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Up converting fluorescent material with nanometer level molybdate substrate and its prepn

A fluorescent material and nano-level technology, applied in the field of nano fluorescent materials, can solve the problems of difficulty in preparing materials, no preparation, etc., and achieve the effects of cheap raw materials, low cost and simple process

Inactive Publication Date: 2002-05-08
CAPITALBIO CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned high-temperature solid-phase method prepares ordinary materials rather than nanomaterials. At present, there are no literature reports on the preparation methods of nanomaterials for such substances. The existing methods are difficult to prepare materials that meet the requirements of biomolecular markers.
In addition, the existing up-conversion fluorescent materials based on molybdate are only doped with ytterbium and erbium, and there are no reports on the preparation of co-doped molybdate up-conversion fluorescent materials such as ytterbium thulium and ytterbium holmium.

Method used

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  • Up converting fluorescent material with nanometer level molybdate substrate and its prepn
  • Up converting fluorescent material with nanometer level molybdate substrate and its prepn
  • Up converting fluorescent material with nanometer level molybdate substrate and its prepn

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Weigh 1.1760g lanthanum oxide (La 2 o 3 ), 0.3692g ytterbium oxide (Yb 2 0 3 ), 0.0537g erbium oxide (Er 2 o 3 ), placed in a 100ml beaker, add 2ml concentrated nitric acid (HNO 3 ) is heated and dissolved, and the molar ratio of rare earth ions is La 3+ :Yb 3+ :Er 3+ =77:20:3, evaporate to dryness, remove the remaining HNO 3 ;

[0025] (2) Add 30ml of deionized water to dissolve the above product, and transfer it to a 100ml three-necked bottle;

[0026] (3) under rapid stirring, the sodium molybdate solution is dripped into the above-mentioned three-neck flask to generate a milky precipitate;

[0027] (4) Centrifuge the precipitate and wash it with water three times to make a hydrogel;

[0028] (5) Putting the hydrogel as a precursor into a high-temperature furnace and calcining at 800° C. for 5 hours to obtain a nanoscale up-conversion fluorescent material with an average particle size of 50 nm.

Embodiment 2

[0030] (1) Weigh 1.1760g lanthanum oxide (La 2 o 3 ), 0.3692g ytterbium oxide (Yb 2 o 3 ), 0.0537g erbium oxide (Er 2 o 3 ), placed in a 100ml beaker, add 2ml of concentrated hydrochloric acid (HCl) and heat to dissolve. At this time, the molar ratio of rare earth ions is La 3+ :Yb 3+ :Er 3+ =77:20:3, evaporate to dryness, remove remaining hydrochloric acid;

[0031] (2) Add 30ml of deionized water to dissolve the above product, and transfer it to a 100ml three-necked bottle;

[0032] (3) under rapid stirring, the potassium molybdate solution is dripped in the above-mentioned three-necked flask to generate a milky precipitate;

[0033] (4) Centrifuge the precipitate and wash it with water three times to make a hydrogel;

[0034] (5) Add ethanol to soak in the prepared hydrogel to make alcohol gel;

[0035] (6) Put the prepared alcohol gel into a high-temperature furnace and calcinate at 400° C. for 10 hours to obtain a nanoscale up-conversion fluorescent material wit...

Embodiment 3

[0037] (1) Measure lanthanum chloride, ytterbium chloride, and erbium chloride to be mixed with 25ml solution, so that the molar ratio of rare earth ions is La 3+ :Yb 3+ :Er 3+ =70.29:1, the total concentration of rare earth ions is 0.04mol / L, placed in a three-necked flask;

[0038] (2) Add 5ml of 0.2mol / L ethylenediaminetetraacetic acid (EDTA) solution to fully complex EDTA with rare earth ions;

[0039] (3) under rapid stirring, the sodium molybdate solution is rapidly injected into the above-mentioned three-necked bottle to generate a milky precipitate;

[0040] (4) adding ethanol to cooking in the prepared hydrogel to make alcohol gel;

[0041] (5) Put the produced alcohol gel as a precursor into a high-temperature furnace, and calcinate at 1100° C. for 1 hour to obtain a nanoscale up-conversion fluorescent material.

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Abstract

The present invention belongs to the field of nano fluorescent material. Lanthanum oxide (or yttrium or gadolinium oxide), ytterbium oxide and erbiom oxide (or thulium or holmium oxide) are first dissolved in acid to prepare solution; complexone and sodium or potassium molybdenate are added into the solution to produce precipitate, which is centrifugally separated and water washed to prepare aqueous gel, aqueous gel or further prepared alcoholic gel is finally cinerated in a high temperature furnace or heated in a hydrothermal reactor to obtain the nano level up converting fluorescent material. The said material has lanthanum molybdenate as matrix and ytterbium molybdenate and erbium molybdenate as dopant. The material thus prepared has small and homogeneous size, average size 50-60 nm and high light glowing strength and may meet the requirement as biological molecular fluorescent mark material.

Description

Technical field: [0001] The invention belongs to the technical field of nano fluorescent materials, in particular to a rare earth ion-doped nano up-conversion fluorescent material with molybdate as a matrix and a preparation method thereof. Background technique: [0002] Up-conversion fluorescent material is a kind of luminescent material that can emit visible light under the excitation of infrared light. Molybdate co-doped with ytterbium and erbium is a relatively high-efficiency up-conversion fluorescent material, which is usually made of molybdenum oxide (MoO 3 ), ytterbium oxide (Yb 2 o 3 ), erbium oxide (Er 2 o 3 ) and so on are mixed evenly, and burned by high-temperature solid-phase reaction at a high temperature of 1200°C. This type of material emits red fluorescence under 970nm infrared excitation (Yu Xianen, Practical Luminescent Materials and Photoluminescence Mechanism, China Light Industry Press, 1997, Beijing). [0003] Due to their special properties, up...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/77
Inventor 衣光舜孙宝全陈德朴周玉祥程京
Owner CAPITALBIO CORP
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