CN102618272A - Phosphate red luminescent material and preparation method thereof - Google Patents

Phosphate red luminescent material and preparation method thereof Download PDF

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CN102618272A
CN102618272A CN2012100694901A CN201210069490A CN102618272A CN 102618272 A CN102618272 A CN 102618272A CN 2012100694901 A CN2012100694901 A CN 2012100694901A CN 201210069490 A CN201210069490 A CN 201210069490A CN 102618272 A CN102618272 A CN 102618272A
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luminescent material
red luminescent
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phosphate
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张占辉
陈力
黄志良
刘恒
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Wuhan Institute of Technology
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Abstract

The invention relates to a phosphate red luminescent material and a preparation method thereof. The chemical formula of the phosphate red luminescent material is A3-x-yBy(PO4)2:xEu<3+>, wherein the element A is one or more of alkali earth metal ions Ca<2+>, Sr<2+> and Ba<2+>; the element B is one or more of alkali metal ions Li<+>, Na<+> and K<+>; x is larger than 0 and smaller than or equal to 1; and y is larger than or equal to 0 and smaller than or equal to 1. Compared with the prior art, the invention has the advantages that 1), as phosphate is taken as matrix, the crystallization temperature is low, the stability is good, the raw material is low in cost and easy to obtain, the manufacturing cost is low, and the product has no radioactivity, so as not to do harm to people and the environment; 2), the luminous intensity of the luminescent material is remarkably enhanced through charge compensation; 3), the phosphate red luminescent material can be excited effectively by short wave ultraviolet, long wave ultraviolet and 465 nm visible light, and also can be applied to fluorescent lamps and LEDs; and 4), the preparation method is simple and is easy to operate.

