Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof

A fluorescent nanomaterial and rare earth up-conversion technology, which is applied in the direction of luminescent materials, chemical instruments and methods, can solve the problems of low ion doping concentration and low luminous efficiency of rare earth luminescent centers, and achieve small particle size, uniform distribution, and absorption The effect of section enhancement

Inactive Publication Date: 2016-03-23
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of low doping concentration and low luminous efficiency of rare earth luminescent center ions in the existing up-conversion fluorescent materials, and to provide a highly doped multi-band excitation rare earth up-conversion fluorescent nanomaterial and its Preparation

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  • Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof
  • Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof
  • Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof

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preparation example Construction

[0036] The present invention also provides a preparation method of highly doped multi-band excitation rare earth up-conversion fluorescent nanomaterials, including:

[0037] Step 1: Preparation of NaErF whose rare earth luminescence center ion is Er ion 4 Nano core structure; the doping concentration of the Er ion is 20%-100%;

[0038] Step 2: Cool down the nano-core structure obtained in Step 1, add an inert shell to react, form an inert shell outside the core structure, and obtain a highly doped multi-band excited rare earth up-conversion fluorescent nanomaterial.

[0039] According to the present invention, prepare the NaErF whose rare earth luminescence center ion is Er ion 4 The method of nano-nucleus structure is a method well known to those skilled in the art. It is preferred to use the chloride-oleic acid precursor method to first prepare the precursor of luminescent nuclear nanoparticles, and then add NH 4 The methanol solution of F and NaOH reacts at 300°C to 320°C...

Embodiment 1

[0042] Example 1: NaErF 4 NaYF 4

[0043] (1) Luminescent nucleus NaErF 4 Preparation of precursors:

[0044] In a three-necked flask, 0.382 g of ErCl 3 Dissolve in 6ml of oleic acid and 15ml of octadecene, deoxygenate for 30 minutes under the protection of argon, gradually raise the temperature to 150°C and stir for 30 minutes to obtain the precursor solution;

[0045] (2) When the precursor solution in (1) drops to room temperature, add 5ml containing 0.148g NH 4 F and 0.1 g of NaOH in methanol solution, gradually warming up to 80°C and stirring for 30 minutes, removing methanol, then gradually raising the temperature to 320°C, the heating rate is about 10°C / min, stirring and maintaining the reaction for 90 minutes to form NaErF 4 luminous nucleus;

[0046] (3) centrifugal separation, and with acetone, ethanol ultrasonic washing, the NaErF in (2) 4 The luminescent nucleus is dispersed in 4ml of cyclohexane to obtain a cyclohexane solution containing the upconversion n...

Embodiment 2

[0056] Example 2: NaGdF 4 :80%ErNaGdF 4

[0057] (1) Luminescent nucleus NaGdF 4 : Preparation of 80% Er precursor:

[0058] In a three-necked flask, 0.0607 g of GdCl 3 , 0.304 g ErCl 3 Dissolve in 6ml of oleic acid and 15ml of octadecene, deoxygenate for 30 minutes under the protection of argon, gradually raise the temperature to 150°C and stir for 30 minutes to obtain the precursor solution;

[0059] (2) When the precursor solution in (1) drops to room temperature, add 5ml containing 0.148g NH 4 F and 0.1 g of NaOH in methanol solution, gradually warming up to 80°C and stirring for 30 minutes to remove methanol. Then gradually raise the temperature to 320°C, the heating rate is about 10°C / min, stir and keep the reaction for 90 minutes to form NaGdF 4 : 80% Er luminescent nucleus;

[0060] (3) centrifugal separation, and ultrasonic washing with acetone and ethanol, the NaGdF obtained in (2) 4 : 80% Er luminescent nucleus is dispersed in 4ml cyclohexane, obtains the c...

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Abstract

The invention provides a highly-doped multi-band excitation rare earth upconversion fluorescence nano material and a preparation method thereof, belonging to the technical field of luminescent material structural design and preparation thereof, and solving the problems that an existing upconversion fluorescence material is low in rare earth luminescence center ion doping concentration and low in luminous efficiency. The material takes NaYF4, NaGdF4 or NaLuF4 as a substrate, is doped with rare earth luminescence center ions and is in a nanocrystalline micro-structure, and a nano core structure is externally coated with an inert shell structure; the rare earth luminescence center ions are Er3<+>, and the doping concentration is 20 percent to 100 percent. The invention also provides the preparation method of the highly-doped multi-band excitation rare earth upconversion fluorescence nano material. The nano material can realize nearly monochromatic upconversion fluorescence under three excitation wavelengths of 800nm, 980nm and 1530nm, and the optimal doping concentration of the singly doped rare earth luminescence center ions Er3<+> is increased to 100 percent.

Description

technical field [0001] The invention belongs to the technical field of structural design and preparation of luminescent materials, and in particular relates to a highly doped multi-band excitation rare earth up-conversion fluorescent nanometer material and a preparation method thereof. Background technique [0002] At present, human society is beginning to face energy shortages and the overwhelming medical costs due to the increasing life expectancy. Sustainable development (clean energy) and effective and economical medical security have become the priority public relations direction of science and technology. Because nanometers are between molecules and bulk materials, nanomaterials have some special properties while retaining molecular and bulk material properties (such as energy band structure), for example, the influence of surface properties / structures on physical / chemical properties of materials Modulation of material properties by large, core-shell structures has bec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
CPCC09K11/7772C09K11/7707
Inventor 涂浪平佐婧刘晓敏孔祥贵张友林常钰磊薛彬
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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