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Method for preparing material convertible in water-solubility

A conversion material, water-soluble technology, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of high gas conduction and anti-explosion capability, high pressure and temperature requirements, expensive equipment, etc., and achieves a simple and economical preparation process. Time, good repeatability, easy to operate effect

Inactive Publication Date: 2005-12-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The former of the above two methods is time-consuming, requires high pressure and temperature, and expensive equipment
The latter method requires higher airtightness, gas conduction and explosion-proof capabilities of the device because of the generation of toxic gases such as nitrogen dioxide.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1, get 1.074g Y (NO 3 ) 3 ·5H 2 Dissolve O in 30ml water, then add 0.002~0.1g Er(AC) 3 and 0.02~0.2g Yb(AC) 3 dissolve. Add base to dissolve and heat on microwave. The power of the microwave is a certain value less than 400W. The heating time is 2.5 minutes to obtain a sol, which is centrifuged to obtain a gel. After washing with ethanol, it can be dried in an oven at 60°C for 5 hours, and then fired at 1000°C for 1 hour to obtain a water-soluble up-conversion material.

Embodiment 2

[0015] Embodiment 2, by the operating process of embodiment 1, by adjusting Y(NO 3 ) 3 ·5H 2 O, Er(AC) 3 and Yb(AC) 3 The ratio of the three realizes the control of the up-conversion luminous color. Taking the amount of Y as 100 mol%, taking 0.1-1 mol% of Er and 1-5 mol% of Yb, a green fluorescent water-soluble up-conversion material can be obtained. By taking 1-5 mol% of Er and 5-10 mol% of Yb, a water-soluble up-conversion material with red fluorescence can be obtained. By taking 5-10 mol% of Er and 10-20 mol% of Yb, a water-soluble up-conversion material with yellow fluorescence can be obtained.

Embodiment 3

[0016] Example 3, during the operation of Example 1, 1 g of EDTA (ethylenediaminetetraacetic acid) was added to the mixture before microwave heating, and the particle size obtained was about 50-100 nm.

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Abstract

The preparation method of the water-soluble up-conversion material of the invention belongs to the preparation process of nano fluorescent materials. With yttrium nitrate, rare earth acetate Er(AC) 3 and Yb(AC) 3 As a precursor, the synthesis process includes mixing materials - microwave heating - gel preparation - high temperature water removal. Mix yttrium nitrate with rare earth acetate to be doped in proportion; heat under 100-400W microwave power for 1-3 minutes to obtain sol; centrifuge and remove water at high temperature to obtain soluble up-conversion nanocrystalline powder. The material prepared by the method has the characteristics of dispersing in water and alcohol, high luminous efficiency, controllable luminous color, and can still emit high-intensity visible light under the excitation of a 980nm semiconductor laser after being dispersed in water; the method has the advantages of low cost, simple device, The advantages of convenient operation and good repeatability provide a reliable method for industrial production.

Description

technical field [0001] The invention belongs to the preparation technology of nano fluorescent material, in particular to the technology method of using microwave to prepare up-conversion material of rare earth doped oxide. Background technique [0002] Up-conversion fluorescent material is a kind of luminescent material that can emit visible light under the excitation of infrared light. Y 2 o 3 :Er 3+ , Yb 3+ It is a high-efficiency up-conversion fluorescent material, which emits bright red, yellow, and green light under the excitation of 980nm excitation light. It is mainly suitable for anti-counterfeiting of commodities, trademarks, securities, etc., and is also widely used in optical fiber communication, biological, medical testing and other fields. [0003] The prior art close to the present invention is the preparation Y introduced by document Chem.Mater.2002.14.2915-2921 2 o 3 There are two methods for up-conversion materials, one is solid-state reaction, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/78
Inventor 贾若琨白玉白李铁津
Owner JILIN UNIV
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