Description

A kind of phosphate red luminescent material and preparation method thereof
Technical field
The invention belongs to the material technology field, be specifically related to a kind of with phosphoric acid salt be matrix, europkium-activated by trivalent, can exciting light be converted into luminescent material of red light and preparation method thereof.
Background technology
Phosphate rock resource is the grand strategy resource of country, and its development and use have material impact to development of world economy.China's phosphate rock resource reserves are very abundant, have significant resources advantage, but consumption structure is very unreasonable, product is single, and the overwhelming majority does not have product advantage in order to low value-added chemical such as production phosphate fertilizer.Country just with " phosphate rock resource integration, resources effective utilization " the active development phosphate rock resource of serving as theme, improves the phosphor resource comprehensive utilization ratio and will become main flow at present, and exploitation high added value phosphorus product is also attached most importance to one-tenth.
Solid material that can visible emitting when luminescent material (fluorescent material) refers generally to receive the external world and excites, be one type be widely used in throwing light on, show, the high added value functional materials in field such as detection, sign.Wherein be that the luminescent material of matrix has the luminous efficiency height, physicochemical property are stable, raw material is easy to get and the low advantage such as industrial production that is fit to of cheap, preparation temperature with phosphoric acid salt.Obviously, the development and use of phosphoric acid salt luminescent material are significant for improving the phosphor resource using value.Yet because the research of foreign technology monopolization and domestic input is less; The luminescent material product is still in the majority with classes such as aluminate, silicate, sulfide at present; Research report about phosphoric acid salt luminescent material product innovation and luminosity thereof is less; Practical phosphoric acid salt luminescent material kind is extremely limited, and further improving phosphoric acid salt luminescent material quality also is the key issue that presses for solution.
Chinese invention patent 200710028070.8 discloses a kind of rare earth pyrophosphate phosphor and compound method thereof; Chinese invention patent 200810026063.9 has reported that a kind of non-mercury florescent lamp is with the basic metal rare earth tetrametaphosphate luminescent material and preparation method thereof that emits white light; Chinese invention patent 200910157359.9 discloses RE phosphate luminescent material of a kind of doped with cerium and preparation method thereof, and the chemical constitution of this luminescent material is X x X ' y Ce 1- x- y PO 4, wherein X and X ' are a kind of among rare-earth elements La, Y, the Gd; Chinese invention patent 201010203408.0 discloses a kind of AB 1- x- y PO 4: Eu 2+ x , Pr 3+ y The type alkali metal alkaline earth metal phosphate phosphor is the preparation method extremely; Chinese invention patent 201010292808.3 discloses a kind of preparation method of phosphoric acid salt luminescent material, does not relate to novel material; Chinese invention patent 201110324833.X discloses a kind of A 3- x- y (PO 4) 2: xEu 2+, yType B phosphate long afterglow luminous material, this material are dominant activator with the divalent europium, are auxiliary activator with the metals ion of one or more high valence states, can launch the steady persistence of blue-greenish colour, blueness or purple.Foregoing invention all do not relate to provided by the present invention with phosphoric acid salt be matrix, by the europkium-activated A of trivalent 3- x- y B y (PO 4) 2: xEu 3+(A is alkaline earth metal ion Ca 2+, Sr 2+Or Ba 2+In one or more; B is alkalimetal ion Li +, Na +Or K +One or more; 0< x≤1; 0≤ y≤1) type luminescent material.
Summary of the invention
Problem to be solved by this invention is to propose a kind of new luminescent material to above-mentioned prior art, and this material is matrix with phosphoric acid salt, is activator with the trivalent europium, can convert exciting light to red light.
Another object of the present invention provides the preparation method of above-mentioned phosphate red luminescent material.
The present invention is adopted solution to be by the problem of the above-mentioned proposition of solution: a kind of phosphate red luminescent material, it has following chemical formula and forms: A 3- x- y B y (PO 4) 2: xEu 3+, wherein, elements A is alkaline earth metal ion Ca 2+, Sr 2+Or Ba 2+In one or more, element B is alkalimetal ion Li +, Na +Or K +One or more, and 0< x≤1,0≤ y≤1.
A kind of preparation method of phosphate red luminescent material is characterized in that, includes following steps:
1) according to chemical formula A 3- x- y B y (PO 4) 2: xEu 3+Form, accurately take by weighing carbonate or the oxide compound of A element, carbonate or oxide compound, phosphoric acid salt and the europium sesquioxide raw material of B element respectively by stoichiometric ratio, wherein, elements A is alkaline earth metal ion Ca 2+, Sr 2+Or Ba 2+In one or more, element B is alkalimetal ion Li +, Na +Or K +One or more, and 0< x≤1,0≤ y≤1;
2) raw materials mix of step 1) is ground evenly; Directly in air, calcined 2 ~ 12 hours down, or, be cooled to room temperature earlier 300 ~ 800 ℃ of following pre-burnings 2 ~ 6 hours in 800 ~ 1300 ℃; Behind the regrinding; In air, calcined 2 ~ 12 hours down, naturally cool to room temperature, then with the levigate the finished product that promptly get of products therefrom in 800 ~ 1300 ℃.
Press such scheme, the preferred temperature of described raw material incinerating is 1000 ~ 1200 ℃.
Press such scheme, the described preferred time of raw material incinerating is 3 ~ 6 hours.
The present invention carries out the non-equivalence replacement through introducing extra monovalent base metals ion B to the divalent alkaline-earth metal ion A, compensates by trivalent active ions Eu 3+Non-equivalence to the divalent alkaline-earth metal ion A replaces caused charge difference.
Eu 3+Replace the divalent alkaline-earth metal ion A, in order to keep charge balance, with producing electronegative defective:
Figure 353970DEST_PATH_IMAGE001
(1)
(2)
Monovalent base metals ion B replaces the divalent alkaline-earth metal ion A, with producing positively charged defective:
Figure 203163DEST_PATH_IMAGE003
(3)
Figure 111820DEST_PATH_IMAGE004
(4)
Two types of defective charge neutralizatioies, thus realize charge compensation, to eliminate lattice imperfection, to stablize the lattice environment, reach the purpose that strengthens the luminescent material luminous intensity.Suitable excessive the mixing of monovalent base metals ion B can also be adjusted the centre symmetry of microtexture, helps eliminating Eu 3+ 5D 0→ 7F 2The parity selection rule of electric dipole transition is further enhanced its red emission intensity.
