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UCNP (up-conversion nanoparticle)-graphene oxide composite material and preparation method thereof

A nanoparticle and composite material technology, applied in the field of nanomaterials, can solve the problems of complex preparation steps, non-water solubility of composite materials, difficulty in accurately controlling the reaction process and results, and achieve good water solubility, good application prospects, and simple process Effect

Active Publication Date: 2015-03-25
山东中科绿碳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of one-step preparation of upconversion-graphene composites is that the composites are insoluble in water and it is difficult to precisely control the reaction process and results
The main defect of the step-by-step method is that the preparation steps are too complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 0.78mmol of Y (CF 3 COO) 3 , 0.2mmol of Yb (CF 3 COO) 3 , 0.02mmol of Er(CF 3 COO) 3 , 10mmol sodium fluoride (NaF) and 20ml organic solvent (10ml oleic acid OA + 10ml carbadecene ODE) were added to a 50mL three-necked flask and heated to 120°C, continuously fed with nitrogen protection and heated for 1h, then Raise the temperature to 320°C at a speed of 1°C / min and stir it magnetically for 1 hour, cool down to room temperature naturally, add absolute ethanol, centrifuge to obtain a precipitate, and then repeatedly wash with water and ethanol to finally obtain various Upconverting nanoparticles (UCNPs) in organic solvents.

[0023] Mix 1g / L of 5mL up-converting luminescent nanoparticles hexane dispersion solution with 0.6g / L of 5mL nitrosonium tetrafluoroborate NOBF 4The dichloromethane solution was mixed at room temperature, and the mixture was shaken gently until the UCNPs precipitated, then centrifuged, the supernatant was removed, and then redispersed in water...

Embodiment 2

[0026] 0.69mmol of Y (CF 3 COO) 3 , 0.3mmol of Yb (CF 3 COO) 3 , 0.01mmol of Er(CF 3 COO) 3 , 10mmol sodium fluoride (NaF) and 20ml organic solvent (10ml oleic acid OA + 10ml carbadecene ODE) were added to a 50mL three-necked flask and heated to 120°C, continuously fed with nitrogen protection and heated for 1h, then Raise the temperature to 320°C at a speed of 1°C / min and stir it magnetically for 1 hour, cool down to room temperature naturally, add absolute ethanol, centrifuge to obtain a precipitate, and then repeatedly wash with water and ethanol to finally obtain various Upconverting nanoparticles (UCNPs) in organic solvents.

[0027] Mix 2g / L of 5mL up-converting luminescent nanoparticles hexane dispersion solution with 0.3g / L of 5mL nitrosonium tetrafluoroborate NOBF 4 The dichloromethane solution was mixed at room temperature, and the mixture was shaken gently until the UCNPs precipitated, then centrifuged, the supernatant was removed, and then redispersed in wate...

Embodiment 3

[0030] 0.78mmol of Y (CF 3 COO) 3 , 0.2mmol of Yb (CF 3 COO) 3 , 0.02mmol of Tm (CF 3 COO) 3 , 10mmol sodium fluoride (NaF) and 20ml organic solvent (10ml oleic acid OA + 10ml carbadecene ODE) were added to a 50mL three-necked flask and heated to 120°C, continuously fed with nitrogen protection and heated for 1h, then Raise the temperature to 320°C at a speed of 1°C / min and stir it magnetically for 1 hour, cool down to room temperature naturally, add absolute ethanol, centrifuge to obtain a precipitate, and then repeatedly wash with water and ethanol to finally obtain various Upconverting nanoparticles (UCNPs) in organic solvents.

[0031] Mix 2g / L of 5mL up-converting luminescent nanoparticles hexane dispersion solution with 0.6g / L of 5mL nitrosonium tetrafluoroborate NOBF 4 The dichloromethane solution was mixed at room temperature, and the mixture was shaken gently until the UCNPs precipitated, then centrifuged, the supernatant was removed, and then redispersed in wat...

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Abstract

The invention discloses a UCNP (up-conversion nanoparticle)-graphene oxide composite material and a preparation method thereof. The method comprises steps as follows: firstly, synthesizing hexagonal-phase UCNPs with a high-temperature pyrolysis method, then treating the UCNPs with NOBF4 to enable oleic acid molecules on surfaces of the UCNPs to be replaced, then adding an amino-terminated hyperbranched polymer aqueous solution, and finally, conducting an ultrasonic reaction with graphene oxide to obtain the UCNP-graphene oxide composite material. The prepared composite material is good in water solubility, the reaction process is easy to control, steps are relatively simple, and the composite material has the broad application prospect in the aspects of photo-thermal therapy, photodynamic therapy, fluorescence labeling, biological probes and the like.

Description

technical field [0001] The invention relates to an upconversion nano particle-graphene oxide composite material and a preparation method thereof, belonging to the field of nanometer materials. Background technique [0002] In 2004, Andre Geim and Konstantin Novoselov, physicists at the University of Manchester in the United Kingdom, successfully separated graphene with single-layer atomic arrangement from graphite by tearing scotch tape. Therefore, he won the Nobel Prize in Physics in 2010 (Science, 2004, 306(5696):666-669). Graphene consists of carbon atoms with sp 2 The hybrid orbitals form a hexagonal honeycomb lattice, and its structural unit is a carbon six-membered ring, which is a two-dimensional material with a thickness of only a single layer of carbon atoms. Graphene is the basic structural unit that constitutes carbon-based materials. It can be wrapped to form zero-dimensional Fullerenes, rolled into one-dimensional carbon nanotube, and stacked layer by layer t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/77B82Y30/00B82Y20/00B82Y40/00
Inventor 赵兵
Owner 山东中科绿碳科技有限公司
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