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Preparation method of rare earth-doped fluoride up-conversion luminescent nano dispersion

A nano-dispersion and rare earth doping technology, which is applied in the field of materials and photonics, and chemical industry, can solve the problems of difficult control of sample shape, sensitivity to air, high synthesis cost, etc., and achieve good up-conversion luminescence performance and small particle size , the effect of narrow particle size distribution

Inactive Publication Date: 2018-01-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the hydrothermal / solvothermal method, the first three methods require a higher reaction temperature. In addition, the preparation process of the thermal decomposition method is sensitive to air, requiring an inert gas as a protective gas, and the synthesis cost is relatively high. ;The preparation process of high-temperature solid-phase method requires high-temperature and high-pressure treatment of raw materials, which is not conducive to mass production
The equipment and conditions of the hydrothermal / solvothermal method are simple, and the synthesis process is easy to operate. It is the most common method for preparing nanomaterials. However, the shape of the sample synthesized by this method is difficult to control. Therefore, based on the simple method of hydrothermal / solvothermal method, the proposed A method that can overcome the shortcomings of uncontrollable product morphology and uneven particle size distribution is very important

Method used

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  • Preparation method of rare earth-doped fluoride up-conversion luminescent nano dispersion
  • Preparation method of rare earth-doped fluoride up-conversion luminescent nano dispersion
  • Preparation method of rare earth-doped fluoride up-conversion luminescent nano dispersion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 2.4g of sodium hydroxide solid and dissolve it in 6mL of deionized water. After completely dissolving, mix the solution with 40mL of oleic acid and 40mL of absolute ethanol as solution A; measure erbium chloride, ytterbium chloride and chlorine 24.8mg, 223.2mg and 776.8mg of yttrium oxide solids were dissolved in 22mL of deionized water as solution B; 16mL of quantitatively prepared ammonium fluoride solution was taken as solution C. Adjust the rotation speed of the external circulation type high gravity rotating packed bed to 1000rpm, pass the A solution into the external circulation type high gravity rotating packed bed through the peristaltic pump, and pass the B solution and the C solution from another feed port through the peristaltic The pump is passed into the external circulation type high gravity rotary packed bed, and the feed flow rate of A solution and B and C solutions is set to 3:1. After all the raw material solutions are passed into the external cir...

Embodiment 2

[0033] Weigh 2.4g of sodium hydroxide solid and dissolve it in 6mL of deionized water. After completely dissolving, mix the solution with 40mL of oleic acid and 40mL of absolute ethanol as solution A; measure erbium chloride, ytterbium chloride and chlorine 24.8mg, 223.2mg and 776.8mg of yttrium oxide solids were dissolved in 22mL of deionized water as solution B; 16mL of quantitatively prepared ammonium fluoride solution was taken as solution C. Adjust the rotation speed of the external circulation type high gravity rotating packed bed to 1500rpm, pass the A solution into the external circulation type high gravity rotating packed bed through the peristaltic pump, and pass the B solution and the C solution from another feed port through the peristaltic The pump is passed into the external circulation type high gravity rotary packed bed, and the feed flow rate of A solution and B and C solutions is set to 3:1. After all the raw material solutions are passed into the external cir...

Embodiment 3

[0035]Weigh 2.4g of sodium hydroxide solid and dissolve it in 6mL of deionized water. After completely dissolving, mix the solution with 40mL of oleic acid and 40mL of absolute ethanol as solution A; measure erbium chloride, ytterbium chloride and chlorine 24.8mg, 223.2mg and 776.8mg of yttrium oxide solids were dissolved in 22mL of deionized water as solution B; 16mL of quantitatively prepared ammonium fluoride solution was taken as solution C. Adjust the rotation speed of the external circulation type high gravity rotating packed bed to 2000rpm, pass the A solution into the external circulation type high gravity rotating packed bed through the peristaltic pump, and pass the B solution and the C solution from another feed port through the peristaltic The pump is passed into the external circulation type high gravity rotary packed bed, and the feed flow rate of A solution and B and C solutions is set to 3:1. After all the raw material solutions are passed into the external circ...

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Abstract

The invention discloses a preparation method of a rare earth-doped fluoride up-conversion luminescent nano dispersion, belongs to the cross fields of chemical engineering, materials and photonics, andrelates to a method for preparing the rare earth-doped fluoride up-conversion luminescent nano dispersion by utilizing a super-gravity reaction intensifying technology, i.e. a rotating packed bed reactor. Raw materials and reagents required for realizing the synthetic method of the rare earth-doped fluoride up-conversion luminescent nano dispersion comprise rare earth chlorate, sodium hydroxide,ammonium fluoride, a surfactant, deionized water and absolute ethanol, wherein the rare earth chlorate comprises yttrium chloride, ytterbium chloride and erbium chloride; the surfactant is respectively prepared from oleic acid, oleylamine and sodium citrate; a dispersion solvent is prepared from ethanol, tetrahydrofuran, cyclohexane, chloroform and toluene. According to the preparation method disclosed by the invention, the rotating packed bed reactor is introduced for premixing a reaction precursor solution, and molecular uniform mixing is realized, so that the rare earth-doped fluoride up-conversion luminescent nano dispersion which is small in particle size and narrow in particle size distribution is synthesized.

Description

technical field [0001] The invention belongs to the cross fields of chemical industry, material and photonics, and in particular relates to a method for up-converting luminescent nano-dispersion with rare earth-doped fluoride by using the supergravity technology. Background technique [0002] The up-conversion luminescent material is a luminescent material that excites visible light by near-infrared light, and is a luminescent material based on the anti-Stokes principle. At present, upconversion luminescent materials have been widely used in bioluminescent imaging, three-dimensional display and anti-counterfeiting. Up-conversion luminescent materials are usually composed of two parts: crystal host material and doped rare earth ions. The matrix materials are fluorides (complex fluorides), rare earth oxides (composite oxides), oxyfluorides, halides (oxyhalides), and sulfur-containing compounds. Among them, fluoride and halide (oxyhalide) have lower phonon energy and higher u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/85B82Y30/00B82Y40/00
Inventor 王丹冷静柠蒲源王洁欣陈建峰
Owner BEIJING UNIV OF CHEM TECH
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