CN105255491B - A kind of photochromic adjustable fluorescent material and preparation method thereof - Google Patents
A kind of photochromic adjustable fluorescent material and preparation method thereof Download PDFInfo
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- CN105255491B CN105255491B CN201510746251.9A CN201510746251A CN105255491B CN 105255491 B CN105255491 B CN 105255491B CN 201510746251 A CN201510746251 A CN 201510746251A CN 105255491 B CN105255491 B CN 105255491B
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Abstract
The present invention relates to a kind of photochromic adjustable fluorescent material and preparation method thereof, the chemical expression of described fluorescent material is as follows：A7‑x‑yB(PO4)6：xTb3+, yEu3+；Wherein, A is selected from one kind in Ca, Sr or Ba, B is Zr or Ti, x span are (0~0.05), and y span is (0~0.05), the excitation band wave-length coverage of fluorescent material is 295~500nm, and its preparation method comprises the following steps：(1) weigh respectively comprising elements A, B, P, Tb and Eu starting compound so that the elements A in each starting compound：B：P：Tb：Eu mol ratio is (7 x y):1:6：x：Y, and each starting compound ground and mixed is uniform, obtain blend sample；(2) blend sample is calcined, is then down to room temperature naturally, regrind and produce purpose product fluorescent material.Compared with prior art, fluorescent material of the invention can be photochromic adjustable from green glow warm white feux rouges under the exciting of near ultraviolet/purple light, and technique is simple, and raw material is cheap and easy to get, green.
Description
Technical field
The present invention relates to rare-earth luminescent material field, the light excited more particularly, to a kind of near ultraviolet to purple LED chip
Adjustable fluorescent material of color and preparation method thereof.
Background technology
White light LEDs are as a kind of new all solid state lighting source, because it has long lifespan, efficiency high, energy-conservation, environmentally friendly nothing
Pollution, it is deep to be paid attention to by people and obtained the support energetically of national governments.In the market obtain white light mode be with
Blue-light LED chip and YAG：Based on Ce combinations.It achieves prominent progress in application field, but exposes some keys simultaneously
Problem.The maximum deficiency of this combination is that colour rendering is relatively low, and maximum is only 85 or so, causes to be combined into due to lacking red color components
White light colour temperature it is higher so that the LED light colour cast being assembled into is cold, dazzling.
The problem of existing in recent years for current business white light, researcher start sight turning near ultraviolet or ultraviolet
The fluorescent material that LED chip excites.Near ultraviolet or UV LED chip have higher energy than blue-light LED chip, more favorably
In excitated fluorescent powder；Although compound by three primary colours can reach preferable colour rendering index, due between various fluorescent material
Differ in the presence of " color declines " degree, cause compound photochromic imbalance.Therefore develop and a kind of be used near ultraviolet excitated single-matrix
White light and photochromic adjustable masstone fluorescent material are particularly important.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of near ultraviolet to purple light
Single-matrix white and photochromic adjustable masstone fluorescent material that LED chip excites and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of photochromic adjustable fluorescent material, its chemical expression are as follows：A7-x-yB(PO4)6：xTb3+, yEu3+；Wherein, A
One kind in Ca, Sr or Ba, B is Zr or Ti, x span are (0~0.05), y span for (0~
0.05), the excitation band wave-length coverage of described fluorescent material is 295~500nm.
A kind of preparation method of photochromic adjustable fluorescent material, comprises the following steps：
(1) weigh respectively comprising elements A, B, P, Tb and Eu starting compound so that the element in each starting compound
A：B：P：Tb：Eu mol ratio is (7-x-y):1:6：x：Y, and each starting compound ground and mixed is uniform, obtain mixture
Sample；
(2) blend sample is calcined, is then down to room temperature naturally, regrind and produce purpose product fluorescent material.
Starting compound comprising element A be selected from the carbonate of element A, nitrate, acetate, fluoride, chloride or
One or more in oxide, wherein,
When A is Ca, its starting compound is selected from calcium carbonate, calcirm-fluoride, calcium chloride, calcium oxide, calcium nitrate or calcium acetate
In one or more；
When A is Sr, its starting compound is selected from strontium carbonate, strontium fluoride, strontium chloride, strontium oxide strontia, strontium nitrate or strontium acetate
In one or more；
When A is Ba, its starting compound is selected from barium carbonate, barium fluoride, barium chloride, barium monoxide, barium nitrate, in barium acetate
One or more.
