CN109628090A - It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix - Google Patents
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix Download PDFInfo
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- CN109628090A CN109628090A CN201811506980.7A CN201811506980A CN109628090A CN 109628090 A CN109628090 A CN 109628090A CN 201811506980 A CN201811506980 A CN 201811506980A CN 109628090 A CN109628090 A CN 109628090A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7737—Phosphates
- C09K11/7738—Phosphates with alkaline earth metals
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Abstract
The present invention relates to luminescent material technical field, be related specifically to it is a kind of mix europium fluorescent powder and preparation method thereof using barium phosphate sodium as matrix, it is characterized in that: chemical general formula is NaBa1‑xPO4: x Eu, wherein 0.01≤x≤0.05.Using barium phosphate sodium as matrix, Eu is activated by doping3+, it is prepared using barium phosphate sodium as matrix and mixes europium fluorescent powder under near ultraviolet excitation, can stablizes and glow.Whole preparation process simple process, short preparation period, high production efficiency.
Description
Technical field
The present invention relates to fluorescent powder preparation technical fields, and in particular to mixes europium fluorescent powder to using barium phosphate sodium as matrix
Preparation method.
Background technique
Currently, the deep favor by people of White-light LED illumination, the at the same time preparation for the fluorescent powder of White-light LED illumination
Increasingly paid attention to.A kind of luminescence mechanism of white light LEDs is that redgreenblue mixing issues white light.Current fluorescent lamp is still
There are some disadvantages, such as service life are shorter, the problems such as polluting environment.Among numerous fluorescent powders, red fluorescence powder is with it
The performance of high quality is a dark horse, and can directly affect hair by the luminous intensity of blue light and the red fluorescence powder of ultraviolet excitation
Optical property, it is short to prepare a kind of manufacturing cycle, long service life, good luminous performance, and environment friendly and pollution-free red fluorescence powder is compeled
The eyebrows and eyelashes.
Summary of the invention
Europium fluorescent powder and preparation method thereof is mixed using barium phosphate sodium as matrix the object of the present invention is to provide a kind of.
Technical solution provided by the invention is to adulterate trivalent europium ion (Eu using barium phosphate sodium as matrix3+), chemical formula is
NaBa1-xPO4 : x Eu, wherein 0.01≤x≤0.05.
The present invention also provides the preparation methods of the fluorescent powder, and steps are as follows:
The first step, according to NaBa1-xPO4 : x Eu, wherein the mol ratio of 0.01≤x≤0.05 accurately weighs carbonic acid
Sodium, barium carbonate, ammonium dihydrogen phosphate and europium oxide.
Raw material load weighted in the first step is mixed in aluminium oxide mortar, is fully ground, obtains mixture by second step.
Mixture is carried out pre-burning by third step.
Sample after pre-burning is fully ground by the 4th step again, and high-temperature calcination is simultaneously kept the temperature, and grinding is somebody's turn to do after natural cooling
Fluorescent powder.
Further, milling time described in the first step is 20 min or more.
Calcined temperature described in third step is 600 DEG C, and soaking time is 2 h.
The heating rate of pre-burning described in third step is 5 DEG C/min.
Calcination temperature described in 4th step is 800 DEG C, and soaking time is 4 h.
The heating rate of calcining described in 4th step is 5 DEG C/min.
Detailed description of the invention
The present invention will be further described below with reference to the drawings.
Attached drawing 1 is the X-ray diffraction (XRD) figure spectrum of fluorescent powder prepared by embodiment 2.
Attached drawing 2 is excitation spectrum of the fluorescent powder of the preparation of embodiment 2 under the excitation of 360 nm wavelength.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments, but is not limited to model of the invention
It encloses, raw material used in embodiment is conventional raw material, can pass through commercially available acquisition；The method is existing unless otherwise specified
There is technology.
Embodiment 1
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
NaBa1-xPO4: x Eu, wherein x=0.01.
