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A kind of tricolor block copolymer type white light phosphor and preparation method thereof

A technology of block copolymers and three primary colors, applied in chemical instruments and methods, luminescent materials, sustainable buildings, etc., can solve the problems of difficult separation and removal of metal catalysts, affecting luminous efficiency, destroying complex structures, etc., achieving LED The chip process is convenient to manufacture, avoids phase separation, and enhances the fluorescence intensity.

Active Publication Date: 2016-03-16
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation of block copolymers by the ATRP method, it is difficult to separate and remove the metal catalyst in the later stage, that is, the purification of the product becomes a problem that cannot be ignored; in addition, since the trichromatic complex involves a rare earth complex, adding metal ions will capture the complex The ligands in it preferentially coordinate with it to destroy the structure of the complex and affect the luminous efficiency

Method used

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  • A kind of tricolor block copolymer type white light phosphor and preparation method thereof
  • A kind of tricolor block copolymer type white light phosphor and preparation method thereof
  • A kind of tricolor block copolymer type white light phosphor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Preparation of europium red light complex Eu(TTA) 3 (MAA)

[0037]Add 10 mL of 0.2 mol / L ethanol solution of 2-thienoyltrifluoroacetone into the reaction vessel, drop 5 mL of 0.2 mol / L europium chloride ethanol solution at a rate of 1 mL / min, adjust the pH value of the solution to 4-5, and heat Stir and react at 55°C for 30 minutes, then add 5 mL of 0.2 mol / L o-phenanthroline ethanol solution dropwise at a rate of 1 mL / min, and finally add 5 mL of 0.2 mol / L ethanol solution of methacrylic acid dropwise at a rate of 1 mL / min, Adjust the pH value of the solution to 6.5-7.0, continue to react for 180 min while stirring, and stop heating. Suction filtration, the filter cake was washed with absolute ethanol to remove unreacted ligands, and dried in a vacuum oven to obtain the europium red complex Eu(C 8 h 5 f 3 o 2 S) 2 (C 12 h 8 N 2 )(C 4 h 5 o 2 ) 0.7118g, yield 65%.

[0038] 2. Preparation of terbium green light complex Tb(p-ABA) 3 MAA

[0039] Add 15 mL...

Embodiment 2

[0050] 1. The preparation of europium red light complex and beryllium blue light complex is the same as in Example 1.

[0051] 2. Preparation of terbium green light complex Tb(o-ABA) 3 MAA

[0052] Add 15 mL of 0.2 mol / L ethanol solution of anthranilic acid and 5 mL of 0.2 mol / L ethanol solution of methacrylic acid into the reaction vessel, adjust the pH value to 5.5-6.5 with sodium alkoxide, heat to 55°C and stir for 10 min, then add 1 mL Add 5 mL of 0.2 mol / L terbium chloride ethanol solution at a drop rate of 1 / min, adjust the pH value with sodium alkoxide to keep it in a coordination environment of 5.5-6.5, continue the reaction for 180 min, and stop heating. Suction filtration, the filter cake was washed with absolute ethanol to remove unreacted ligands, and placed in a vacuum oven to dry to obtain the terbium green light complex Tb(C 7 h 6 NO 2 ) 3 (C 4 h 5 o 2 ) 0.5312g, yield 61%.

[0053] 3. Preparation of red, green and blue tri-color tri-block copolymer whi...

Embodiment 3

[0059] 1. The preparation of terbium green light complex and beryllium blue light complex is the same as in Example 1.

[0060] 2. Preparation of europium red light complexes

[0061] Add 10 mL of 0.2 mol / L ethanol solution of 2,4-hexanedione into the reaction vessel, drop 5 mL of 0.2 mol / L europium chloride ethanol solution at a rate of 1 mL / min, adjust the pH value of the solution to 4-5, and heat to Stir and react at 55°C for 30min, then add 5mL of 0.2mol / L ethanol solution of phenanthroline dropwise at a rate of 1mL / min, and finally add 5mL of ethanol solution of 0.2mol / L methacrylic acid dropwise at a rate of 1mL / min. The pH value of the solution was 6.5-7.0, and the reaction was continued for 180 minutes under stirring, and the heating was stopped. Suction filtration, the filter cake was washed with absolute ethanol to remove unreacted ligands, and dried in a vacuum oven to obtain the europium red complex Eu(C 8 h 10 o 2 ) 2 (C 12 h 8 N 2 )(C 4 h 5 o 2 ) 0.4834g...

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Abstract

The invention relates to a tri-phosphor block copolymer type white phosphor powder and a preparation method thereof. The red, green and blue single-phosphor complexes respectively copolymerize with styrene to form a macromolecular precursor, and under the action of trisulfide functionalization cross-linking agent, the macromolecular precursor forms the locally-random wholly-block copolymer with a structure of formula (I), wherein the relative molecular weight of the copolymer is 2.8*10<3>-5.3*10<3>, and the relative molecular weight distribution index is 1.3-1.5. The tri-phosphor block copolymer type white phosphor powder eliminates the fluorescence quenching phenomenon of the tri-phosphor doped macromolecular phosphor powder, solves the problem that the glass transition temperature of the phosphor powder is lower than the using temperature of LEDs, and the fluorescence is enhanced. The tri-phosphor phosphor powder is bonded in one large macromolecular chain to be used as a single-structure light emitting layer, and furthermore the phase separation is avoided, and later the production of LED chips is facilitated.

Description

technical field [0001] The invention relates to a preparation method of red, green and blue trichromatic block copolymer type white light fluorescent powder, which belongs to the technical field of preparation and application of luminescent materials. Background technique [0002] White LEDs have the advantages of small size, low energy consumption, and long life, and are called the fourth-generation green light source. The mainstream solution to realize white light LED is to combine LED chips with three-primary-color phosphors, and use ultraviolet semiconductor LED chips to excite three-primary-color phosphors to realize white light illumination. [0003] The current three-primary-color phosphors use the reactive three-primary-color complex phosphors and the polymer monomer methyl methacrylate (MMA) to bond respectively to prepare red, green and blue three-primary-color polymer phosphors, and then according to The ratio adopts the solvent blending method to mix the three p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F212/08C08F2/38C09K11/06
CPCY02B20/00
Inventor 贾虎生张爱琴李利平王淑华刘旭光许并社
Owner TAIYUAN UNIV OF TECH