CN104418869A - Preparation method of rare-earth luminescent material containing Eu<3+> - Google Patents
Preparation method of rare-earth luminescent material containing Eu<3+> Download PDFInfo
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- CN104418869A CN104418869A CN201310405456.1A CN201310405456A CN104418869A CN 104418869 A CN104418869 A CN 104418869A CN 201310405456 A CN201310405456 A CN 201310405456A CN 104418869 A CN104418869 A CN 104418869A
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- solution
- preparation
- luminescent material
- rare earth
- rare
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 35
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 claims description 18
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- -1 rare earth nitrate Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 2
- CASFCVRUBIJLBN-UHFFFAOYSA-N 2-(1,10-phenanthrolin-2-yl)ethanol Chemical compound OCCc1ccc2ccc3cccnc3c2n1 CASFCVRUBIJLBN-UHFFFAOYSA-N 0.000 abstract 1
- PVYNVFAWOJTPKB-UHFFFAOYSA-N C(C)O.C1(=CC=C(C=C1)C(=O)O)C Chemical compound C(C)O.C1(=CC=C(C=C1)C(=O)O)C PVYNVFAWOJTPKB-UHFFFAOYSA-N 0.000 abstract 1
- 229910016644 EuCl3 Inorganic materials 0.000 abstract 1
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- 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
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- 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
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/182—Metal complexes of the rare earth metals, i.e. Sc, Y or lanthanide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a preparation method of a rare-earth luminescent material containing Eu<3+>. The preparation method comprises the following steps: (1) preparing rare-earth Eu nitrate; (2) preparing a EuCl3 solution; (3) preparing a phenanthroline ethanol solution; (4) preparing a p-toluic acid ethanol solution; and (5) preparing the rare-earth luminescent material containing Eu<3+>. By the preparation method, the rare-earth luminescent material containing Eu<3+> is successfully prepared. The prepared organic rare-earth luminescent material has particle diameter of about 100nm, stable structure, excellent thermodynamic properties and fluorescence properties and a melting point of 173 DEG C and is decomposed at 335 DEG C in a fastest manner. The rare-earth luminescent material has broad application prospects in agricultural luminescent materials, fluorescent decorative materials, fluorescent anti-counterfeit materials and luminescent fibers.
Description
Technical field
The present invention relates to a kind of preparation of rare earth luminescent material, particularly a kind of Eu
3+the preparation method of rare earth luminescent material.
Background technology
Current luminescent material and the research of laserable material, in the practical application of national economy and national security, account for leading and most important position.After entering the new millennium, rare earth luminescent material Science and Technology becomes prevailing flat pannel display from now on, the new lighting source of forth generation, modern medical service electronics, the development of the new and high technologies such as more advanced opticfiber communication and innovate reliable basisandguarantee.So fully comprehensive utilization China's rare earth resources storehouse, developing rare earth luminous (fluorescence) material is concrete important channel China's rare earth resources advantage being converted into economy and technical superiority.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method providing a kind of rare earth luminescent material.
Technical scheme of the present invention is:
A kind of containing Eu
3+the preparation method of rare earth luminescent material, comprise the following steps, the preparation of (1) rare earth Eu nitrate: take rare earth Eu oxide compound and be placed in beaker, add the dense HNO of 1:1 little over amount
3dissolve, be evaporated to dry at 50 ~ 60 DEG C, obtain required rare earth nitrate; (2) EuCl
3the preparation of solution: by a certain amount of Eu (NO)
3be dissolved in the EuCl obtaining 0.2mol/L in the ethanol of a certain amount of 99.7%
3solution (solution 1); (3) preparation of phenanthroline ethanolic soln: by l, 10-phenanthroline is dissolved in the ethanol of 99.7% and obtains 0.1mol/L phenanthroline ethanolic soln (solution 2); (4) preparation of p-methylbenzoic acid ethanolic soln: be dissolved in by p-methylbenzoic acid in the ethanol of 99.7%, is stirred to and dissolves completely under 50 DEG C of conditions, and by its pH value ammoniacal liquor (25 ~ 28%NH
3) be adjusted to 10, obtain 0.05mol/L p-methylbenzoic acid ethanolic soln (solution 3); (5) Eu
3+the preparation of rare earth luminescent material: solution 1 and solution 2 stir 30min under 50 DEG C of conditions, then add solution 3, continue to stir left at room temperature 24h after 2h under 50 DEG C of conditions, filter, respectively wash 5 times with ethanol and distilled water, dry in 80 DEG C of vacuum drying ovens, obtain white solid powder, be Eu
3+rare earth luminescent material.
At Eu
3+the preparation of rare earth luminescent material time, solution 1: solution 2: solution 3 is 1:4:12.
