Ion thermal growth method of near infrared light upper conversion fluoride nano crystal

A nano-crystal and near-infrared light technology is applied in the field of preparation of nano-fluorescent materials, which can solve the problems of large hexagonal phase particle size, low product yield and low synthesis amount, and achieve uniform distribution, low reaction temperature and high heat capacity. and the effect of thermal storage density

Inactive Publication Date: 2009-07-08
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

The coordination of rare earth doping ions has been basically determined in NaYF 4 In general, the particle size distribution of nanocrystals is determined by the particle size distribution of the host material, while the luminous intensity and luminous efficiency are mainly determined by the NaYF 4 The phase structure itself (cubic phase or hexagonal phase) is determined by the crystallinity. Although it is known that the hexagonal phase NaYF co-doped with rare earth ions 4 The host has a higher near-infrared light upconversion fluorescence efficiency, however, many existing researches on rare earth ion co-doped NaYF 4 The aqueous phase preparation method of the nanomaterial system, most of which are cubic phases, and the obtained hexagonal phases have larger particle sizes
Although the hexagonal phase infrared light up-conversion fluorescent nanocrystals prepared by the oil-phase trifluoroacetate decomposition method have small particle size, uniform distribution, and high luminous efficiency, they are hydrophobic due to the coating of oleic acid or oleylamine on the surface of the particles. , the product yield is low, and the amount of synthesis is very small
More importantly, people have not yet found an ideal phase transition from the oil phase to the water phase, thus limiting its application in the biomedical field.

Method used

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  • Ion thermal growth method of near infrared light upper conversion fluoride nano crystal
  • Ion thermal growth method of near infrared light upper conversion fluoride nano crystal
  • Ion thermal growth method of near infrared light upper conversion fluoride nano crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Using [EMIM][BF 4 ] Synthesis of NaYF from Ionic Liquids 4 : Yb, Er nanocrystals.

[0031] (1) Weigh 0.2985 grams of Y (NO 3 ) 3 ·6H 2 O, 0.093 g Yb (NO 3 ) 3 ·6H 2 O, 0.0092 g Er(NO 3 ) 3 ·6H 2 O, the molar ratio of rare earth ions in the mixed solid is yttrium ion: ytterbium ion: erbium ion is equal to 78:20:2.

[0032] (2) Add 4 ml of 1-ethyl-3-methylimidazolium tetrafluoroboric acid ([EMIM][BF 4 ]) ionic liquid, heated at 150° C. with vigorous stirring for 20 minutes.

[0033] (3) Weigh 0.058 g of NaCl and add it into the above mixed solution, and continue to stir for 30 minutes, so that the rare earth nitrate and NaCl are fully dissolved in the ionic liquid.

[0034] (4) Put the mixed solution obtained in step (3) into a polytetrafluoroethylene-lined autoclave, place it in an oven, heat it at 180° C. for 18 hours, and cool it down to room temperature naturally.

[0035] (5) The precipitate was separated by centrifugation and ultrasonically washed three...

Embodiment 2

[0037] Using [BMIM][BF 4 ] Synthesis of NaYF from Ionic Liquids 4 : Yb, Er nanocrystals.

[0038] (1) Weigh 0.2985 grams of Y (NO 3 ) 3 ·6H 2 O, 0.093 g Yb (NO 3 ) 3 ·6H 2 O, 0.0092 g Er(NO 3 ) 3 ·6H 2 O, the molar ratio of rare earth ions in the mixed solid is yttrium ion: ytterbium ion: erbium ion is equal to 78:20:2.

[0039] (2) Add 4 ml of 1-butyl-3-methylimidazolium tetrafluoroboric acid ([BMIM][BF 4 ]) ionic liquid, heated at 150° C. with vigorous stirring for 20 minutes.

[0040] (3) Weigh 0.058 g of NaCl and add it into the above mixed solution, and continue to stir for 30 minutes, so that the rare earth nitrate and NaCl are fully dissolved in the ionic liquid.

[0041] (4) Put the mixed solution obtained in step (3) into a polytetrafluoroethylene-lined autoclave, place it in an oven, heat it at 180° C. for 18 hours, and cool it down to room temperature naturally.

[0042] (5) The precipitate was separated by centrifugation and ultrasonically washed three...

Embodiment 3

[0044] Using [OMIM][BF 4 ] Synthesis of NaYF from Ionic Liquids 4 : Yb, Er nanocrystals.

[0045] (1) Weigh 0.2985 grams of Y (NO 3 ) 3 ·6H 2 O, 0.093 g Yb (NO 3 ) 3 ·6H 2 O, 0.0092 g Er(NO 3 ) 3 ·6H 2 O, the molar ratio of rare earth ions in the mixed solid is yttrium ion: ytterbium ion: erbium ion is equal to 78:20:2.

[0046] (2) Add 4 ml of 1-octyl-3-methylimidazolium tetrafluoroboric acid ([OMIM][BF 4 ]) ionic liquid, heated at 150° C. with vigorous stirring for 20 minutes.

[0047] (3) Weigh 0.058 g of NaCl and add it into the above mixed solution, and continue to stir for 30 minutes, so that the rare earth nitrate and NaCl are fully dissolved in the ionic liquid.

[0048] (4) Put the mixed solution obtained in step (3) into a polytetrafluoroethylene-lined autoclave, place it in an oven, heat it at 180° C. for 18 hours, and cool it down to room temperature naturally.

[0049] (5) The precipitate was separated by centrifugation and ultrasonically washed three...

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Abstract

The invention relates to an ion thermal growth method for converting fluoride nano crystal near infrared light which includes steps as follows: weighing some solid yttrium nitrate (lanthanum nitrate), ytterbium nitrate, erbium nitrate (thulium nitrate or holmium nitrate) pro rata. Mol ratio of the rare earth ion is that yttrium ion (lanthanum ion) : ytterbium ion : erbium ion (thulium ion, holmium ion) equal to 70-90 : 0 : 0.001-15; adding tetrafluoroborate type ion liquor into the mixing solid, selective adding some NaCl solid according with various basic, then placing the mixing solution into a high pressure reaction kettle with polyfluortetraethylene lining, placing into an oven for heating reacting, finally, washing, centrifugating, drying and obtaining the product. The prepared nano upper converting fluorescence material has small and uniform granule, strong lighting strength, better water-solubility and can satisfy need of biomolecule fluorescence mark material.

Description

technical field [0001] The invention belongs to a preparation method of a nano fluorescent material, in particular to a preparation method of a near-infrared light up-conversion nano fluorescent material with a fluoride-based rare earth ion doping. Background technique [0002] Infrared light up-conversion fluorescent nanomaterials are fluorescent materials that can up-convert low-energy near-infrared light into high-energy visible light when excited by near-infrared light. It has important application prospects in different fields such as anti-counterfeiting marks, infrared radiation detection, solid-state lasers, and biomolecular fluorescent labeling and identification. In recent years, near-infrared light upconversion fluorescent nanomaterials have attracted more and more attention in the field of nanomedicine. This kind of material can not only be used for the recognition and detection of specific biomolecules, but also can be used as a multifunctional nanocarrier for p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/12C09K9/00
Inventor 刘晓敏孔祥贵孙雅娟曾庆辉张友林
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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