material;
Fig. 2, Fig. 3 and Fig. 4 respectively illustrate the fluorescence excitation of the obtained fluorescent material of embodiment 5, embodiment 6 and embodiment 1 under different excitation band wavelength and emmission spectrum, in figure, a represents embodiment 5, b and represents embodiment 6, c represents embodiment 1, Fig. 2 and Fig. 3 shows single dopant ion Tb respectively 3+, Eu 3+characteristic peak, represent obtain Eu respectively 3and Tb 3+feature ruddiness and green glow, by contrasting can find out with Fig. 4, Tb 3+, Eu 3+mix the crest demonstrating to go out at 544nm altogether decline but strengthen at the crest that 613nm goes out, this shows Tb 3+with Eu 3+between there is transmission ofenergy, this for adjustment photochromic most important;
Fig. 5 shows the obtained utilizing emitted light spectrogram of fluorescent material under 374nm excitation band of embodiment 1 ~ 5, can find out, as fixing Tb 3+content is 0.01, along with increase Eu 3+content, this fluorescence pattern demonstrates and is declining gradually at the crest of 544nm, and the crest at 613nm place rises gradually, shows Tb 3+with Eu 3+between there is transmission ofenergy, corresponding photochromicly to be changed by green glow-warm white-ruddiness.This shows successfully to synthesize photochromic adjustable fluorescent material, and industrially can modulate different photochromic according to different demand, tool is of great significance.
Embodiment 8
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); The excitation band wavelength region of this fluorescent material is 295 ~ 500nm.
The preparation method of above-mentioned photochromic adjustable fluorescent material, comprises the following steps:
(1) respectively by 6.9molSrF 2, 1molZrCl 4, 6molNH 4h 2pO 4, 0.025molEu 2o 3, 0.025molTb 2o 3, and by after each starting compound mixing, add the dehydrated alcohol of mixture total mass 25%, ground and mixed is even, obtains blend sample;
(2) by blend sample roasting 2h at 1300 DEG C, be then naturally down to room temperature, again grind and obtain object product fluorescent material.
Embodiment 9
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); Its preparation method compared with described in embodiment 8, except SrF 2replace with SrCl 2, 0.025molEu 2o 3replace with 0.05molEu (NO 3) 3, 0.025molTb 2o 3replace with 0.05molTb (NO 3) 3outward, all the other are all identical.
Embodiment 10
A photochromic adjustable fluorescent material, its chemical expression is Sr 7-x-yti (PO 4) 6: xTb 3+, yEu 3+(x=0.04, y=0.05); Its preparation method compared with described in embodiment 8, except 6.9molSrF 2replace with 2.91molSrO, 3molSr (NO 3) 2, 1molSr (CH 3cOO) 2, 1molZrCl 4replace with 1molTiO 2, 0.025molEu 2o 3replace with 0.025molEuCl 3, 0.025molEuF 3, 0.025molTb 2o 3replace with 0.02molTbCl 3, 0.02molTbF 3outward, all the other are all identical.
Embodiment 11
A photochromic adjustable fluorescent material, its chemical expression is Ca 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); Its preparation method compared with described in embodiment 8, except SrF 2replace with outside CaO, all the other are all identical.
Embodiment 12
A photochromic adjustable fluorescent material, its chemical expression is Ca 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.03, y=0.03); Its preparation method compared with described in embodiment 11, except 6.9molCaO replaces with 6.95molCaCl 2, 0.025molEu 2o 3replace with 0.01molEu (CH 3cOO) 3, 0.005molEu 2(CO 3) 3, 0.005molEu 2(SO 4) 3, 0.025molTb 2o 3replace with 0.005molTb 2(CO 3) 3, 0.01molTbF 3, 0.01molTbCl 3outward, all the other are all identical.
Embodiment 13
A photochromic adjustable fluorescent material, its chemical expression is Ca 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); Its preparation method compared with described in embodiment 11, except 6.9molCaO replaces with 2.9molCa (CO 3) 3, 3molCa (NO 3) 2, 1molCa (CH 3cOO) 2, 6molNH 4h 2pO 4replace with 3molNH 4h 2pO 4with 3mol (NH 4) 2hPO 4outward, all the other are all identical.
Embodiment 14
A photochromic adjustable fluorescent material, its chemical expression is Ca 7-x-yti (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); Its preparation method compared with described in embodiment 11, except 6.9molCaO replaces with 3molCaCl 2and 3.9molCaF 2, 1molZrCl 4replace with 1molTiCl 4outward, all the other are all identical.
Embodiment 15
A photochromic adjustable fluorescent material, its chemical expression is Ba 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.05, y=0.05); Its preparation method compared with described in embodiment 8, except SrF 2replace with BaO, dehydrated alcohol addition is 35% of mixture total mass, and maturing temperature is 1200 DEG C, and roasting time is outside 3h, and all the other are all identical.
Embodiment 16
A photochromic adjustable fluorescent material, its chemical expression is Ba 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.015, y=0.015); Its preparation method compared with described in embodiment 15, except 6.9molBaO replaces with (7-x-y) molBaCl 2, 0.025molEu 2o 3replace with 0.05molEu (CH 3cOO) 3, 0.0025molEu 2(CO 3) 3, 0.0025molEu 2(SO 4) 3, 0.025molTb 2o 3replace with 0.0025molTb 2(CO 3) 3, 0.05molTbF 3, 0.05molTbCl 3outward, all the other are all identical.
Embodiment 17
A photochromic adjustable fluorescent material, its chemical expression is Ba 7-x-yzr (PO 4) 6: xTb 3+, yEu 3+(x=0.01, y=0.01); Its preparation method compared with described in embodiment 15, except 6.9molBaO replaces with 2.98molBa (CO 3) 3, 3molBa (NO 3) 2, 1molBa (CH 3cOO) 2, 6molNH 4h 2pO 4replace with 3molNH 4h 2pO 4with 3mol (NH 4) 2hPO 4outward, all the other are all identical.
Embodiment 18
A photochromic adjustable fluorescent material, its chemical expression is Ba 7-x-yti (PO 4) 6: xTb 3+, yEu 3+(x=0.04, y=0.02); Its preparation method compared with described in embodiment 15, except 6.9molBaO replaces with 2.94molBaCl 2and 4molBaF 2, 1molZrCl 4replace with 1molTiCl 4outward, all the other are all identical.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.

