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Rare earth core-shell nano material and preparation method thereof

A core-shell nanomaterial and a technology for nanomaterials, which are applied in the field of rare earth core-shell nanomaterials and their preparation, can solve the problems of long synthesis time, poor dispersion of rare earth luminescent nanomaterials, unstable luminescence performance and the like

Pending Publication Date: 2022-03-11
SHENZHEN INST OF ADVANCED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the excitation light of rare earth luminescent nanomaterials used for biological imaging is in the infrared band, but infrared light has defects such as poor tissue penetration and poor three-dimensionality, which in turn leads to low luminous efficiency and poor imaging effect of rare earth luminescent nanomaterials.
X-rays have good penetrability to the human body, which is conducive to the application in biological imaging. However, there are few kinds of rare earth luminescent nanomaterials that use X-rays as excitation light to realize biological imaging, and the preparation methods are complicated, and the production cost is high. For a long time, the resulting rare earth luminescent nanomaterials have poor dispersion and unstable luminescent performance, which is not conducive to popularization and use.

Method used

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  • Rare earth core-shell nano material and preparation method thereof
  • Rare earth core-shell nano material and preparation method thereof
  • Rare earth core-shell nano material and preparation method thereof

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preparation example Construction

[0045] The application also provides the above-mentioned rare earth core-shell nanomaterial β-NaLuF 4 :Tb@NaYF 4 For preparation methods, see figure 1 , figure 1 The method for preparing rare earth core-shell nanomaterials provided in one embodiment of the present application includes:

[0046] Step 100: performing a first mixing treatment on terbium salt, lutetium salt and solvent to form a first mixed liquid;

[0047] Step 200: performing a second mixing treatment on the first mixed solution, ammonium fluoride and alkali to obtain rare earth core nanomaterials; the second mixing includes ultrasonic mixing;

[0048] Step 300: performing a third mixing treatment on the yttrium salt, the rare earth core nanomaterial and the solvent to form a second mixed liquid;

[0049] Step 400: performing a fourth mixing treatment with the second mixed solution, ammonium fluoride and alkali to obtain rare earth core-shell nanomaterials; the fourth mixing includes ultrasonic mixing.

[0...

Embodiment 1

[0069] A preparation method of rare earth core-shell nanomaterials, comprising the following steps:

[0070] (1) Synthesis of rare earth core nanomaterials:

[0071] a. Add 1.6mmol of LuCl 3 ·6H 2 O and 0.4 mmol of Tb(CH 3 CO 2 ) 3 Place in a 100mL four-neck flask, add 12mL of anhydrous oleic acid and 30mL of anhydrous octadecene into the bottle, and feed argon gas into the flask at a gas flow rate of 200mL / min for 5min, and simultaneously perform stirring and ultrasonic treatment (power 200W , frequency 50kHz), under the protection of argon, the temperature was raised to 160° C. and kept for 60 minutes, while stirring and ultrasonic treatment (power 60W, frequency 40kHz), and the first mixed solution was obtained after cooling.

[0072] b. 10mL methanol (dissolved with 2mmolNH 4 F and 1.25mmol NaOH) were added in the first mixed solution. Stir and sonicate for 10 minutes (power 150W, frequency 50kHz), heat up to 60°C and vacuumize, stir and sonicate at this temperature...

Embodiment 2

[0077] The difference between embodiment 2 and embodiment 1 is that the reaction conditions of step b in embodiment 2 are specifically: 10mL methanol (dissolved with 2mmolNH 4 F and 1.25mmol NaOH) were added to the first mixed liquid, heated to 60°C and vacuumed, stirred at this temperature and ultrasonicated for 60min (power 150W, frequency 50kHz), switched to nitrogen protection three times, and then at 20°C / min The temperature was raised to 300° C. and stirred and ultrasonically treated for 10 minutes (power 200 W, frequency 50 kHz). After cooling to room temperature, add ethanol to the reaction solution to precipitate the rare earth core nanomaterial, centrifuge at 8000rpm for 5min, and wash twice with absolute ethanol to obtain the rare earth core nanomaterial β-NaLuF 4 : Tb, the yield is 45%. The conditions for synthesizing rare earth core-shell nanomaterials in Example 2 are the same as in Example 1, and the resulting rare earth core-shell nanomaterials β-NaLuF 4 :Tb@...

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Abstract

The invention provides a preparation method of a rare earth core-shell nano material. The preparation method comprises the following steps: performing first mixing treatment on terbium salt, lutetium salt and a solvent to form a first solution; carrying out second mixing treatment on the first solution, ammonium fluoride and alkali to obtain the rare earth core nano material, wherein the second mixing treatment comprises ultrasonic mixing; the rare earth core nano material comprises beta-NaLuF4: Tb; performing third mixing treatment on yttrium salt, a rare earth core nano material and a solvent to form a second solution; performing fourth mixing treatment on the second solution, ammonium fluoride and alkali to obtain a rare earth core-shell nano material; the fourth mixing treatment comprises ultrasonic mixing; the shell layer of the rare earth core-shell nano material comprises NaYF4. The method is simple in process, low in cost and beneficial to large-scale production. The invention further provides the rare earth core-shell nanometer material, the rare earth core-shell nanometer material is regular in morphology and uniform in granularity, a strong light-emitting effect can be generated under X-ray excitation, and application of the rare earth core-shell nanometer material to biological imaging is facilitated.

Description

technical field [0001] The present application relates to the field of nanomaterials, in particular to a rare earth core-shell nanomaterial and a preparation method thereof. Background technique [0002] Rare earth luminescent nanomaterials have many advantages such as narrow emission spectrum, high color purity, long fluorescence lifetime, and good luminescence stability, and have important application value in biomarkers and bioimaging. At present, the excitation light of rare earth luminescent nanomaterials used for biological imaging is in the infrared band, but infrared light has defects such as poor tissue penetration and poor three-dimensionality, which in turn leads to low luminous efficiency and poor imaging effect of rare earth luminescent nanomaterials. X-rays have good penetrability to the human body, which is conducive to the application in biological imaging. However, there are few kinds of rare earth luminescent nanomaterials that use X-rays as excitation ligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/77B82Y30/00
CPCC09K11/7773C09K11/02B82Y30/00
Inventor 郑海荣胡德红盛宗海
Owner SHENZHEN INST OF ADVANCED TECH