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One-step synthesis method of tetragonal zirconium dioxide by means of water-assisted diethylene glycol

A technology of diethylene glycol and zirconia, applied in the field of nanomaterials

Inactive Publication Date: 2013-09-11
CHINA FIRST AUTOMOBILE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the patent CN 1935670A, the tetragonal phase zirconia was synthesized by adding hydrazine hydrate as an alkaline mineralizer by hydrothermal method, but there is still a relatively large proportion of monoclinic phase zirconia in the product

Method used

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  • One-step synthesis method of tetragonal zirconium dioxide by means of water-assisted diethylene glycol
  • One-step synthesis method of tetragonal zirconium dioxide by means of water-assisted diethylene glycol
  • One-step synthesis method of tetragonal zirconium dioxide by means of water-assisted diethylene glycol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Measure 3ml of water and 7ml of diethylene glycol, stir well and add 2.15g of zirconium nitrate pentahydrate; prepare 5ml of 5mol / L sodium hydroxide solution;

[0022] Step 2: Under stirring conditions, mix the two solutions prepared above, continue to stir for 15 minutes to make the reaction system uniform, move to a 25ml polytetrafluoroethylene-lined stainless steel reaction kettle, seal it and place it in an oven at 180°C for 8 hours ; Step 3: Wash the reaction product 2-3 times with water, 2 times with alcohol, and dry at 40°C for 10 hours.

[0023] Obtain high-purity tetragonal self-stabilized zirconia nanoparticles with a particle size of about 50nm. like figure 1 It is the X-ray diffraction spectrum of the product tetragonal phase zirconia nanoparticles, and the particle size is calculated to be about 50nm through computer simulation. figure 2 It is a scanning electron micrograph of the product tetragonal phase zirconia, as shown in the figure, the par...

Embodiment 2

[0025] Step 1: Measure 3ml of water and 7ml of diethylene glycol, stir well and add 2.15g of zirconium nitrate pentahydrate; prepare 7.5ml of 5mol / L sodium hydroxide solution;

[0026] Step 2: with embodiment 1 step 2;

[0027] Step 3: same as embodiment 1 step 3;

[0028] Obtain high-purity tetragonal self-stabilized zirconia nanoparticles with a particle size of about 50nm.

Embodiment 3

[0030] Step 1: Measure 3ml of water, 7ml of diethylene glycol, stir evenly and add 1.61g of zirconium oxychloride octahydrate; prepare 5ml of 5mol / L sodium hydroxide solution;

[0031] Step 2: with embodiment 1 step 2;

[0032] Step 3: same as embodiment 1 step 3;

[0033] Obtain high-purity tetragonal self-stabilized zirconia nanoparticles with a particle size of about 50nm.

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Abstract

The invention relates to a one-step synthesis method of tetragonal zirconium dioxide by means of water-assisted diethylene glycol. The method is characterized by comprising the following specific steps of: (1) preparing a mixed solvent according to the diethylene glycol / water volume ratio of 3 / 7-7 / 3, and adding zirconate into the mixed solvent to prepare a 0.1-0.5mol / L solution; and preparing a 1-5mol / L sodium hydroxide solution or a potassium hydroxide solution; (2) uniformly mixing the two solutions, moving the mixed solution to a polytetrafluoroethylene lined stainless steel reaction kettle, placing the reaction kettle in a constant-temperature drying box at 150-200 DEG C and still standing for 4-20 hours; and (3) centrifugally separating the obtained solid product, water-washing the solid product for 2-3 times, washing the product by using anhydrous ethanol for 2 times, and drying the washed product at 40-60 DEG C. The synthesis method is simple in process, high in product purity, small in product particle size, good in experimental repeatability, and excellent in thermal stability, and can be applied to a high-temperature reaction catalyst carrier.

Description

technical field [0001] The invention relates to a water-assisted one-step synthesis method of tetragonal zirconium dioxide and belongs to the technical field of nanometer materials. Background technique [0002] Zirconium dioxide is an extremely important p-type semiconductor material, which has important applications in the fields of high-performance materials, fuel cells, catalysts, and sensors. [0003] Zirconium dioxide has three crystal phases: monoclinic phase, tetragonal phase and cubic phase. Zirconium dioxide only appears in monoclinic phase at room temperature, and it will transform into tetragonal phase when heated to about 1100 ° C. It will transform into cubic phase when heated to a higher temperature. Mutually. Since a large volume change occurs when the monoclinic phase transforms to the tetragonal phase, a large volume change occurs in the opposite direction when cooled. High-purity single tetragonal zirconia is stable at room temperature, does not change i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y40/00
Inventor 张斌王金兴韩金磊张克金米新艳王丹曹婷婷魏晓川安宇鹏
Owner CHINA FIRST AUTOMOBILE
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