Claims (10)

1. a photochromic adjustable fluorescent material, is characterized in that, its chemical expression is as follows: A 7-x-yb (PO 4) 6: xTb 3+, yEu 3+; Wherein, A is selected from Ca, the one in Sr or Ba, and B is the span of Zr or Ti, x is (0 ~ 0.05), and the span of y is (0 ~ 0.05), and the excitation band wavelength region of described fluorescent material is 295 ~ 500nm.
2. a preparation method for photochromic adjustable fluorescent material as claimed in claim 1, is characterized in that, comprise the following steps:
(1) starting compound of containing element A, B, P, Tb and Eu is respectively taken, make the elements A in each starting compound: the mol ratio of B:P:Tb:Eu is (7-x-y): 1:6:x:y, and each starting compound ground and mixed is even, obtain blend sample;
(2) by blend sample roasting, be then naturally down to room temperature, again grind and obtain object product fluorescent material.
3. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, it is characterized in that, the starting compound comprising element A is selected from one or more in the carbonate of element A, nitrate, acetate, fluorochemical, muriate or oxide compound, wherein
When A is Ca, its starting compound be selected from calcium carbonate, Calcium Fluoride (Fluorspan), calcium chloride, calcium oxide, nitrocalcite or calcium acetate one or more;
When A is Sr, its starting compound be selected from Strontium carbonate powder, strontium fluoride, strontium chloride, strontium oxide, strontium nitrate or strontium acetate one or more;
When A is Ba, its starting compound is selected from barium carbonate, barium fluoride, bariumchloride, barium oxide, nitrate of baryta, one or more in barium acetate.
4. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, it is characterized in that, the starting compound comprising B element is selected from oxide compound or the muriate of B element, wherein,
When B is Zr, its compound is zirconium white or zirconium chloride;
When B is Ti, its compound is titanium oxide or titanium tetrachloride.
5. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, is characterized in that, the starting compound of containing element Tb be selected from Terbium trinitrate, terbium carbonate, terbium sesquioxide, terbium chloride or fluoridize in terbium one or more.
6. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, it is characterized in that, the starting compound of containing element Eu be selected from europium nitrate, Europium trichloride, acetic acid europium, europium carbonate, europium, europium sulfate or europium sesquioxide one or more.
7. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, is characterized in that, the starting compound of containing element P be selected from Secondary ammonium phosphate or primary ammonium phosphate one or both.
8. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, is characterized in that, in step (1) during each starting compound grinding, also adds dehydrated alcohol and assists grinding, after having ground, dry and obtain blend sample.
9. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 8, it is characterized in that, the addition of described dehydrated alcohol is 25 ~ 40% of blend sample quality.
10. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 2, is characterized in that, in step (2), the maturing temperature of blend sample is more than 1000 DEG C, and roasting time is 2 ~ 4h.
CN201510746251.9A 2015-11-05 2015-11-05 A kind of photochromic adjustable fluorescent material and preparation method thereof Expired - Fee Related CN105255491B (en)

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