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A small size β-naref 4 Preparation method of phosphor powder

A fluorescent powder, small-sized technology, applied in chemical instruments and methods, luminescent materials, nano optics, etc., can solve the problems of unreported hydrothermal, difficult control of reaction conditions, poor dispersion, etc.

Inactive Publication Date: 2020-08-07
INNER MONGOLIA NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction conditions are not easy to control, the product agglomerates seriously, the dispersion is poor, it is not easy for biological application, and subsequent high temperature treatment is required
[0007] The hydrothermal method can prepare nanomaterials in large quantities, and has good repeatability and is easy to operate, but the particle size of the prepared nanomaterials is relatively large, and it is impossible to prepare small-sized nanomaterials (such as nanomaterials smaller than 20nm)
[0008] Hydrothermal (solvothermal) / thermal decomposition combined technology has not been reported so far

Method used

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  • A small size β-naref <sub>4</sub> Preparation method of phosphor powder
  • A small size β-naref <sub>4</sub> Preparation method of phosphor powder
  • A small size β-naref <sub>4</sub> Preparation method of phosphor powder

Examples

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preparation example Construction

[0028] (1) Preparation of the precursor: the rare earth oxide 78% RE with a total molar mass of 4-6 mmol 2 o 3 and other doped rare earth oxides Ln 2 o 3 (Ln=20%Yb, 2%Ho or Er or Tm) into a 100mL high-temperature reactor, then add a mixed solution of trifluoroacetic acid and water with a volume of 11-66mL, and then electric heating at 80-140°C Reaction in blast drying oven for 12-24h. After the reactor was cooled for 12 hours, the reaction solution of the trifluoroacetate precursor was taken out and divided into 4-6 parts (about 1 mmol in total) and transferred to a three-necked round-bottomed flask, followed by stirring and drying at 60°C for 8 hours to obtain 4-6 parts of trifluoroacetate precursor of white solid powder.

[0029] (2) Rare earth doped β-NaREF 4Preparation of nanocrystals: the total volume is 30-40mL, the mixed solution of oleic acid (OA) and 1-octadecene (ODE) (volume ratio is 1:1) is added to the above-mentioned white solid trifluoroacetate precursor I...

example 1

[0030] Example 1: β-NaGdF 4 : Preparation of 20%Yb, 2%Er nanocrystals

[0031] Weigh 0.0153g erbium oxide (Er 2 o 3 ), 0.1577g ytterbium oxide (Yb 2 o 3 ) and 0.5658g gadolinium oxide (Gd 2 o 3 ) into a 100mL high-temperature reactor, and then a mixed solution of trifluoroacetic acid and water (volume ratio = 2:9) with a total volume of 44mL was added, and the reaction was carried out in an electrothermal constant temperature blast drying oven at 80°C for 24h. After the reaction kettle was cooled for 12 hours, the reaction solution of the trifluoroacetate precursor was taken out and divided into 4 parts (about 1 mmol in total molar weight) and transferred to four 100 mL three-necked round-bottomed flasks, followed by stirring and drying at 60 °C for 8 hours. 4 parts of trifluoroacetate precursors of white solid powder were obtained respectively. A one-to-one mixed solution of oleic acid (OA) and 1-octadecene (ODE) with a total volume of 30 mL was added to the above-ment...

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Abstract

The invention relates to the technical field of preparation of nano-materials, in particular to a method for preparing beta-NaRE F4 fluorescent powder, particularly to a method for preparing small-sized (less than or equal to 10 nm) nano beta--NaREF4 fluorescent powder. The technological process has the technical characteristic that the hydrothermal method and the thermolysis are combined. A precursor (RE(CF3COO)3:20% Yb, 2% Er) is prepared by the hydrothermal method, and a product NaREF4:20% Yb, 2% Er (Ho / Tm) is prepared from such high-melting-point organic solvents as oleic acid and octadecene by the thermolysis method.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to β-NaRE F 4 Powder preparation method, especially small size (≤10nm) nanometer β-NaREF 4 Preparation method of fluorescent powder. Background technique [0002] Rare earth-doped upconversion luminescent nanomaterials refer to rare earth luminescent materials that convert low-energy photons into high-energy photons through mechanisms such as multi-photon absorption and energy transfer. Compared with fluorescent dyes and quantum dot materials, rare earth-doped upconversion luminescent nanomaterials have the advantages of non-toxicity, good optical stability, good chemical stability, long luminescent lifetime, and narrow emission peak. In addition, since rare earth-doped upconversion luminescent nanomaterials use infrared light as the excitation light source, it can avoid the interference of biological samples’ own fluorescence background, and can effectively impro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85B82Y40/00B82Y20/00
Inventor 德格吉呼
Owner INNER MONGOLIA NORMAL UNIVERSITY