CN111019654A - Auxiliary combustion method for preparing LaYAlO3: method for preparing Eu fluorescent powder material - Google Patents
Auxiliary combustion method for preparing LaYAlO3: method for preparing Eu fluorescent powder material Download PDFInfo
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- CN111019654A CN111019654A CN201911406567.8A CN201911406567A CN111019654A CN 111019654 A CN111019654 A CN 111019654A CN 201911406567 A CN201911406567 A CN 201911406567A CN 111019654 A CN111019654 A CN 111019654A
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- layalo
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- phosphor
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- 239000000843 powder Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 title abstract description 21
- 238000009841 combustion method Methods 0.000 title abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910003101 Y(NO3)3·6H2O Inorganic materials 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002339 La(NO3)3 Inorganic materials 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 229910002422 La(NO3)3·6H2O Inorganic materials 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 8
- 238000005286 illumination Methods 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- -1 rare earth ions Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000000333 X-ray scattering Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007850 fluorescent dye Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
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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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
Abstract
Auxiliary combustion method for preparing LaYAlO3: a method for preparing Eu fluorescent powder material, belonging to the field of nano luminescent material. LaYAlO3The chemical formula of the fluorescent powder material is La(0.5‑0.5x)Y(0.5‑0.5x)AlO3：EuxX is 0.01-0.06, and Al (NO)3)3·9H2O (analytically pure), Urea (99.99%), Eu (NO)3)3(99.99％)，Y(NO3)3·6H2O(99.99％)，La(NO3)3·6H2O (99.99%) is used as a raw material and is synthesized and prepared by an auxiliary combustion method; LaYAlO of the invention3The fluorescent powder material has higher absorption in an ultraviolet region.
Description
Technical Field
The invention relates to an auxiliary combustion method for preparing LaYAlO3: a method of Eu fluorescent powder, belonging to the field of nano luminescent material.
Background
Because the inorganic nano material doped with rare earth ions has excellent physical and chemical properties in the aspects of light, magnetism, heat, catalysis and the like, and meanwhile, the rare earth Eu ions are easily influenced by the surrounding environment, the nano material doped with the rare earth Eu ions is a hot spot of research of people all the time.
The rare earth ions have stable physicochemical properties, rich energy level structures and longer energy level service life, can be doped into a proper matrix material as a luminescent center, and have photoluminescence properties under the excitation of near ultraviolet or blue light. The rare earth luminescent material is an important rare earth functional material, and can be widely applied to the fields of illumination, display technology and the like. With the continuous deep research of rare earth luminescence and the development of scientific technology, people put forward higher and higher requirements on the performance of luminescent materials. Therefore, the search for a novel matrix material which is beneficial to doping of rare earth ions becomes an important research direction for improving the fluorescence performance.
Disclosure of Invention
The invention aims to provide a LaYAlO3: a preparation method of Eu fluorescent powder.
In order to achieve the above purpose, the solution of the invention is as follows:
the LaYAlO3: the chemical formula of the Eu fluorescent powder is La(0.5-0.5x)Y(0.5-0.5x)AlO3：EuxAnd x is 0.01-0.06, such as 0.01, 0.02, 0.04, 0.05, 0.06, preferably x is 0.05, i.e. the molar percent doping of Eu to La and Y is 100 x%.
Preparation of LaYAlO emitting light under excitation of X-ray and 254nm by auxiliary combustion method3: the method for preparing Eu fluorescent powder is characterized by comprising the following steps:
(1) with Al (NO)3)3·9H2O (analytically pure), Urea (99.99%), Eu (NO)3)3(99.99％)，Y(NO3)3·6H2O(99.99％)，La(NO3)3·6H2And O (99.99%) is used as a raw material, the corresponding raw material is weighed according to the metal molar ratio in the chemical formula of the fluorescent powder, urea is added, deionized water is added for stirring until solid particles are completely dissolved, the mixed solution is transparent, and the stirring is carried out for 2-3 minutes to fully mix reactants, wherein the total molar number of metal elements is as follows: the mole number of the urea is 1: (5-10);
(2) drying the mixed solution obtained in the step (1), placing the dried mixed solution in a muffle furnace preheated to 500-900 ℃, heating for 3-4 minutes, discharging flame, waiting for 8-12 seconds, taking out, and recovering to room temperature to obtain fluffy LaYAlO3: eu phosphor.
LaYAlO obtained by the technical scheme of the invention3: the Eu fluorescent powder can emit light under the excitation of X rays and 254 nm. The fluorescent label or the anti-counterfeiting ink is prepared by mixing glue or ink and the like by utilizing the characteristic that the fluorescent label or the anti-counterfeiting ink emits visible spectrum under specific excitation wavelength and is applied to the anti-counterfeiting field of printing and packaging.
Drawings
FIG. 1 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: and comparing the Eu fluorescent powder material sample under daily illumination with 254nm ultraviolet illumination, wherein the upper row is photos under the irradiation of a fluorescent lamp, and the lower row is photos under the irradiation of 254nm ultraviolet.
FIG. 2 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: an XRD spectrum of a Eu fluorescent powder material sample, wherein the doping concentration of Eu is 0%, 1%, 2%, 4%, 5%, 6%; the abscissa in the figure represents the diffraction angle 2 θ in degrees and the ordinate represents the relative intensity of diffraction.