The preparation method of above-mentioned fluorescent powder, comprising steps of
The first step, according to the composition of above-mentioned fluorescent powder, 1.1316 g of precise sodium carbonate, 4.1294 g of barium carbonate, di(2-ethylhexyl)phosphate
0.0376 g of 2.7015 g of hydrogen ammonium and europium oxide.
Above-mentioned four kinds of raw materials are put into aluminium oxide mortar and grind 20 min by second step, are uniformly mixed raw material, are mixed
Close material；Obtained mixture is placed in corundum crucible, which is placed in Muffle furnace, is calcined in air atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C, 2 h are kept the temperature, room temperature is then cooled to, take out sample, grinding, then at air atmosphere
In with the heating rate of 5 DEG C/min be warming up to 800 DEG C, keep the temperature 4 h, take out sample after being cooled to room temperature, be fully ground, i.e.,
It is available to mix europium fluorescent powder using barium phosphate sodium as matrix.
Embodiment 2
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
NaBa1-xPO4: x Eu, wherein x=0.02.
The preparation method of above-mentioned fluorescent powder, comprising steps of
The first step, according to the composition of above-mentioned fluorescent powder, 1.1263 g of precise sodium carbonate, 4.1101 g of barium carbonate, di(2-ethylhexyl)phosphate
0.0748 g of 2.6889 g of hydrogen ammonium and europium oxide.
Above-mentioned four kinds of raw materials are put into aluminium oxide mortar and grind 20 min by second step, are uniformly mixed raw material, are mixed
Close material；Obtained mixture is placed in corundum crucible, which is placed in Muffle furnace, is calcined in air atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C, 2 h are kept the temperature, room temperature is then cooled to, take out sample, grinding, then at air atmosphere
In with the heating rate of 5 DEG C/min be warming up to 800 DEG C, keep the temperature 4 h, take out sample after being cooled to room temperature, be fully ground, i.e.,
It is available to mix europium fluorescent powder using barium phosphate sodium as matrix.
Embodiment 3
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
NaBa1-xPO4 : x Eu, wherein x=0.03.
The preparation method of above-mentioned fluorescent powder, comprising steps of
The first step, according to the composition of above-mentioned fluorescent powder, 1.1210 g of precise sodium carbonate, 4.0909 g of barium carbonate, di(2-ethylhexyl)phosphate
0.1117 g of 2.6764 g of hydrogen ammonium and europium oxide.
Above-mentioned four kinds of raw materials are put into aluminium oxide mortar and grind 20 min by second step, are uniformly mixed raw material, are mixed
Close material；Obtained mixture is placed in corundum crucible, which is placed in Muffle furnace, is calcined in air atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C, 2 h are kept the temperature, room temperature is then cooled to, take out sample, grinding, then at air atmosphere
In with the heating rate of 5 DEG C/min be warming up to 800 DEG C, keep the temperature 4 h, take out sample after being cooled to room temperature, be fully ground, i.e.,
It is available to mix europium fluorescent powder using barium phosphate sodium as matrix.
Embodiment 4
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
NaBa1-xPO4: x Eu, wherein x=0.04.
The preparation method of above-mentioned fluorescent powder, comprising steps of
The first step, according to the composition of above-mentioned fluorescent powder, 1.1158 g of precise sodium carbonate, 4.0720 g of barium carbonate, di(2-ethylhexyl)phosphate
0.1482 g of 2.6640 g of hydrogen ammonium and europium oxide.
Above-mentioned four kinds of raw materials are put into aluminium oxide mortar and grind 20 min by second step, are uniformly mixed raw material, are mixed
Close material；Obtained mixture is placed in corundum crucible, which is placed in Muffle furnace, is calcined in air atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C, 2 h are kept the temperature, room temperature is then cooled to, take out sample, grinding, then at air atmosphere
In with the heating rate of 5 DEG C/min be warming up to 800 DEG C, keep the temperature 4 h, take out sample after being cooled to room temperature, be fully ground, i.e.,
It is available to mix europium fluorescent powder using barium phosphate sodium as matrix.
Embodiment 5
It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
KBa1-xPO4: x Eu, wherein x=0.05.