Starting compound comprising B element is selected from the oxide or chloride of B element, wherein,
When B is Zr, its compound is zirconium oxide or zirconium chloride；
When B is Ti, its compound is titanium oxide or titanium tetrachloride.
The one kind of starting compound comprising element T b in terbium nitrate, terbium carbonate, terbium oxide, terbium chloride or fluorination terbium
It is or a variety of.
Starting compound comprising element Eu be selected from europium nitrate, Europium chloride, acetic acid europium, europium carbonate, europium, europium sulfate or
One or more in europium oxide.
Starting compound comprising element P is selected from one or both of diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
In step (1) during each starting compound grinding, it is additionally added absolute ethyl alcohol and assists grinding, after the completion of grinding, dry
To blend sample.
The addition of described absolute ethyl alcohol is the 25~40% of blend sample quality.
In step (2), the sintering temperature of blend sample is more than 1000 DEG C, and roasting time is 2~4h；Preferably, roast
It is 1000~1300 DEG C to burn temperature.
In the fluorescent material of the present invention, A7B(PO4)6As matrix, Tb3+For sensitizer, Eu3+For activator, by raw material
According to a certain ratio, it is well mixed.Under hot conditions, by contact between solid phase interface, react, nucleation, so as to form new knot
Crystallization compound.During fluorescent material is synthesized, under certain reaction temperature, the proper extension reaction time is advantageous to crystal nucleation
Be advantageous to improve the fluorescence intensity of fluorescent material.And reaction temperature is too high will cause fluorescent quenching, temperature is too low, can not obtain
Target product.In the present invention, when singly mixing Eu in matrix3+Or Tb3+When, fluorescent material can be distinguished under near ultraviolet excitation
Feature feux rouges or green glow are obtained, when being co-doped with Eu in matrix3+And Tb3+When, under ultraviolet excitation, due to Eu3+And Tb3+Between
Energy transmission, Eu be present3+And Tb3+Launch the fluorescence spectrum of its feature, by improving Eu3+/Tb3+Ratio, it is photochromic can be by
Green glow-warm white-feux rouges transformation, is realized photochromic adjustable.
Compared with prior art, the present invention has advantages below：
1) photochromic adjustable range is big：Chemical expression produced by the present invention is A7-x-yB(PO4)6：xTb3+, yEu3+It is photochromic
Adjustable fluorescent material, its excitation band wave-length coverage is in 290~500nm of near ultraviolet to purple light, the near ultraviolet core with the market
Piece has good matching degree, meanwhile, by adjusting the doping ratio of rare earth, fixed Tb3+Concentration, increase Eu3+Concentration,
The photochromic transformation by green glow-warm white-feux rouges can be obtained, so that the LED light colour cast being assembled into warms up, will not be dazzling；
2) preparation technology of the invention is simple, and raw material is cheap and easy to get, and course of reaction does not have three industrial wastes, has green ring
The features such as guarantor, low energy consumption, high benefit, it is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of embodiments of the invention 1~4 and the fluorescent material of embodiment 7；
Fig. 2 is the fluorescence excitation and emission spectrum of the fluorescent material of embodiments of the invention 5；
Fig. 3 is the fluorescence excitation and emission spectrum of the fluorescent material of embodiments of the invention 6；
Fig. 4 is the fluorescence excitation and emission spectrum of the fluorescent material of embodiments of the invention 1；
Fig. 5 is the fluorescence excitation and emission spectrum of the fluorescent material of embodiments of the invention 1~5.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.01,
Y=0.005)；The excitation band wave-length coverage of the fluorescent material is 295~500nm.
The preparation method of above-mentioned photochromic adjustable fluorescent material, comprises the following steps：
(1) 6.985mol SrCO are weighed respectively3, 1mol ZrO2, 6mol (NH4)2HPO4, 0.0025mol Eu2O3,
0.005mol Tb2O3, and by after the mixing of each starting compound, add the absolute ethyl alcohol of mixture gross mass 40%, ground and mixed
Uniformly, blend sample is obtained；
(2) blend sample is calcined 4h at 1000 DEG C, is then down to room temperature naturally, regrinds and produce purpose product
Fluorescent material.
