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Method for preparing CaF2:Eu<3+> luminescent nano material with enhanced fluorescence intensity and nano material

A technology of nanomaterials and fluorescence enhancement, applied in the field of nanomaterials, can solve the problems of high biological toxicity, high light transmittance, low refractive index, etc., achieve good fluorescence performance, control the number of feeding, and uniform appearance

Inactive Publication Date: 2019-04-16
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Rare earth-doped luminescent nanomaterials currently reported mainly use LaF 3 and NaYF 4 As a doping matrix, but LaF 3 and NaYF 4 High biological toxicity, CaF 2 It is a cubic fluorite structure with high light transmittance and low refractive index. It has good light transmittance to light in the wavelength range from ultraviolet (UV) to infrared (IR), and is optically transparent. Its biological toxicity is relatively low compared to other substrates. Such as LaF 3 、NaYF 4 etc. are lower, so it is an ideal rare earth doped host material while

Method used

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  • Method for preparing CaF2:Eu&lt;3+&gt; luminescent nano material with enhanced fluorescence intensity and nano material
  • Method for preparing CaF2:Eu&lt;3+&gt; luminescent nano material with enhanced fluorescence intensity and nano material
  • Method for preparing CaF2:Eu&lt;3+&gt; luminescent nano material with enhanced fluorescence intensity and nano material

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Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: prepare CaF 2 :5%Eu 3+ Nanocrystalline

[0018] Accurately weigh 0.64mmol of Ca(CF 3 COO) 2 and 0.1mmol Eu(CF 3 COO) 3 Add it into a three-necked flask containing 40mmol oleic acid (OA) and 40mmol octadecene (ODE), stir at 70°C to dissolve it completely, heat up to 110°C and vacuumize for 30min to remove the moisture present in the system;

[0019] After heating up to 300°C for 20 minutes, 0.63 mmol of Ca(CF 3 COO) 2 Add it to the flask, react at 300°C for 20min, and then continue to add 0.63mmol of Ca(CF 3 COO) 2 In a flask, react at 300°C for 20min.

[0020] Cool to room temperature, then add ethanol to the generated nanoparticles, centrifuge, add cyclohexane to the obtained nanoparticles to clean the residual reactants, then precipitate with ethanol, centrifuge, wash twice in this way, and ultrasonically disperse in cyclohexane Stored in the middle, that is, CaF 2 :5%Eu 3+ nanoparticles.

Embodiment 2

[0021] Embodiment 2: prepare CaF 2 :10%Eu 3+ Nanocrystalline

[0022] Accurately weigh 0.6mmol of Ca(CF 3 COO) 2 and 0.2mmol of Eu(CF 3 COO) 3 Add it into a three-necked flask containing 40mmol oleic acid (OA) and 40mmol octadecene (ODE), stir at 70°C to dissolve it completely, raise the temperature to 110°C and apply vacuum for 30min to remove the moisture that may exist in the system.

[0023] Then the temperature was raised to 300°C for 20 minutes, and 0.6 mmol of Ca(CF 3 COO) 2 Add it into the flask, react at 300°C for 20min, and continue to add 0.6mmol of Ca(CF 3 COO) 2 In the flask, react at 300°C for 20min.

[0024] Cool to room temperature, then add ethanol to the generated nanoparticles, centrifuge, add cyclohexane to the obtained nanoparticles to clean the residual reactants, then precipitate with ethanol, centrifuge, wash twice in this way, and ultrasonically disperse in cyclohexane Stored in the middle, that is, CaF 2 :10Eu 3+ nanoparticles.

Embodiment 3

[0025] Embodiment 3: prepare CaF 2 :20%Eu 3+ Nanocrystalline

[0026] Accurately weigh 0.54mmol of Ca(CF 3 COO) 2 and 0.4mmol of Eu(CF 3 COO) 3 Add it into a three-necked flask containing 40mmol oleic acid (OA) and 40mmol octadecene (ODE), stir at 70°C to dissolve it completely, raise the temperature to 110°C and apply vacuum for 30min to remove the moisture that may exist in the system.

[0027] Then the temperature was raised to 300°C for 20 minutes and a certain amount of Ca(CF 3 COO) 2 (0.53mmol) into the flask, reacted at 300°C for 20min, then continued to add 0.53mmol Ca(CF 3 COO) 2 In the flask, react at 300°C for 20min.

[0028] Cool to room temperature, then add ethanol to the generated nanoparticles, centrifuge, add cyclohexane to the obtained nanoparticles to clean the residual reactants, then precipitate with ethanol, centrifuge, wash twice in this way, and ultrasonically disperse in cyclohexane Stored in the middle, that is, CaF 2 :20%Eu 3+ nanoparticl...

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Abstract

The invention discloses a method for preparing a CaF2:Eu<3+> luminescent nano material with an enhanced fluorescence intensity and the prepared nano material thereof. The method comprises the steps ofusing trifluoroacetic acid rare earth salt and calcium trifluoroacetate as organic precursors, and a monodisperse cubic phase CaF2:Eu3+ luminescent nanocrystal having a particle diameter of 5-30 nanometre is synthesized by a thermal decomposition method. The results show that the particle diameter of the obtained CaF2:Eu3+ nanocrystal decreases with the increase of an Eu3+ doping amount and the increase of the number of addition. The nanocrystal has good crystallinity. When an Eu3+ luminescence quenching doping concentration is as high as 40%, the nanocrystal fluorescence lifetime is greaterthan 3ms, and the nano material can be used as a fluorescent material for photoluminescence time-resolved spectrum detection.

Description

technical field [0001] The invention relates to nanomaterials, in particular to a CaF with enhanced fluorescence intensity 2 :Eu 3+ Luminescent nanomaterials and methods for their preparation. Background technique [0002] Rare earth-doped luminescent materials have attracted widespread attention due to their advantages such as good chemical stability, strong and stable luminous brightness, and high quantum efficiency. Among them, alkaline earth metal fluorides and rare earth fluorides not only have suitable chemical stability, but also have relatively low phonon energy, so they are ideal host materials for various luminescent lanthanide ions. Since the last century, a lot of research has been done on rare earth-doped fluoride luminescent materials, and many new nanomaterials with controllable morphology and excellent luminescent properties have been synthesized. [0003] Rare earth-doped luminescent nanomaterials currently reported mainly use LaF 3 and NaYF 4 As a dopi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61G01N21/64B82Y30/00B82Y40/00
CPCG01N21/6408C09K11/7733B82Y30/00B82Y40/00
Inventor 夏奡王亚穷蒋雪峰沈健黄晓华牛倩倩胡瑾杨明月翟珂邓莎
Owner NANJING NORMAL UNIVERSITY