The preparation method of above-mentioned fluorescent powder, comprising steps of
The first step, according to the composition of above-mentioned fluorescent powder, 1.1107 g of precise sodium carbonate, 4.0532 g of barium carbonate, di(2-ethylhexyl)phosphate
0.1844 g of 2.6517 g of hydrogen ammonium and europium oxide.
Above-mentioned four kinds of raw materials are put into aluminium oxide mortar and grind 20 min by second step, are uniformly mixed raw material, are mixed
Close material；Obtained mixture is placed in corundum crucible, which is placed in Muffle furnace, is calcined in air atmosphere, with 5
DEG C/heating rate of min rises to 600 DEG C, 2 h are kept the temperature, room temperature is then cooled to, take out sample, grinding, then at air atmosphere
In with the heating rate of 5 DEG C/min be warming up to 800 DEG C, keep the temperature 4 h, take out sample after being cooled to room temperature, be fully ground, i.e.,
It is available to mix europium fluorescent powder using barium phosphate sodium as matrix.
Performance comparison
The fluorescent powder that above-described embodiment 2 is obtained carries out X-ray diffraction (XRD) analysis, as shown in Fig. 1, what embodiment 2 obtained
Fluorescent powder, diffraction maximum and standard PDF#81-2250(NaBaPO4) corresponding.
The fluorescent powder that above-described embodiment 2 is obtained carries out fluorometric investigation, obtains fluorescent powder under the excitation of 360 nm wavelength
Excitation spectrum is as shown in Fig. 2.
The bound value of each raw material and each raw material cited by the present invention and the bound of each technological parameter take
Value, can realize the present invention, embodiment numerous to list herein.
Claims (8)
1. a kind of mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: using barium phosphate sodium as matrix, chemical formula is
NaBa1-xPO4 : x Eu, wherein 0.01≤x≤0.05.
2. a kind of preparation method of fluorescent powder for mixing europium using barium phosphate sodium as matrix according to claim 1, feature exist
In: specific preparation process is as follows:
The first step, according to NaBa1-xPO4 : x Eu, wherein the mol ratio of 0.01≤x≤0.05 accurately weighs carbonic acid
Sodium, barium carbonate, ammonium dihydrogen phosphate and europium oxide；
Raw material load weighted in the first step is mixed in aluminium oxide mortar, is fully ground, obtains mixture by second step；
Mixture is carried out pre-burning by third step；
Sample after pre-burning is fully ground by the 4th step again, and high-temperature calcination is simultaneously kept the temperature, and grinding obtains the fluorescence after natural cooling
Powder.
3. according to claim 2 using barium phosphate sodium as the preparation method for mixing europium fluorescent powder of matrix, it is characterised in that: the
Milling time described in two steps is 20 min or more.
4. according to claim 2 using barium phosphate sodium as the preparation method for mixing europium fluorescent powder of matrix, it is characterised in that: step
Calcined temperature described in third step is 600 DEG C, and soaking time is 2 h.
5. according to claim 2 or 4 using barium phosphate sodium as the preparation method for mixing europium fluorescent powder of matrix, feature exists
In: the heating rate of pre-burning described in third step is 5 DEG C/min.
6. according to claim 2 using barium phosphate sodium as the preparation method for mixing europium fluorescent powder of matrix, it is characterised in that: the
Calcination temperature described in four steps is 800 DEG C, and soaking time is 4 h.
7. using barium phosphate sodium as the preparation method for mixing europium fluorescent powder of matrix according to claim 2 or 6, feature exists
In: the heating rate of calcining described in the 4th step is 5 DEG C/min.
8. according to claim 2 mix europium fluorescent powder using barium phosphate sodium as matrix, it is characterised in that: by changing Eu3 + Content adjust fluorescent powder luminescent properties.
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| CN201811506980.7A CN109628090A (en) | 2018-12-10 | 2018-12-10 | It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix |
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| CN201811506980.7A CN109628090A (en) | 2018-12-10 | 2018-12-10 | It is a kind of to mix europium fluorescent powder using barium phosphate sodium as matrix |
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