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Preparation method of rare earth doped zirconia fluorescent marking material, product and application thereof

A technology of zirconium dioxide and fluorescent labeling, which is applied in the field of luminescent materials in luminescence physics, can solve the problems of concentration quenching, reduction of fluorescence emission intensity, interaction enhancement, etc., and achieve low cost, easy operation, and uniform particle distribution Effect

Active Publication Date: 2020-07-24
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the doping concentration is too high, due to the shortening of the distance between the rare earth ions and the strengthening of the interaction, the rare earth ions at a high energy level can easily transfer their energy to the host material through surface defects, thereby reducing the fluorescence emission intensity, which is the concentration Quenching phenomenon

Method used

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  • Preparation method of rare earth doped zirconia fluorescent marking material, product and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 0.2 mol zirconium salt ZrOCl 2 ﹒ 8H 2 O and 0.01mol erbium salt Er(ClO 4 ) 3 Add it into 15ml of deionized water, stir magnetically to dissolve the salt completely, then add acetic acid according to the molar ratio of the total molar amount of metal ions to the solvent amount of 1:100, and add reaction butenedioic acid to form a transparent solution, and magnetic stirring was carried out to make the solution evenly mixed, and the obtained solution was transferred into a glass bottle with a Teflon cap. Put the glass bottle containing the solution into a hydrothermal kettle that has been preheated at 120°C, and keep the temperature at a constant temperature for 24 hours. After the reaction, collect the reaction product, that is, the crystals at the bottom of the bottle, wash the crystals once with deionized water and ethanol, and dry them at room temperature to obtain Er-Zr-MOF powder. When the powder is excited by a 280nm laser, the luminescence peak is 620nm. No c...

Embodiment 2

[0023] 0.2 mol zirconium salt ZrOCl2﹒8H2O and 0.02mol erbium salt Er(ClO4) 3 Add it into 15ml of deionized water, stir magnetically to dissolve the salt completely, then add acetic acid according to the molar ratio of the total molar amount of metal ions to the solvent amount of 1:120, and add reaction butenedioic acid to form a transparent solution, and magnetic stirring was carried out to make the solution evenly mixed, and the obtained solution was transferred into a glass bottle with a Teflon cap. Put the glass bottle containing the solution into a preheated 120°C hydrothermal kettle, and keep the temperature at a constant temperature for 28 hours. After the reaction, collect the reaction product, that is, the crystals at the bottom of the bottle, wash the crystals once with deionized water and ethanol, and dry them at room temperature to obtain Er-Zr-MOF powder. When the powder is excited by a 280nm laser, the luminescence peak is 630nm. No concentration quenching pheno...

Embodiment 3

[0025] Add 0.2 mol of zirconium salt ZrOCl2.8H2O and 0.06 mol of erbium salt Er(ClO4)3 into 15ml of deionized water, stir magnetically to dissolve the salt completely, and then add Acetic acid, add fumaric acid according to the molar ratio of metal ion molar amount and solvent amount as 1:3, form a transparent solution, carry out magnetic stirring to make the solution mix evenly, transfer the obtained solution into a glass with a Teflon bottle cap in the bottle. Put the glass bottle containing the solution into a hydrothermal kettle that has been preheated at 120°C, and keep the temperature at a constant temperature for 36 hours. After the reaction, collect the reaction product, that is, the crystals at the bottom of the bottle, wash the crystals once with deionized water and ethanol, and dry them at room temperature to obtain Er-Zr-MOF powder. Under the excitation of 280nm laser, the powder has a luminescence peak of 610nm. No concentration quenching phenomenon occurred.

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Abstract

The invention provides a preparation method of a rare earth doping zirconium dioxide fluorescence labeling material as well as a product and application thereof. Zirconium salt and erbium salt are added into deionized water to be dissolved according to the mol ratio; acetic acid and trans-butene diacid are added; the obtained solution is transferred into a glass bottle with a Teflon bottle cap; aglass bottle containing a solution is put into a preheated 120 DEG C hydrothermal kettle; the constant temperature maintenance is performed for 24 to 36 hours; after taking out, reaction products arecollected and are crystals at the bottle bottom. The crystals are sequentially washed once respectively by deionized water and ethanol; drying is performed at room temperature; Er-Zr-MOF powder is obtained. The method has the advantages that the process is simple; the cost is low; the operation is easy. The obtained powder has the smaller particle diameter; the particle distribution is uniform; the specific surface area is larger; more surface state is realized; more luminous centers can be accommodated; the illumination efficiency is higher. The luminous powder is excited by laser being 280 nm; the luminous peak is about 630 nm.

Description

technical field [0001] The invention relates to a preparation method of a nano fluorescent marking material, more precisely to a preparation method of a rare earth-doped zirconia fluorescent marking material and its product and application, belonging to the field of luminescent materials in luminescence physics. Background technique [0002] Rare earths are a huge treasure trove of luminescent materials. Whether rare earth elements are used as the matrix part of luminescent (fluorescent) materials, or as activators, co-activators, sensitizers or dopants, the luminescent materials made Generally collectively referred to as rare earth luminescent materials or rare earth fluorescent materials. Because there are 4f orbitals in the electron configuration of the rare earth element atoms, when the 4f electrons jump from a high energy level to a low energy level by radiative galloping, they emit light of different wavelengths. Rare earth element atoms have abundant electronic energ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/00C09K11/06C09K11/77H01L33/50
CPCC09K11/06C09K11/77C09K2211/183H01L33/502
Inventor 何丹农卢玉英张芳吴晓燕段磊李敏金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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