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Preparation method of NaGdF4@CaF2 core-shell nanometer crystals

A nanocrystal and core-shell technology, which is applied in the field of preparation of NaGdF4CaF2 core-shell nanocrystals, can solve the problems of complex process, complex operation, and long synthesis time, and achieve the effects of simple operation, simplified operation process, and low cost

Inactive Publication Date: 2015-06-10
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention provides a NaGdF 4 CaF 2 The preparation method of core-shell nanocrystals solves the technical proble

Method used

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  • Preparation method of NaGdF4@CaF2 core-shell nanometer crystals
  • Preparation method of NaGdF4@CaF2 core-shell nanometer crystals
  • Preparation method of NaGdF4@CaF2 core-shell nanometer crystals

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Embodiment 1

[0029] This embodiment prepares NaGdF according to the following steps 4 CaF 2 Core-shell nanocrystals:

[0030] a. Add 10 mL of oleic acid to the first reactor, and add 0.1 g of GdCl 3 , stir evenly, set the temperature at 80°C, and keep it warm for 5 hours to form a transparent liquid A, and cool it down to room temperature naturally to obtain the precursor of gadolinium oleate complex;

[0031] b. Add 10mL oleic acid and 0.1g CaO to the second reactor, stir evenly, set the temperature at 100°C, and keep it warm for 5h to form a clear clear liquid B, then naturally cool to room temperature to obtain the calcium oleate complex precursor ;

[0032]c. In the third reactor, add 10mL of oleic acid and 10mL of octadecene, stir evenly, and add 0.0178g of NH 4 F and 0.00356g NaOH methanol solution 10mL, then heated to 50°C, kept for 2h to remove methanol, heated the mixed solution to 240°C under nitrogen protection flow, and obtained reaction solution C;

[0033] d. Rapidly inj...

Embodiment 2

[0039] This embodiment prepares NaGdF according to the following steps 4 CaF 2 Core-shell nanocrystals:

[0040] a. Add 10mL of oleic acid to the first reactor, and add 2g of GdCl 3 , stir evenly, set the temperature at 150°C, and keep it warm for 20 minutes to form a transparent liquid A, and cool it down to room temperature naturally to obtain the precursor of gadolinium oleate complex;

[0041] b. Add 10mL of oleic acid and 1g of CaO into the second reactor, stir evenly, set the temperature at 150°C, and keep it warm for 30min to form a clear clear liquid B, then cool it naturally to room temperature to obtain the calcium oleate complex precursor;

[0042] c. In the third reactor, add 10mL of oleic acid and 40mL of octadecene, stir evenly, and add 1.7845g of NH 4 F and 1.96295g NaOH methanol solution 10mL, then heated to 150°C, kept for 30min to remove methanol, heated the mixed solution to 320°C under nitrogen protection flow, and obtained reaction solution C;

[0043]...

Embodiment 3

[0049] This embodiment prepares NaGdF according to the following steps 4 CaF 2 Core-shell nanocrystals:

[0050] a, add 10mL of oleic acid in the first reactor, and add 0.5g Gd(NO 3 ) 3 , stir evenly, set the temperature at 100°C, keep it warm for 4 hours, form a transparent clear liquid A, cool it down to room temperature naturally, and obtain the precursor of gadolinium oleate complex;

[0051] b. Add 10 mL of oleic acid and 0.3 g of CaO into the second reactor, stir evenly, set the temperature at 110°C, keep it warm for 4 hours, form a clear clear liquid B, and naturally cool to room temperature to obtain the calcium oleate complex precursor;

[0052] c. In the third reactor, add 10mL of oleic acid and 15mL of octadecene, stir evenly, and add 0.0256g of NH 4 F and 0.0282g NaOH methanol solution 10mL, then heated to 60°C, kept for 1.5h to remove methanol, heated the mixed solution to 260°C under nitrogen protection flow, and obtained reaction solution C;

[0053] d. Rap...

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Abstract

The invention discloses a preparation method of NaGdF4@CaF2 core-shell nanometer crystals. The method is characterized by comprising the following steps: by taking ammonium fluoride and sodium hydroxide as a fluorine source and a sodium source respectively, quickly injecting an oleic acid-gadolinium compound precursor at a high temperature to prepare NaGdF4 nanometer crystals, and slowing injecting an oleic acid-calcium compound precursor into a system to prepare the NaGdF4@CaF2 core-shell nanometer crystals. During the preparation process of the NaGdF4@CaF2 core-shell nanometer crystals, toxic fluorides are not used, and oleic acid compounds are stable and easy to store; and during synthesis of a multi-layer structure, complex processes such as purification are avoided, the cost is low, the operation is continuous, and the popularization and production are easy.

Description

technical field [0001] The present invention relates to a kind of NaGdF 4 CaF 2 A method for preparing core-shell nanocrystals, belonging to the technical field of nanomaterial preparation Background technique [0002] Magnetic resonance imaging (MRI) is a medical diagnostic technique based on atomic nuclear magnetic resonance and proton spin relaxation, without radiation damage under magnetic field conditions. As an important auxiliary means of MRI, MRI contrast agents are divided into T1 type and T2 type according to the type of enhancement. Compared with T2 contrast agents (such as iron oxide), T1 contrast agents improve spatial resolution through positive enhancement and have stronger signals. Therefore, T1-weighted magnetic resonance imaging is more commonly used clinically. Compared with the magnetic resonance contrast agent Gd-DTPA (Magenweixian), which is commonly used clinically at present, NaGdF 4 Nanocrystals exhibit a higher longitudinal molar relaxation rat...

Claims

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Application Information

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IPC IPC(8): A61K49/18A61K49/08B82Y5/00B82Y40/00
Inventor 钱海生丁彬彬章富刘坤李耀武彭煌用吴双
Owner HEFEI UNIV OF TECH
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