Embodiment 2
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.01,
Y=0.01)；The excitation band wave-length coverage of the fluorescent material is 295~500nm.
Its preparation method is compared with described in embodiment 1, except Eu2O3Addition be 0.005mol, SrCO3Addition
Outside for 6.98mol, remaining all same.
Embodiment 3
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.01,
Y=0.015)；The excitation band wave-length coverage of the fluorescent material is 295~500nm.
Its preparation method is compared with described in embodiment 1, except Eu2O3Addition be 0.0075mol, SrCO3Addition
Outside for 6.975mol, remaining all same.
Embodiment 4
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.01,
Y=0.02)；The excitation band wave-length coverage of the fluorescent material is 295~500nm.
Its preparation method is compared with described in embodiment 1, except Eu2O3Addition be 0.01mol, SrCO3Addition be
Outside 6.97mol, remaining all same.
Embodiment 5
A kind of fluorescent material, its chemical expression are Sr7-xZr(PO4)6：xTb3+(x=0.01)；Its preparation method and reality
Apply and compared described in example 1, except being not added with Eu2O3Outside, remaining all same.
Embodiment 6
A kind of fluorescent material, its chemical expression are Sr7-yZr(PO4)6：yEu3+((y=0.01))；Its preparation method with
Compared described in embodiment 2, except being not added with Tb2O3Outside, remaining all same.
Embodiment 7
A kind of fluorescent material, its chemical expression are Sr7Zr(PO4)6；Its preparation method removes compared with described in embodiment 1
It is not added with Tb2O3And Eu2O3Outside, remaining all same.
The performance of fluorescent material obtained by embodiment 1~7 is tested, and carries out Integrated comparative, it can be deduced that：
Fig. 1 shows embodiment 1~4 and the fluorescent material obtained by embodiment 7, with Sr7Zr(PO4)6Standard card PDF#
34-0065 X-ray diffractogram, in figure, a represents embodiment 7, and b represents embodiment 1, and c represents embodiment 2, and d represents embodiment
3, e represent embodiment 4, pass through X-ray diffraction analysis, it can be seen that do not have the thing for changing matrix by rare earth doped element
Phase structure, this explanation made from be pure phase fluorescent material；
Fig. 2, Fig. 3 and Fig. 4 respectively illustrate embodiment 5, embodiment 6 and fluorescent material made from embodiment 1 and Bu Tong swashed
Fluorescence excitation and emission spectrum under hair band wavelength, in figure, Fig. 2 and Fig. 3 show single Doped ions Tb respectively3+, Eu3+'s
Characteristic peak, expression obtain Eu respectively3And Tb3+Feature feux rouges and green glow, by with Fig. 4 contrasts as can be seen that Tb3+, Eu3+
It is co-doped with showing the crest enhancing that the crest gone out in 544nm declines but in 613nm goes out, this shows Tb3+With Eu3+Between exist
Energy transmission, this is photochromic most important for adjusting；
Fig. 5 shows launching light spectrogram of the fluorescent material under 374nm excitation bands made from embodiment 1~5, can see
Go out, as fixed Tb3+Content is 0.01, with increase Eu3+Content, the fluorescence pattern shows the crest in 544nm gradual
Decline, and the crest at 613nm is gradually increasing, and shows Tb3+With Eu3+Between energy transmission be present, it is corresponding photochromic by green
Light-warm white-feux rouges transformation.This shows successfully to synthesize photochromic adjustable fluorescent material, industrially can be according to difference
Demand modulates different photochromic, and tool is of great significance.
Embodiment 8
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；The excitation band wave-length coverage of the fluorescent material is 295~500nm.
The preparation method of above-mentioned photochromic adjustable fluorescent material, comprises the following steps：
(1) respectively by 6.9mol SrF2, 1mol ZrCl4, 6mol NH4H2PO4, 0.025mol Eu2O3, 0.025mol
Tb2O3, and by after the mixing of each starting compound, the absolute ethyl alcohol of mixture gross mass 25% is added, ground and mixed is uniform, obtains
Blend sample；
(2) blend sample is calcined 2h at 1300 DEG C, is then down to room temperature naturally, regrinds and produce purpose product
Fluorescent material.
