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Preparation method of nanocrystal containing manganese and fluoride compounds

A technology of nanocrystals and manganese fluoride, which is applied in the field of synthesis of manganese-containing fluoride nanocrystals, can solve the problems of high crystallinity and small size, and achieve the effect of easy operation and wide application prospects

Active Publication Date: 2017-06-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the control method that can synthesize monochromatic emission light with uniform particle size, small size, high crystallinity, and long wavelength, and can realize solid and hollow upconversion nanocrystals.

Method used

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  • Preparation method of nanocrystal containing manganese and fluoride compounds
  • Preparation method of nanocrystal containing manganese and fluoride compounds
  • Preparation method of nanocrystal containing manganese and fluoride compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: prepare the NaMnF of hollow structure 3 nanocrystal

[0048] Completely dissolve 0.03mol sodium hydroxide in 4mL water and 9mL absolute ethanol, add 20mL oleic acid, stir for 10min; then add 1mL0.5mmol / mL manganese chloride aqueous solution and 4mL0.375mmol / mL potassium fluoride aqueous solution in sequence , stirred for 1h to get NaMnF 3 The nanocrystal precursor was then transferred to a 50mL reactor and reacted at 160°C for 24h. After the reaction, cool to room temperature, add absolute ethanol to precipitate the product, centrifuge at 8000rpm for 15min, and wash the precipitate obtained by centrifugation with water and absolute ethanol several times to obtain hollow NaMnF 3 nanocrystals. figure 1 Hollow NaMnF prepared for this example 3 TEM photographs of nanocrystals, figure 2 Hollow NaMnF prepared for this example 3 The powder X-ray diffraction spectrum of nanocrystals, its diffraction peaks are similar to those of NaMnF 3 The standard diffra...

Embodiment 2

[0049] Embodiment 2: prepare the KMnF of solid structure 3 nanocrystal

[0050] The steps of this embodiment are basically the same as in Example 1, except that 0.03 mol of potassium hydroxide is used to replace 0.03 mol of sodium hydroxide. image 3 Solid KMnF prepared for this example 3 TEM photographs of nanocrystals, Figure 4 Solid KMnF prepared for this example 3 The powder X-ray diffraction spectrum of nanocrystals, its diffraction peaks are consistent with the standard diffraction peaks of KMnF3, proving that the obtained product is pure KMnF 3 .

Embodiment 3

[0051] Example 3: Preparation of solid KMnF doped with a single rare earth ion 3 nanocrystal

[0052] Dissolve 0.03mol potassium hydroxide completely in 4mL water and 9mL absolute ethanol, then add 20mL oleic acid, stir for 10min, then add 1mL 0.5mmol / mL manganese chloride and neodymium chloride (molar ratio Mn:Nd=49 : 1) mixed aqueous solution and 4mL 0.5mmol / mL potassium fluoride aqueous solution, stirred for 1h to obtain KMnF doped with rare earth ion neodymium 3 The nanocrystal precursor was then transferred to a 50mL reactor and reacted at 160°C for 24h. After the reaction, cool to room temperature, centrifuge the reaction system at 11,000 rpm for 15 minutes, and wash the product obtained after high-speed centrifugation with cyclohexane and absolute ethanol several times. Figure 5 The solid KMnF doped rare earth ion neodymium prepared for this embodiment 3 TEM photographs of nanocrystals, Figure 6 The solid KMnF doped rare earth ion neodymium prepared for this embod...

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Abstract

The invention provides a preparation method of a nanocrystal containing manganese and fluoride compounds. The preparation method comprises the following steps: firstly, dissolving alkali into an alcohol-water solution, then adding organic compounds CH3(CH2)nCOOH and / or CH3(CnH2n-2)COOH, and uniformly mixing to obtain an alcohol-water-oil reaction system, wherein n is greater than or equal to 6 and smaller than or equal to 18; secondly, adding an aqueous solution containing Mn<2+> and F<-> into the alcohol-water-oil reaction system, and then carrying out a reaction at the temperature of 25 to 200 DEG C to obtain the nanocrystal containing the manganese and fluoride compounds; adding rare earth ions into the second step to obtain a rare earth ion-doped nanocrystal containing the manganese and fluoride compounds. According to the method, a solid or hollow nanocrystal with smaller size, uniform particle size and high crystallinity degree is directly prepared according to a one-pot method; a solid and hollow structure of the nanocrystal is regulated and controlled by regulating and controlling the proportion of alcohol-water-oil and distribution of the Mn<2+> and the F<-> in the alcohol-water-oil; by regulating and controlling doped rare earth ions, upconversion and downconversion regulation and control of monochromatic emitted light of the nanocrystal are realized; in addition, regulation and control of magnetic properties of the nanocrystal also can be realized.

Description

technical field [0001] The invention relates to a method for synthesizing manganese-containing fluoride nanocrystals. Background technique [0002] Hollow nanomaterials have larger specific surface area, lower density, and higher loading capacity than solid nanocrystals of the same size, and have broad application prospects in catalysis, energy storage, biomedicine, sensors, and environmental restoration. For example, in the field of biomedicine, on the one hand, the cavity of hollow nanomaterials can be used to load drugs, and on the other hand, the magnetic and optical properties of hollow nanomaterials can be used, so they have significant advantages in multimodal imaging and treatment of tumors. Hollow nanomaterials are usually prepared by template methods (such as hard template method, soft template method, self-template method) and template-free methods. The template method usually involves a multi-step synthesis process and has high requirements for temperature contr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61B82Y40/00
CPCB82Y40/00C09K11/616C09K11/7757C09K11/7791
Inventor 李桢任峰高明远
Owner SUZHOU UNIV
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