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Submicron-scale lumpy calcium titanate based upconversion luminescent material and preparation method thereof

A luminescent material, submicron technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of high preparation temperature, uneven size, irregular shape, etc., and achieve stable physicochemical properties, uniform size, and regular shape. Effect

Inactive Publication Date: 2018-10-19
BEIHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims to solve the technical problems of uneven size, irregular shape, high preparation temperature and difficult doping in the preparation of calcium titanate-based rare earth up-conversion luminescent materials in the prior art, and provides a submicron-sized bulk calcium titanate-based up-conversion luminescent material. A conversion luminescent material and a preparation method thereof. The present invention adopts a solvothermal method to prepare a submicron block calcium titanate-based up-conversion luminescent material. The obtained material has strong green up-conversion luminescent properties, high purity, regular shape, uniform distribution, and is prepared The method is simple and easy

Method used

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  • Submicron-scale lumpy calcium titanate based upconversion luminescent material and preparation method thereof
  • Submicron-scale lumpy calcium titanate based upconversion luminescent material and preparation method thereof
  • Submicron-scale lumpy calcium titanate based upconversion luminescent material and preparation method thereof

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preparation example Construction

[0038] The invention provides a method for preparing a submicron block calcium titanate-based up-conversion luminescent material, comprising the following steps:

[0039] The chemical expression of the submicron bulk calcium titanate-based up-conversion luminescent material is Ca (1-x-y) TiO 3 :M 3+ x , Yb 3+ y ; where x and y are mole fractions of elements, and their value ranges are: 0.0001≤x≤0.10, 0.0001≤y≤0.20, and M is one of the rare earth elements Ho and Er;

[0040] Step 1, measure Ca(NO 3 ) 2 , Yb(NO 3 ) 3 , and Er(NO 3 ) 3 or Ho(NO 3 ) 3 , after mixing these three nitrates, add 16.27mL-17.22mL polyethylene glycol PEG-200, n(Ca 2+ +Yb 3+ +Er 3+ or Ho 3+ )=1mmol, prepared to obtain alcohol mixed solution;

[0041] Step 2. Add 0.33mL tetrabutyl titanate dropwise into the alcohol mixed solution prepared in step 1, and stir for 30min;

[0042] Step 3, adjust the mixed solution prepared in step 2 with an aqueous sodium hydroxide solution, the concentratio...

Embodiment 1

[0053] By expression Ca (1-x-y) TiO 3 :M 3+ x , Yb 3+ y , y=0.03, x=0.01, the stoichiometric ratio of each substance in the 50mL small beaker is respectively measured 240 μ L Ca(NO 3 ) 2 , 150μL Yb(NO 3 ) 3 , 50μL Er(NO 3 ) 3 , then add about 17.03mL polyethylene glycol PEG-200; add 0.33mL tetrabutyl titanate dropwise to the above mixture while stirring, stir for 30min, then add sodium hydroxide dropwise to the above mixture while stirring Aqueous solution 2.2mL, stirred for 30min, the obtained suspension was put into a hydrothermal reaction kettle at 180°C for 15 hours, cooled naturally, the precipitate was taken out by centrifugation, first with acetone, then with dilute acetic acid, and finally with absolute ethanol Wash by centrifugation 3 times. Put it in an oven and dry at 80°C for 15 hours to obtain the precipitate of the reactant precursor; put the precipitate of the reactant precursor into a corundum crucible and cover it, and place it in a high-temperature...

Embodiment 2

[0059] By expression Ca (1-x-y) TiO 3 :M 3+ x , Yb 3+ y , y=0.15, x=0.01, the stoichiometric ratio of each substance in the 50mL small beaker is respectively measured 210 μ L Ca(NO 3 ) 2 , 750 μL Yb (NO 3 ) 3 , 50μL Er(NO 3 ) 3 , then add about 16.46mL of polyethylene glycol PEG-200; add 0.33mL of tetrabutyl titanate dropwise to the above mixed solution while stirring, stir for 30min, then add sodium hydroxide dropwise to the above mixed solution while stirring Aqueous solution 2.2mL, stirred for 30min, the obtained suspension was put into a hydrothermal reaction kettle at 180°C for 15 hours, cooled naturally, the precipitate was taken out by centrifugation, first with acetone, then with dilute acetic acid, and finally with absolute ethanol Wash by centrifugation 3 times. Put it in an oven and dry at 80°C for 15 hours to obtain the precipitate of the reactant precursor; put the precipitate of the reactant precursor into a corundum crucible and cover it, and place it...

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Abstract

The invention belongs to the field of luminescent materials and relates to a submicron-scale lumpy calcium titanate based upconversion luminescent material and a preparation method thereof. The submicron-scale lumpy calcium titanate based upconversion luminescent material is used for solving the technical problem in the prior art that prepared calcium titanate based rare-earth upconversion luminescent materials are non-uniform in size, irregular in shape, high in preparation temperature and difficult in doping. According to the preparation method provided by the invention, the raw materials are cheap, the preparation process is simple and convenient, the operation is easy, the calcination temperature is low, and the production facilities are readily available. According to the upconversionluminescent material, the morphology, size and luminescent intensity of prepared rare-earth doped CaTiO3:Yb<3+> / Er<3+> or Ho<3+> can be regulated and controlled through changing a solvothermal environment, and the upconversion luminescent material is high in purity, uniform in size, regular in shape and relatively good in dispersity and has the average side length of 500 nm. Bright visible lightwith the wavelength of 400 nm to 750 nm can be viewed under the excitation of infrared light with the wavelength of 980 nm. Compared with calcium titanate upconversion luminescent materials prepared by the traditional methods, the upconversion luminescent material has the advantages that the light emitting brightness is further improved, and the material is stable in physico-chemical properties; the luminescence efficiency is also higher than that of commonly-used titanate materials.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a submicron block calcium titanate-based up-conversion luminescent material excited by infrared light and a preparation method thereof. Background technique [0002] Due to their stable physical and chemical properties, rich energy level structure and long energy level lifetime, rare earth ions can obtain rich photoluminescence properties under the excitation of near-infrared light, so they can be used as luminescent centers to be doped into appropriate matrix materials. middle. Rare earth up-conversion luminescent materials are important rare earth functional materials, among which rare earth doped titanate luminescent materials have been widely used in the fields of ceramics, laser technology and display technology. With the continuous deepening and development of research on rare earth materials, people put forward higher and higher requirements for ...

Claims

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Application Information

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IPC IPC(8): C09K11/67
CPCC09K11/7768
Inventor 牟佳佳何畅意管越孙伟杰陈力
Owner BEIHUA UNIV
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