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A size-tunable β-na(luy)f 4 Preparation method of miscible nanocrystals

A nanocrystal and solution technology, applied in the field of nano-fluorescent materials, can solve the problems of affecting luminous efficiency, lower conversion luminous characteristics, weakened up-conversion emission, etc., achieve excellent luminous performance, continuously adjustable size, and solve the effect of human error

Active Publication Date: 2022-05-27
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is usually accompanied by changes in properties such as crystal phase or morphology, which in turn affects the luminous efficiency.
For example, in NaLuF 4 Gd 3+ Ions can prepare nanocrystalline materials with smaller sizes, but their up-conversion luminescence properties will be greatly reduced
Under high power density excitation, Gd 3+ The ions act as energy acceptors, causing other upconversion emissions to be weakened

Method used

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  • A size-tunable β-na(luy)f <sub>4</sub> Preparation method of miscible nanocrystals
  • A size-tunable β-na(luy)f <sub>4</sub> Preparation method of miscible nanocrystals
  • A size-tunable β-na(luy)f <sub>4</sub> Preparation method of miscible nanocrystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] β-Na(LuY)F with crystal size of 21.00 nm 4 The preparation method of mutual solution nanocrystal comprises the following steps:

[0039] (1) First, add 2mmol RECl to the 100mL three-necked flask in turn 3 ·6H 2 O solid powder (wherein RE 3+ : 25% Y 3+ , 54.5%Lu 3+ , 20% Yb 3+ , 0.5%Tm 3+ ), 30 mL of 1-octadecene liquid, 12 mL of oleic acid liquid, and the value of x is 25, which were placed in an automatic nano-synthesizer and waited to start the experiment.

[0040] (2) The mixture in the bottle was heated to 160° C. after the argon gas flow with a flow rate of 200 mL / min was used to fully purify the air in the bottle, and the mixture was continuously stirred for 60 min to form a clear and translucent yellow solution, and cooled to room temperature to obtain the precursor solution.

[0041] (3) 10 mL methanol solution A containing 5 mmol NaOH and 20 mL containing 8 mmol NH 4 The methanol solution B of F was added dropwise to the precursor solution at the same t...

Embodiment 2

[0049] β-Na(LuY)F with crystal size of 16.48 nm 4 The preparation of mutual solution nanocrystals includes the following steps:

[0050] (1) First, add 2mmol RECl to the 100mL three-necked flask in turn 3 ·6H 2 O solid powder (RE3+ : 40% Y 3 + , 39.5%Lu 3+ , 20% Yb 3+ , 0.5%Tm 3+ ), 30mL 1-octadecene liquid, 12mL oleic acid liquid, x value is 40, it is placed in automatic nano-synthesizer and waits to start experiment;

[0051] (2) this step is identical with embodiment 1;

[0052] (3) this step is identical with embodiment 1;

[0053] (4) this step is identical with embodiment 1;

[0054] (5) this step is identical with embodiment 1;

[0055] Depend on figure 1 It can be seen from j that when the value of x is 40, β-Na(LuY)F with a size of 16.48 nm can be obtained 4 Mutual solution nanocrystals, and the morphology is regular spherical, and the dispersion and crystallinity are very good.

[0056] Depend on figure 2 It can be seen that when the value of x corresp...

Embodiment 3

[0061] β-Na(LuY)F with crystal size of 16.23 nm 4 The preparation of mutual solution nanocrystals includes the following steps:

[0062] (1) This step removes the RE 3+ : 40% Y 3+ , 39.5%Lu 3+ , 20% Yb 3+ , 0.5%Tm 3+ change to RE 3+ : 40% Y 3+ , 38%Lu 3+ , 20% Yb 3+ , 2%Er 3+ , and others are the same as in Example 2.

[0063] (2) this step is identical with embodiment 1;

[0064] (3) this step is identical with embodiment 1;

[0065] (4) this step is identical with embodiment 1;

[0066] (5) this step is identical with embodiment 1;

[0067] Depend on Image 6 a, it can be seen that when the value of x corresponding to Example 3 is 60, β-Na(LuY)F with a size of 16.23 nm can be obtained 4 The size of the mutual solution nanocrystal is between 42.53nm and 13.47nm, and the shape is regular spherical. The dispersibility and crystallinity are very good, which is basically consistent with the crystallization of the sample in Example 2.

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Abstract

The invention discloses a size-adjustable β-Na(LuY)F 4 The invention discloses a preparation method of mutual-solubility nanocrystals, belonging to the technical field of nanometer fluorescent materials. The present invention uses rare earth ion Lu 3+ and Y 3+ Work together as matrix cations to bind NaLuF 4 with NaYF 4 The characteristics of these two excellent up-conversion luminescent substrates are synthesized by thermal decomposition method and automatic nano-synthesizer. While keeping the preparation parameters such as reaction temperature, time, pressure, sodium source and fluorine source concentration unchanged, through Regulating Lu 3+ and Y 3+ The nanocrystalline size of the product is adjusted by the feeding ratio of the two ions, and the β-Na(LuY)F with continuously adjustable size is realized. 4 Synthesis of miscible nanocrystals. The preparation method of the invention can obtain the miscible nanocrystal with good monodispersity, strong crystallinity, small crystal size, regular shape, uniform particle size distribution and excellent luminous performance.

Description

technical field [0001] The invention belongs to the technical field of nano fluorescent materials, in particular to a size-adjustable beta-Na(LuY)F 4 Preparation method of mutual solution nanocrystals. Background technique [0002] Due to the low phonon energy and high luminous efficiency, the rare earth fluoride β-NaREF 4 (RE: rare earth element) nanocrystals are often used as optical functional materials, such as up-conversion fluorescent probes in the biomedical field, infrared detection materials in the military and anti-counterfeiting fields, and optical frequency conversion materials in the photovoltaic field. However, different applications have different requirements for the size and optical properties of nanocrystals. In biological applications, the size of the nanocrystals is usually small enough, and the average particle size is usually less than 50 nm. Researchers have been working to find a suitable β-NaREF 4 Nanocrystals and reasonable preparation methods, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85B82Y20/00B82Y30/00
CPCC09K11/7773B82Y20/00B82Y30/00
Inventor 秦伟平张丹贾恒董妍惠李大光赵丹秦冠仕尹升燕贾志旭
Owner JILIN UNIV
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