Compared with prior art, the present invention has following advantage:
(1) red illuminating material of the present invention is matrix with phosphoric acid salt, and the low and good stability of Tc, is easy to get at low in raw material cost, and production cost is low, and product is "dead", can not work the mischief to human and environment;
(2) red illuminating material of the present invention through introducing extra monovalent base metals ion B, to realize charge compensation, has remarkable enhancing before the relative charge compensation of the luminous intensity of luminescent material behind charge compensation;
(3) red illuminating material of the present invention can effectively be excited by shortwave ultraviolet, long wave ultraviolet and 465 nm visible lights, can be applicable to luminescent lamp, photodiode etc.;
(4) preparation method of the present invention is simple, and easy handling is low for equipment requirements, environmental friendliness.
Description of drawings
The excitation spectrum of phosphate red luminescent material when 613 nm monitor that Fig. 1 provides for the embodiment of the invention 1,6,7;
The emmission spectrum of phosphate red luminescent material under 394 nm excite that Fig. 2 provides for the embodiment of the invention 1,6,7.
Embodiment
Following instance is that the present invention comprises but is not limited to following instance to the further specifying of technology of the present invention.
Embodiment 1
Raw material is CaCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.7:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding, places crucible, puts into High Temperature Furnaces Heating Apparatus, in 1000 ℃ of calcination 8 hours, naturally cools to room temperature, levigate, obtains phosphate red luminescent material Ca 2.7(PO 4) 2: 0.3Eu 3+, principal phase is Ca 3(PO 4) 2Its excitation spectrum and emmission spectrum are seen accompanying drawing 1 and accompanying drawing 2 respectively.Excitation spectrum is positioned near the wide excitation band 254 nm by a peak and the several sharp wire excitation peak that is distributed between 310 ~ 500 nm is formed; Wherein, The excitation intensity at 394 nm and 465 nm places is higher, and promptly this material can effectively be excited by shortwave ultraviolet, long wave ultraviolet and 465 nm visible lights; Emmission spectrum is made up of several sharp wire emission peaks that are distributed between 550 ~ 750 nm, and wherein, the intensity of 613 nm emission peaks is the highest, and promptly this material presents emitting red light.
Embodiment 2
Raw material is BaCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.9:2:0.05, and it is even accurately to take by weighing each raw material and mixed grinding, places crucible, puts into High Temperature Furnaces Heating Apparatus, in 1200 ℃ of calcination 4 hours, naturally cools to room temperature, levigate, obtains phosphate red luminescent material Ba 2.9(PO 4) 2: 0.1Eu 3+, principal phase is Ba 3(PO 4) 2
Embodiment 3
Raw material is SrO (analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.1:2:0.45, and it is even accurately to take by weighing each raw material and mixed grinding, places crucible, puts into High Temperature Furnaces Heating Apparatus, in 1100 ℃ of calcination 6 hours, naturally cools to room temperature, levigate, obtains phosphate red luminescent material Sr 2.1(PO 4) 2: 0.9Eu 3+, principal phase is Sr 3(PO 4) 2
Embodiment 4
Raw material is CaCO 3(analytical pure), BaCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.6:0.1:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1200 ℃ of calcination 4 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ca 2.6Ba 0.1(PO 4) 2: 0.3Eu 3+, principal phase is Ca 3(PO 4) 2
Embodiment 5
Raw material is CaCO 3(analytical pure), SrCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.5:0.1:2:0.2, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1100 ℃ of calcination 6 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ca 2.5Sr 0.1(PO 4) 2: 0.4Eu 3+, principal phase is Ca 3(PO 4) 2
Embodiment 6
Raw material is CaCO 3(analytical pure), NaHCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.4:0.3:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1000 ℃ of calcination 8 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ca 2.4Na 0.3(PO 4) 2: 0.3Eu 3+, principal phase is Ca 3(PO 4) 2Its emissive porwer is about embodiment 1 provides 2.8 times of material emissive porwer.Its excitation spectrum and emmission spectrum are seen accompanying drawing 1 and accompanying drawing 2 respectively, and spectral shape is similar with embodiment 1, and intensity has remarkable enhancing, shows charge compensation agent Na +Introducing can reach the purpose that strengthens luminous intensity.
Embodiment 7
Raw material is CaCO 3(analytical pure), NaHCO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.3:0.4:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1000 ℃ of calcination 8 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ca 2.3Na 0.4(PO 4) 2: 0.3Eu 3+, principal phase is Ca 3(PO 4) 2Its emissive porwer is about embodiment 1 provides 2.9 times of material emissive porwer.Its excitation spectrum and emmission spectrum are seen accompanying drawing 1 and accompanying drawing 2 respectively, and spectral shape is similar with embodiment 6 with embodiment 1, and the relative embodiment 6 of intensity has enhancing to a certain degree, shows charge compensation agent Na +Suitable excessive mixing can further strengthen luminous intensity.Analyze the ratio of red emission (613 nm) intensity and orange light emission (595 nm) intensity, i.e. blood orange ratio, embodiment 7 is higher than embodiment 6.Because red emission and centre symmetry are inversely proportional to, and orange light emission is basic and centre symmetry is irrelevant, so charge compensation agent Na +Excessive mixing make Eu 3+Weakening of the centre symmetry of lattice environment of living in.
Embodiment 8
Raw material is SrCO 3(analytical pure), K 2CO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.4:0.15:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1100 ℃ of calcination 6 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Sr 2.4K 0.3(PO 4) 2: 0.3Eu 3+, principal phase is Sr 3(PO 4) 2
Embodiment 9
Raw material is CaCO 3(analytical pure), Li 2CO 3(analytical pure), K 2CO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.4:0.075:0.075:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, in 1000 ℃ of calcination 6 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ca 2.4Li 0.15K 0.15(PO 4) 2: 0.3Eu 3+, principal phase is Ca 3(PO 4) 2
Embodiment 10
Raw material is BaCO 3(analytical pure), SrO (analytical pure), K 2CO 3(analytical pure), (NH 4) 2HPO 4(analytical pure) and Eu 2O 3(99.99%), the mol ratio between them is 2.38:0.02:0.15:2:0.15, and it is even accurately to take by weighing each raw material and mixed grinding; Place crucible, put into High Temperature Furnaces Heating Apparatus, prior to 800 ℃ of pre-burnings 2 hours; Again in 1200 ℃ of calcination 4 hours; Naturally cool to room temperature, levigate, obtain phosphate red luminescent material Ba 2.38Sr 0.02K 0.3(PO 4) 2: 0.3Eu 3+, principal phase is Ba 3(PO 4) 2