The present invention successfully prepares containing Eu
3+rare earth luminescent material.The organic RE luminescent material grains diameter of preparation is approximately 1OOnm, and there is stable structure, excellent thermodynamic property and photoluminescent property, fusing point is 173 DEG C, decompose the fastest 335 DEG C time, this kind of rare earth luminescent material has broad application prospects in agricultural luminescent material, fluorescent decoration material, fluorescence falsification preventing material, luminescent fibre.
embodiment:
A kind of containing Eu
3+the preparation method of rare earth luminescent material, comprise the following steps:
(1) preparation of rare earth Eu nitrate: take rare earth Eu oxide compound and be placed in beaker, adds the dense HNO of 1:1 little over amount
3dissolve, be evaporated to dry at 50 ~ 60 DEG C, obtain required rare earth nitrate;
(2) EuCl
3the preparation of solution: the Eu (NO) of the 1mmol that step (1) is configured
3be dissolved in the EuCl obtaining 0.2mol/L in the ethanol of 99.7% of 5ml
3solution (solution 1);
(3) preparation of phenanthroline ethanolic soln: by 2mmol l, 10-phenanthroline is dissolved in the ethanol of 20ml99.7% and obtains 0.1mol/L phenanthroline ethanolic soln (solution 2);
(4) preparation of p-methylbenzoic acid ethanolic soln: be dissolved in the ethanol of 60ml99.7% by 3mmol p-methylbenzoic acid, is stirred to and dissolves completely under 50 DEG C of conditions, and by its pH value ammoniacal liquor (25 ~ 28%NH
3) be adjusted to 10, obtain 0.05mol/L p-methylbenzoic acid ethanolic soln (solution 3);
(5) Eu
3+the preparation of rare earth luminescent material: solution 1 and solution 2 stir 30min under 50 DEG C of conditions, then add solution 3, continue to stir left at room temperature 24h after 2h under 50 DEG C of conditions, filter, respectively wash 5 times with ethanol and distilled water, dry in 80 DEG C of vacuum drying ovens, obtain white solid powder, be Eu
3+rare earth luminescent material;
(6) the organic RE luminescent material grains diameter prepared is approximately 1OOnm, and has stable structure, excellent thermodynamic property and photoluminescent property, and fusing point is 173 DEG C, decomposes the fastest 335 DEG C time.
Claims (2)
1. one kind contains Eu
3+the preparation method of rare earth luminescent material, it is characterized in that: comprise the following steps, the preparation of (1) rare earth Eu nitrate: take rare earth Eu oxide compound and be placed in beaker, add the dense HNO of 1:1 little over amount
3dissolve, be evaporated to dry at 50 ~ 60 DEG C, obtain required rare earth nitrate; (2) EuCl
3the preparation of solution: by a certain amount of Eu (NO)
3be dissolved in the EuCl obtaining 0.2mol/L in the ethanol of a certain amount of 99.7%
3solution (solution 1); (3) preparation of phenanthroline ethanolic soln: by l, 10-phenanthroline is dissolved in the ethanol of 99.7% and obtains 0.1mol/L phenanthroline ethanolic soln (solution 2); (4) preparation of p-methylbenzoic acid ethanolic soln: be dissolved in by p-methylbenzoic acid in the ethanol of 99.7%, is stirred to and dissolves completely under 50 DEG C of conditions, and by its pH value ammoniacal liquor (25 ~ 28%NH
3) be adjusted to 10, obtain 0.05mol/L p-methylbenzoic acid ethanolic soln (solution 3); (5) Eu
3+the preparation of rare earth luminescent material: solution 1 and solution 2 stir 30min under 50 DEG C of conditions, then add solution 3, continue to stir left at room temperature 24h after 2h under 50 DEG C of conditions, filter, respectively wash 5 times with ethanol and distilled water, dry in 80 DEG C of vacuum drying ovens, obtain white solid powder, be Eu
3+rare earth luminescent material.
2. technique according to claim 1, is characterized in that: at Eu
3+the preparation of rare earth luminescent material time, volume proportion solution 1: solution 2: solution 3 is 1:4:12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310405456.1A CN104418869A (en) | 2013-09-09 | 2013-09-09 | Preparation method of rare-earth luminescent material containing Eu<3+> |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310405456.1A CN104418869A (en) | 2013-09-09 | 2013-09-09 | Preparation method of rare-earth luminescent material containing Eu<3+> |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104418869A true CN104418869A (en) | 2015-03-18 |
Family
ID=52969065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310405456.1A Pending CN104418869A (en) | 2013-09-09 | 2013-09-09 | Preparation method of rare-earth luminescent material containing Eu<3+> |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104418869A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750357A (en) * | 2017-01-11 | 2017-05-31 | 重庆师范大学 | A kind of rare earth polymer green fluorescent material and preparation method thereof |
| CN106757412A (en) * | 2016-11-09 | 2017-05-31 | 大连工业大学 | A kind of method that application rare earth compounding prepares nano fluorescence fiber material |
| CN110862547A (en) * | 2019-11-13 | 2020-03-06 | 华中科技大学 | Rare earth supermolecule gel luminescent material, preparation and application thereof |
-
2013
- 2013-09-09 CN CN201310405456.1A patent/CN104418869A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757412A (en) * | 2016-11-09 | 2017-05-31 | 大连工业大学 | A kind of method that application rare earth compounding prepares nano fluorescence fiber material |
| CN106757412B (en) * | 2016-11-09 | 2018-11-16 | 大连工业大学 | A method of nano fluorescence fiber material is prepared using rare earth compounding |
| CN106750357A (en) * | 2017-01-11 | 2017-05-31 | 重庆师范大学 | A kind of rare earth polymer green fluorescent material and preparation method thereof |
| CN110862547A (en) * | 2019-11-13 | 2020-03-06 | 华中科技大学 | Rare earth supermolecule gel luminescent material, preparation and application thereof |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150318 |
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| WD01 | Invention patent application deemed withdrawn after publication |