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Method for synthesizing zirconium dioxide nanoparticles of special shapes with alcohol-assisted hydrothermal process in one step

A zirconium dioxide and nanoparticle technology, applied in the field of nanomaterials, can solve the problems of increased production cost, high product price, difficulty in finding and the like, and achieves the effects of high yield, low cost, and simple and easy method.

Inactive Publication Date: 2013-07-31
PLA SECOND ARTILLERY ENGINEERING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the solid-phase method reduces the powder calcination temperature and reduces energy consumption, the particle size of the prepared particles is not easy to control
The disadvantage of the gas phase method is that the process is relatively complicated, and the corresponding products are expensive
Although the microemulsion method and the template method can effectively control the size and shape of the product, it is difficult to find a suitable microemulsion system and reaction template.
Although the sol-gel method has low reaction temperature, small product particle size and uniform distribution, the production cost is increased due to the introduction of complexing agents and other organic reagents.
The hydrothermal method has its serious limitations. The most obvious shortcoming is that this method is often only suitable for the preparation of oxides or a few sulfides that are not sensitive to water, while for other water-sensitive compounds such as III-V The preparation of new phosphorus (or arsenic) salt molecular sieve framework materials is not applicable

Method used

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  • Method for synthesizing zirconium dioxide nanoparticles of special shapes with alcohol-assisted hydrothermal process in one step
  • Method for synthesizing zirconium dioxide nanoparticles of special shapes with alcohol-assisted hydrothermal process in one step
  • Method for synthesizing zirconium dioxide nanoparticles of special shapes with alcohol-assisted hydrothermal process in one step

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Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1: Preparation of spindle-shaped monoclinic phase zirconia nanoparticles

[0025] Step 1: Weigh 6.44g ZrOCl 2 ·8H 2 O was dissolved in 14 mL of deionized water to make solution (1); weighed 8.00 g of sodium hydroxide and dissolved in 20 mL of deionized water to make solution (2);

[0026] Step 2: Add solution (2) into solution (1) while stirring, and continue magnetic stirring for 30 minutes;

[0027] Step 3: Then add 6mL of absolute ethanol, at this time Zr 4+ The concentration is 0.5mol / L, OH - The concentration is 5.0mol / L, magnetically stirred for 30min;

[0028] Step 4: After stirring, transfer the solution to a Teflon liner with a volume of 50mL and seal it in a stainless steel autoclave, and react at 150°C for 10h;

[0029] Step 5: Finally, the white precipitate obtained from the above reaction was washed several times with absolute ethanol and distilled water until no chloride ions were detected. The samples obtained by centrifugation were dried...

Embodiment 2

[0031] Embodiment 2: Preparation of rectangular monoclinic phase zirconia nanoparticles

[0032] Step 1: Weigh 6.44g of ZrOCl 2 ·8H 2 O, the sodium hydroxide of 8.00g is mixed with the ZrOCl that concentration is 0.5mol / L 2 or Zr(NO 3 ) 4 Solution (1) and concentration are the sodium hydroxide solution (2) of 5mol / L;

[0033] Step 2: first add solution (1) to deionized water, and then add solution (2) while stirring;

[0034] Step 3: Dissolve the two in a solution of 40mL ethylene glycol and water, at this time Zr 4+ The concentration is 0.5mol / L, OH - The concentration is 5.0mol / L, magnetically stirred for 1h;

[0035] Step 4: After the stirring, transfer the solution to a Teflon liner with a volume of 50 mL and seal it in a stainless steel reactor, and react at 200°C for 12 hours.

[0036] Step 5: After the reactor was naturally cooled to room temperature, the obtained white precipitate was washed several times with absolute ethanol and distilled water until no chlor...

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Abstract

The invention relates to a method for synthesizing zirconium dioxide nanoparticles of special shapes with an alcohol-assisted hydrothermal process in one step. In the method, monoclinic phase fusiform ZrO2 nanoparticles are prepared with an ethanol-assisted hydrothermal process by taking ZrOC12*8H2O and NaOH as raw materials and controlling solution concentration, volume ratio, stirring speed, reaction time and drying temperature to a proper degree; and rectangular monoclinic phase ZrO2 nanoparticles are prepared with an glycol-assisted hydrothermal process by taking ZrOC12*8H2O and NaOH as raw materials and controlling solution concentration, volume ratio, stirring speed, reaction time and drying temperature to a proper degree. Compared with the prior art, the synthesis of the monoclinicphase fusiform ZrO2 nanoparticles and the rectangular monoclinic phase ZrO2 nanoparticles needs no other supplementary means, the process is simple, and the product has high purity, good experimentalrepeatability and excellent heat stability and optical property.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials and relates to zirconium dioxide (ZrO 2 ) A one-step synthesis method of nanoparticles, in particular to a one-step synthesis method of special-morphology zirconia nanoparticles by an alcohol-assisted hydrothermal method. Background technique [0002] Nano Zirconium Dioxide ZrO 2 It is the only amphoteric metal oxide that has both acidic and basic centers, oxidizing and reducing properties among transition metal oxides. At the same time, it is also a p-type semiconductor, which is easy to generate oxygen holes. As a catalyst carrier, it can interact with active components. In addition, ZrO 2 The photophysical and photochemical properties have special application value and can be used for effective treatment of pollutants. ZrO 2 It also has good adsorption effect on dyes, wide adsorption acidity, large adsorption capacity and high adsorption efficiency. If the ZrO 2 When the nanopartic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y40/00
Inventor 贾瑛罗成余志勇刘田田
Owner PLA SECOND ARTILLERY ENGINEERING UNIVERSITY
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