Preparation method of up-conversion fluorescent material with controllable grain diameter

A fluorescent material and particle size technology, applied in the field of nanomaterials, can solve problems such as affecting the accuracy and sensitivity of detection, high requirements for detection instruments, and unclean running boards, and achieve the effect of uniform morphology, uniform particle size, and improved sensitivity.

Pending Publication Date: 2018-08-24
康永生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the small particle size and weak fluorescence of the first material, when it is applied to the field of immunochromatography, it has high requirements for detection instruments and low sensitivity.
Due to the irregular shape of the second material, the running plate is not clean during immunochromatography, and the signal-to-noise ratio is low, which affects the accuracy and sensitivity of detection.

Method used

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  • Preparation method of up-conversion fluorescent material with controllable grain diameter
  • Preparation method of up-conversion fluorescent material with controllable grain diameter
  • Preparation method of up-conversion fluorescent material with controllable grain diameter

Examples

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preparation example Construction

[0029] A method for preparing an up-conversion fluorescent material with a controllable particle size, comprising the following steps:

[0030] Step 1, adding rare earth chloride or rare earth acetic acid compound into the container, then adding oleic acid, and then heating to obtain a clear and transparent rare earth-oleic acid precursor; adding sodium hydroxide and ammonium fluoride into a low-boiling organic solvent , to obtain a clear and transparent sodium fluoride precursor;

[0031] Step 2, adding octadecene to the rare earth-oleic acid precursor of step 1, and then heating;

[0032] Step 3, the rare earth oleic acid precursor of step 2 is cooled down, the sodium fluoride precursor is added to the rare earth oleic acid precursor, and then the reactant is heated under the protection of argon and kept for reaction, and after the reaction is completed, the reaction mother liquor Cooling, then centrifuging to precipitate the product out of the solution, then washing, preci...

Embodiment 1

[0036] like Figures 1 to 3 As shown in the figure, a method for preparing an up-conversion fluorescent material with controllable particle size is characterized by comprising the following steps:

[0037] Step 1, add 2 mmol of rare earth chloride in a certain proportion, which contains 20% ytterbium (Yb), 2% erbium (Er) and 78% lutetium (Lu), into a three-necked round bottom flask, and then add 8 ml of oil Acid (OA), heated to 140 degrees Celsius and held for 2 minutes under magnetic stirring to finally obtain a clear and transparent rare earth-oleic acid precursor; 5 mmol of sodium hydroxide (NaOH) and 8 mmol of ammonium fluoride (NH4F) were added into 10 ml of methanol, and sonicated to obtain a clear and transparent sodium fluoride precursor;

[0038] Step 2, adding 20ml of octadecene (ODE) to the rare earth-oleic acid precursor of step 1, heating to 140 degrees Celsius under magnetic stirring and holding for 2 minutes;

[0039] In step 3, after the preparation of the ra...

Embodiment 2

[0044] This example is basically the same as Example 1, except that in Example 2, the rare earth chloride in step 1 contains 20% ytterbium (Yb), 2% erbium (Er) and 78% yttrium (Y), oleic acid The mass ratio to rare earth chloride is 10:1; the mass ratio of octadecene to rare earth-oleic acid precursor in step 2 is 100:1; in step 3, the reactant is heated to 300 under the protection of high-purity argon gas Celsius and incubated for 60 minutes.

[0045] The average particle size of the obtained nanoparticles was 32.7 nm, the standard deviation of the particle size within the batch was 1.8, and the standard deviation of the particle size between the batches was 2.2.

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Abstract

The invention discloses a preparation method of an up-conversion fluorescent material with a controllable grain diameter. The preparation method comprises the following steps: step 1, adding rare earth chloride or a rare earth acetic acid compound into a container; then adding oleic acid and heating to obtain a clarified and transparent rare earth-oleic acid precursor; adding sodium hydroxide andammonium fluoride into an organic solvent with a low boiling point so as to obtain a clarified and transparent sodium fluoride precursor; step 2, adding octadecene into the rare earth-oleic acid precursor in step 1 and heating; step 3, cooling the rare earth-oleic acid precursor in step 2; adding the sodium fluoride precursor into the rare earth-oleic acid precursor; raising the temperature of a reactant under the protection of argon gas and carrying out heat insulation and reaction; after the reaction is finished, cooling a reaction mother solution; then centrifuging to precipitate a productin the solution; then washing and precipitating the washed product; dissolving the product in the organic solvent and storing or drying and storing.

Description

technical field [0001] The invention belongs to the field of nanomaterials, in particular to a method for preparing an up-conversion fluorescent material with controllable particle size. Background technique [0002] At present, fluorescent immunochromatography test strips are used in the detection of antigens and antibodies of human-related diseases. Compared with traditional colloidal gold technology, fluorescent immunochromatography technology has the advantages of high sensitivity, wide linear range, and quantitative detection. However, the current fluorescence immunochromatographic detection technology mainly uses down-conversion fluorescence technology, that is, the luminescent substances (fluorescein, lanthanide nanospheres, quantum dot nanoparticles, etc.) are excited by ultraviolet light, and then the emitted visible light is detected for quantification. or qualitative analysis. Due to the inherent problems of fluorescent materials, down-conversion fluorescence tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85B82Y40/00
CPCB82Y40/00C09K11/7773
Inventor 李湘徐琪
Owner 康永生物技术有限公司
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