Embodiment 9
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；Its preparation method is compared with described in embodiment 8, except SrF2Replace with SrCl2, 0.025mol Eu2O3Replace with
0.05mol Eu(NO3)3, 0.025mol Tb2O3Replace with 0.05mol Tb (NO3)3Outside, remaining all same.
Embodiment 10
A kind of photochromic adjustable fluorescent material, its chemical expression is Sr7-x-yTi(PO4)6：xTb3+, yEu3+(x=0.04,
Y=0.05)；Its preparation method is compared with described in embodiment 8, except 6.9mol SrF2Replace with 2.91mol SrO, 3mol Sr
(NO3)2、1mol Sr(CH3COO)2, 1mol ZrCl4Replace with 1mol TiO2, 0.025mol Eu2O3Replace with 0.025mol
EuCl3、0.025mol EuF3, 0.025mol Tb2O3Replace with 0.02mol TbCl3、0.02mol TbF3Outside, remaining is homogeneous
Together.
Embodiment 11
A kind of photochromic adjustable fluorescent material, its chemical expression is Ca7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；Its preparation method is compared with described in embodiment 8, except SrF2Replace with outside CaO, remaining all same.
Embodiment 12
A kind of photochromic adjustable fluorescent material, its chemical expression is Ca7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.03,
Y=0.03)；Its preparation method is compared with described in embodiment 11, except 6.9mol CaO replace with 6.95molCaCl2, 0.025mol
Eu2O3Replace with 0.01mol Eu (CH3COO)3、0.005mol Eu2(CO3)3、0.005mol Eu2(SO4)3, 0.025mol
Tb2O3Replace with 0.005mol Tb2(CO3)3、0.01mol TbF3、0.01mol TbCl3Outside, remaining all same.
Embodiment 13
A kind of photochromic adjustable fluorescent material, its chemical expression is Ca7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；Its preparation method is compared with described in embodiment 11, except 6.9mol CaO replace with 2.9mol Ca (CO3)3、3mol
Ca(NO3)2、1mol Ca(CH3COO)2, 6mol NH4H2PO4Replace with 3mol NH4H2PO4With 3mol (NH4)2HPO4Outside, remaining
All same.
Embodiment 14
A kind of photochromic adjustable fluorescent material, its chemical expression is Ca7-x-yTi(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；Its preparation method is compared with described in embodiment 11, except 6.9mol CaO replace with 3mol CaCl2And 3.9mol
CaF2, 1mol ZrCl4Replace with 1mol TiCl4Outside, remaining all same.
Embodiment 15
A kind of photochromic adjustable fluorescent material, its chemical expression is Ba7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.05,
Y=0.05)；Its preparation method is compared with described in embodiment 8, except SrF2BaO is replaced with, absolute ethyl alcohol addition is that mixture is total
The 35% of quality, sintering temperature are 1200 DEG C, and roasting time is remaining all same outside 3h.
Embodiment 16
A kind of photochromic adjustable fluorescent material, its chemical expression is Ba7-x-yZr(PO4)6：xTb3+, yEu3+(x=
0.015, y=0.015)；Its preparation method is compared with described in embodiment 15, except 6.9mol BaO are replaced with (7-x-y)
molBaCl2, 0.025mol Eu2O3Replace with 0.05mol Eu (CH3COO)3、0.0025mol Eu2(CO3)3、0.0025mol
Eu2(SO4)3, 0.025mol Tb2O3Replace with 0.0025mol Tb2(CO3)3、0.05mol TbF3、0.05mol TbCl3Outside,
Remaining all same.
Embodiment 17
A kind of photochromic adjustable fluorescent material, its chemical expression is Ba7-x-yZr(PO4)6：xTb3+, yEu3+(x=0.01,
Y=0.01)；Its preparation method is compared with described in embodiment 15, except 6.9mol BaO replace with 2.98mol Ba (CO3)3、3mol
Ba(NO3)2、1mol Ba(CH3COO)2, 6mol NH4H2PO4Replace with 3mol NH4H2PO4With 3mol (NH4)2HPO4Outside, remaining
All same.
