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Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges

A technology with positive charges and rare earth metals, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of easy dehydration structure of hydroxide nanosheets, poor thermal stability, and reduced luminescence performance of rare earth hydroxide materials and other issues, to achieve good application prospects, good luminous performance, and save preparation time

Inactive Publication Date: 2014-09-17
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most rare earth ion-doped nanoluminescent materials reported in the past are rare earth hydroxide nanosheets, but rare earth hydroxide nanosheets have certain disadvantages.
For example: there are a large number of hydroxyl groups in rare earth hydroxide nanosheets, and the phonon coupling vibration of hydroxyl groups will absorb the characteristic fluorescence of some rare earth elements (such as: Eu 3+ ), which in turn will lead to a significant reduction in the luminescent properties of rare earth hydroxide materials
In addition, the rare earth hydroxide nanosheets have poor thermal stability. When the temperature exceeds a certain temperature, the hydroxide nanosheets are easy to dehydrate and the structure is destroyed.

Method used

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  • Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges
  • Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges
  • Preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Take 2.0005gY 2 o 3 and 0.1641gEu 2 o 3 , dissolved in 150ml of 0.5mol / L nitric acid solution to obtain a transparent solution, then added 35ml of 1mol / L oxalic acid solution to obtain an oxalate precipitate, and calcined the oxalate precipitate at 720°C for 2 hours to obtain Y 1.9 Eu 0.1 o 3 . Take 1.0529gY 1.9 Eu 0.1 o 3 , add 1.7770gNH 4 Br, and then grind the two in a mortar and mix well.

[0022] b. Transfer the mixture obtained in the above steps into a crucible, shake it tightly and put it into a muffle furnace. The heating condition is 420°C for 2 hours, then heat up to 700°C for 2 hours, after cooling to room temperature, take out the sample and use the pre-prepared 100ml concentration of 1×10 -4 mol / L acetic acid solution, 200ml distilled water to wash the sample, then suction filter and dry to obtain pure Y 0.95 Eu 0.05 OBr.

[0023] c. Take the Y obtained in the previous step of 1.0000g 0.95 Eu 0.05 OBr, put it in 100ml of sodium benzoate...

Embodiment 2

[0026] a. Take 1.0025gY 2 o 3 and 0.0822gEu 2 o 3 , dissolved in 80ml of nitric acid solution with a concentration of 0.5mol / L to obtain a transparent solution, then add 25ml of oxalic acid solution with a concentration of 1mol / L to obtain an oxalate precipitate, and calcinate the oxalate precipitate at 750°C for 2 hours, get Y 1.9 Eu 0.1 o 3 . Take 0.5026gY 1.9 Eu 0.1 o 3 , adding 1.0602gNH 4 Br, and then grind the two in a mortar and mix well.

[0027] b. Transfer the mixture obtained in the above steps into a crucible, shake it tightly and put it into a muffle furnace. The heating condition is 450°C for 2 hours, then heat up to 680°C for 2 hours, after cooling to room temperature, take out the sample and use the pre-prepared 80ml concentration of 1×10 -4 mol / L acetic acid solution, 120ml distilled water to wash the sample, then suction filter and dry to obtain pure Y 0.95 Eu 0.05 OBr.

[0028] c. Take 1.5000g of Y obtained in the previous step 0.95 Eu 0.05 ...

Embodiment 3

[0031] a. Take 3.5000gY 2 o 3 and 0.2985gTb 2 o 3 , dissolved in 220ml of nitric acid solution with a concentration of 0.5mol / L to obtain a transparent solution, then add 60ml of oxalic acid solution with a concentration of 1mol / L to obtain an oxalate precipitate, and calcinate the oxalate precipitate at 750°C for 3 hours, get Y 1.9 Tb 0.1 o 3 . Take 2.5890gY 1.9 Tb 0.1 o 3 , adding 10.8912gNH 4 Br, and then grind the two in a mortar and mix well.

[0032] b. Transfer the mixture obtained in the above steps into a crucible, shake it tightly and put it into a muffle furnace. The heating condition is 400°C for 2.5 hours, then heat up to 720°C for 2 hours, after cooling to room temperature, take out the sample and use the pre-prepared 250ml concentration of 1×10 -4 mol / L acetic acid solution, 500ml distilled water to wash the sample, then suction filter and dry to obtain pure Y 0.95 Tb 0.05 OBr.

[0033] c. Take 2.0000g of Y obtained in the previous step 0.95 Tb ...

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Abstract

The invention discloses a preparation method of fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges. The method takes yttrium oxide, europium oxide, terbium oxide, ammonium bromide, sodium benzoate, HTTA (thenoyltrifluoroacetone) and the like as materials. The preparation method comprises the steps of firstly, roasting at a high temperature to obtain Y1.93Ln0.1O3 and Y0.95Ln0.05OBr layered materials; under microwave heating condition, intercalating for the layered materials by utilizing sodium benzoate liquor to obtain intercalated materials; and finally, carrying out ultrasonic treatment onto the intercalated materials and the HTTA in a n-butyl alcohol solvent to obtain the fluorescence-enhanced rear-earth metal oxide nanosheet sol with positive charges. The preparation method disclosed by the invention is simple in preparation process and environmental friendly.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis materials, in particular to a positively charged rare earth metal oxide (Y 0.95 ln 0.05 o + ) Preparation method of nanosheet sol. Background technique [0002] Nano-luminescent materials are an important solid functional material. Due to their various characteristics in shape and properties, they have incomparable advantages in various applications. The emergence of nano-luminescent materials has greatly promoted the development of nano-electronic devices. develop. In recent years, nano-luminescent materials doped with rare earth ions have attracted widespread attention. However, whether it is a zero-dimensional quantum dot or a one-dimensional nanowire, the rare earth ions in the inner layer cannot be fully utilized. If layered luminescent materials can be obtained, and single-layer nanosheet luminescent materials can be obtained by methods such as exfoliation, then the above...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C09K11/78
Inventor 李强张琳张艳艳史王艳杨薇吴莲莲
Owner EAST CHINA NORMAL UNIV
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