Claims (4)

1. phosphate red luminescent material, it has following chemical formula and forms: A 3- x- y B y (PO 4) 2: xEu 3+, wherein, elements A is alkaline earth metal ion Ca 2+, Sr 2+Or Ba 2+In one or more, element B is alkalimetal ion Li +, Na +Or K +One or more, and 0< x≤1,0≤ y≤1.
2. the preparation method of the described phosphate red luminescent material of claim 1 is characterized in that, includes following steps:
1) according to chemical formula A 3- x- y B y (PO 4) 2: xEu 3+Form, accurately take by weighing carbonate or the oxide compound of A element, carbonate or oxide compound, phosphoric acid salt and the europium sesquioxide raw material of B element respectively by stoichiometric ratio, wherein, elements A is alkaline earth metal ion Ca 2+, Sr 2+Or Ba 2+In one or more, element B is alkalimetal ion Li +, Na +Or K +One or more, and 0< x≤1,0≤ y≤1;
2) raw materials mix of step 1) is ground evenly; Directly in air, calcined 2 ~ 12 hours down, or, be cooled to room temperature earlier 300 ~ 800 ℃ of following pre-burnings 2 ~ 6 hours in 800 ~ 1300 ℃; Behind the regrinding; In air, calcined 2 ~ 12 hours down, naturally cool to room temperature, then with the levigate the finished product that promptly get of products therefrom in 800 ~ 1300 ℃.
3. by the preparation method of the described phosphate red luminescent material of claim 2, it is characterized in that described raw material incinerating temperature is 1000 ~ 1200 ℃.
4. by the preparation method of claim 2 or 3 described phosphate red luminescent materials, it is characterized in that the described preferred time of raw material incinerating is 3 ~ 6 hours.
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CN103382390A (en) * 2013-07-11 2013-11-06 中国科学院福建物质结构研究所 Phosphate fluorescent powder used for white light LED and its preparation
CN103450897A (en) * 2013-08-12 2013-12-18 昆明理工大学 Red fluorescent powder and preparation method thereof
CN103555328A (en) * 2013-11-07 2014-02-05 韦胜国 Preparation method of singe matrix LED (light-emitting diode) fluorescent powder
CN103848409A (en) * 2014-03-07 2014-06-11 河南理工大学 Barium phosphate potassium compound crystal and preparation method and use thereof
CN108485667A (en) * 2018-03-28 2018-09-04 青岛科技大学 A kind of novel luminescent color is adjustable to fluorescent powder of white light and preparation method thereof
CN109321248A (en) * 2018-11-15 2019-02-12 大连工业大学 A kind of Eu doping calcium phosphate luminescent material and the preparation method and application thereof
CN113150780A (en) * 2021-04-06 2021-07-23 中国地质大学（北京） High-quantum-yield whitlockite type mineral fluorescent powder and application thereof

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Cited By (10)

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Publication number Priority date Publication date Assignee Title
CN103382390A (en) * 2013-07-11 2013-11-06 中国科学院福建物质结构研究所 Phosphate fluorescent powder used for white light LED and its preparation
CN103382390B (en) * 2013-07-11 2017-07-18 中国科学院福建物质结构研究所 A kind of white light LEDs phosphate phosphor and its preparation
CN103450897A (en) * 2013-08-12 2013-12-18 昆明理工大学 Red fluorescent powder and preparation method thereof
CN103555328A (en) * 2013-11-07 2014-02-05 韦胜国 Preparation method of singe matrix LED (light-emitting diode) fluorescent powder
CN103848409A (en) * 2014-03-07 2014-06-11 河南理工大学 Barium phosphate potassium compound crystal and preparation method and use thereof
CN108485667A (en) * 2018-03-28 2018-09-04 青岛科技大学 A kind of novel luminescent color is adjustable to fluorescent powder of white light and preparation method thereof
CN108485667B (en) * 2018-03-28 2020-09-22 青岛科技大学 Novel fluorescent powder with adjustable light-emitting color to white light and preparation method thereof
CN109321248A (en) * 2018-11-15 2019-02-12 大连工业大学 A kind of Eu doping calcium phosphate luminescent material and the preparation method and application thereof
CN109321248B (en) * 2018-11-15 2021-06-22 大连工业大学 Eu-doped calcium phosphate luminescent material and preparation method and application thereof
CN113150780A (en) * 2021-04-06 2021-07-23 中国地质大学（北京） High-quantum-yield whitlockite type mineral fluorescent powder and application thereof

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Application publication date: 20120801