FIG. 3 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: photoluminescence spectrum of Eu fluorescent powder material sample.
FIG. 4 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: the scanning electron microscope photo of the Eu fluorescent powder material sample shows that the doping concentration of europium is 5%.
FIG. 5 is an x-ray scattering spectrum of a 500 ℃ europium-doped sample in example 1 of the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
According to the chemical formula La(0.5-0.5x)Y(0.5-0.5x)AlO3：EuxThe molar ratio of each metal is weighed, and urea with the ratio of the total molar number of metal elements to the molar number of urea being 1:8 is weighed and placed in a crucible, in this example, LaYAlO3: the method for synthesizing the Eu fluorescent powder material comprises the following steps: placing the weighed materials in a crucible, adding 12ml of deionized water, and uniformly stirring for 3-5 minutesTransferring the crucible containing the solution to a muffle furnace preheated to 500 ℃ when the solution becomes transparent, keeping the temperature constant for 3-5 minutes at the temperature, instantly raising the temperature by a few degrees centigrade when a reaction system emits a large amount of heat, taking out the crucible when a temperature display returns to about 500 ℃, and naturally cooling to room temperature to obtain a material, namely LaYAlO3: eu phosphor material.
FIG. 1 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: a comparison graph of a Eu fluorescent powder material sample under daily illumination and 254nm ultraviolet illumination, wherein Eu doping concentration is 0%, 1%, 2%, 4%, 5% and 6% from left to right in sequence; LaYAlO3: the Eu fluorescent powder does not have any luminescence condition under the irradiation of daily light, the states of a plurality of samples are the same, but Eu is doped under the irradiation of 254nm ultraviolet light3+The sample (2) emits red light, and the sample with the doping concentration of 5% has the highest luminous intensity.
FIG. 2 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: the XRD spectrum of Eu fluorescent powder material sample, wherein the doping concentration of Eu is 0%, 1%, 2%, 4%, 5%, 6%, LaYAlO can be seen from the figure3: the Eu phosphor has high phase purity.
FIG. 3 shows LaYAlO obtained after a 500 ℃ heat treatment in example 1 of the present invention3: photoluminescence spectrum of Eu fluorescent powder material sample.
FIG. 4 shows a schematic view of a display device according to example 1 of the present invention
FIG. 5 is a graph showing the x-ray scattering spectrum of the 500 ℃ europium-doped sample of example 1.
Claims (4)
1. LaYAlO3: eu fluorescent powder characterized in that the chemical formula is La(0.5-0.5x)Y(0.5-0.5x)AlO3：EuxAnd x is 0.01-0.06, namely the molar doping percentage of Eu to La and Y is 100 x%.
2. A LaYAlO according to claim 13: a Eu phosphor, wherein x is 0.05.
3. Preparation of a LaYAlO according to claim 13: the method for preparing Eu fluorescent powder is characterized by comprising the following steps:
(1) with Al (NO)3)3·9H2O (analytically pure), Urea (99.99%), Eu (NO)3)3(99.99％)，Y(NO3)3·6H2O(99.99％)，La(NO3)3·6H2And O (99.99%) is used as a raw material, the corresponding raw material is weighed according to the metal molar ratio in the chemical formula of the fluorescent powder, urea is added, deionized water is added for stirring until solid particles are completely dissolved, the mixed solution is transparent, and the stirring is carried out for 2-3 minutes to fully mix reactants, wherein the total molar number of metal elements is as follows: the mole number of the urea is 1: (5-10);
(2) drying the mixed solution obtained in the step (1), placing the dried mixed solution in a muffle furnace preheated to 500-900 ℃, heating for 3-4 minutes, discharging flame, waiting for 8-12 seconds, taking out, and recovering to room temperature to obtain fluffy LaYAlO3: eu phosphor.
4. A LaYAlO according to claim 13: application of Eu phosphor, LaYAlO3: the Eu fluorescent powder emits light under the excitation of X rays and 254 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911406567.8A CN111019654A (en) | 2019-12-31 | 2019-12-31 | Auxiliary combustion method for preparing LaYAlO3: method for preparing Eu fluorescent powder material |
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| CN201911406567.8A CN111019654A (en) | 2019-12-31 | 2019-12-31 | Auxiliary combustion method for preparing LaYAlO3: method for preparing Eu fluorescent powder material |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576350A (en) * | 2003-06-13 | 2005-02-09 | 松下电器产业株式会社 | Phosphors and related manufacturing method, display device, and fluorescent lamp |
| CN102477299A (en) * | 2010-11-30 | 2012-05-30 | 海洋王照明科技股份有限公司 | Lanthanum aluminate luminescent material and preparation method thereof |
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2019
- 2019-12-31 CN CN201911406567.8A patent/CN111019654A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576350A (en) * | 2003-06-13 | 2005-02-09 | 松下电器产业株式会社 | Phosphors and related manufacturing method, display device, and fluorescent lamp |
| CN102477299A (en) * | 2010-11-30 | 2012-05-30 | 海洋王照明科技股份有限公司 | Lanthanum aluminate luminescent material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ZHENXING FU, ET AL.: "Solution combustion synthesis, photoluminescence and X-ray luminescence of Eu3+-doped LaAlO3 nanophosphors", 《CERAMICS INTERNATIONAL》 * |
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Application publication date: 20200417 |
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