Embodiment 18
A kind of photochromic adjustable fluorescent material, its chemical expression is Ba7-x-yTi(PO4)6：xTb3+, yEu3+(x=0.04,
Y=0.02)；Its preparation method is compared with described in embodiment 15, except 6.9mol BaO replace with 2.94mol BaCl2And 4mol
BaF2, 1mol ZrCl4Replace with 1mol TiCl4Outside, remaining all same.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using invention.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel do not depart from improvement that scope made and modification all should be the present invention's according to the announcement of the present invention
Within protection domain.
Claims (9)
- A kind of 1. preparation method of photochromic adjustable fluorescent material, it is characterised in that the chemical expression of described fluorescent material It is as follows：A7-x-yB(PO4)6：xTb3+, yEu3+；Wherein, A is selected from one kind in Ca, Sr or Ba, and B is Zr or Ti, 0 ＜ x≤0.05, and 0 ＜ y≤0.05, the excitation band wave-length coverage of described fluorescent material is 295~500nm, and the preparation method includes following step Suddenly：(1) weigh respectively comprising elements A, B, P, Tb and Eu starting compound so that the elements A in each starting compound：B： P：Tb：Eu mol ratio is (7-x-y)：1：6：x：Y, and each starting compound ground and mixed is uniform, obtain blend sample；(2) blend sample is calcined, is then down to room temperature naturally, regrind and produce purpose product fluorescent material；(3) Eu is improved3+/Tb3+Ratio, be made that fluorescent material is photochromic to be changed by green glow-warm white-feux rouges, realize it is photochromic can Adjust.
- 2. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 1, it is characterised in that include A members Carbonate of the starting compound selected from element A, nitrate, acetate, fluoride, chloride or one kind in oxide of element or It is several, wherein,When A is Ca, its starting compound is in calcium carbonate, calcirm-fluoride, calcium chloride, calcium oxide, calcium nitrate or calcium acetate It is one or more kinds of；When A is Sr, its starting compound is in strontium carbonate, strontium fluoride, strontium chloride, strontium oxide strontia, strontium nitrate or strontium acetate It is one or more kinds of；When A is Ba, its starting compound is selected from barium carbonate, barium fluoride, barium chloride, barium monoxide, barium nitrate, and one in barium acetate Kind is a variety of.
- 3. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 1, it is characterised in that include B members The starting compound of element is selected from the oxide or chloride of B element, wherein,When B is Zr, its compound is zirconium oxide or zirconium chloride；When B is Ti, its compound is titanium oxide or titanium tetrachloride.
- 4. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 1, it is characterised in that include element One or more of the Tb starting compound in terbium nitrate, terbium carbonate, terbium oxide, terbium chloride or fluorination terbium.
- 5. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 1, it is characterised in that include element One kind in europium nitrate, Europium chloride, acetic acid europium, europium carbonate, europium, europium sulfate or europium oxide of Eu starting compound or It is a variety of.
- 6. the preparation method of a kind of photochromic adjustable fluorescent material according to claim 1, it is characterised in that include element P starting compound is selected from one or both of diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
- A kind of 7. preparation method of photochromic adjustable fluorescent material according to claim 1, it is characterised in that step (1) In the grinding of each starting compound when, be additionally added absolute ethyl alcohol and assist grinding, after the completion of grinding, drying obtains blend sample.
- A kind of 8. preparation method of photochromic adjustable fluorescent material according to claim 7, it is characterised in that described nothing The addition of water-ethanol is the 25~40% of blend sample quality.
- A kind of 9. preparation method of photochromic adjustable fluorescent material according to claim 1, it is characterised in that step (2) In, the sintering temperature of blend sample is more than 1000 DEG C, and roasting time is 2~4h.
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| CN102604635A (en) * | 2012-01-19 | 2012-07-25 | 苏州大学 | Zirconium-phosphate-based luminescent material, preparation method thereof, and application thereof |
| CN103289692A (en) * | 2012-02-28 | 2013-09-11 | 海洋王照明科技股份有限公司 | Europium-terbium co-doped zirconium phosphate luminescent material as well as preparation method and application thereof |
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| CN102604635A (en) * | 2012-01-19 | 2012-07-25 | 苏州大学 | Zirconium-phosphate-based luminescent material, preparation method thereof, and application thereof |
| CN103289692A (en) * | 2012-02-28 | 2013-09-11 | 海洋王照明科技股份有限公司 | Europium-terbium co-doped zirconium phosphate luminescent material as well as preparation method and application thereof |
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