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Method of preparing nanometer hafnium oxide particles of different crystal forms by adjusting alkali concentration

A technology of hafnium dioxide and hafnium oxychloride is applied in the field of preparation of nanometer hafnium dioxide materials, can solve the problems of poor powder dispersibility, expensive raw materials, high agglomeration, etc., and achieves good application prospects, good dispersibility, and particle size. Evenly distributed effect

Inactive Publication Date: 2016-11-09
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sol-gel method is a powder material preparation method developed in the 1960s. The advantages of this method are low reaction temperature, easy control, and high purity of the obtained powder, but the required raw materials are usually expensive and not easy to produce. Industrial production; the microemulsion method requires subsequent high-temperature roasting, and the obtained powder has poor dispersion and high agglomeration

Method used

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  • Method of preparing nanometer hafnium oxide particles of different crystal forms by adjusting alkali concentration
  • Method of preparing nanometer hafnium oxide particles of different crystal forms by adjusting alkali concentration
  • Method of preparing nanometer hafnium oxide particles of different crystal forms by adjusting alkali concentration

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Effect test

Embodiment 1

[0029] (1) Weigh 0.16g of hafnium tetrachloride powder and dissolve it in 10mL of deionized water to form a hafnium oxychloride solution;

[0030] (2) Weigh 2.4g of sodium hydroxide and dissolve it in 10mL of deionized water, then drop the alkali solution into the hafnium oxychloride solution to obtain a mixed solution;

[0031] (3) Transfer the obtained mixed solution to a high-pressure hydrothermal reactor with a polytetrafluoroethylene liner of 100 mL, then tighten the reactor, place it in a blast drying oven, and react at 120° C. for 24 hours.

[0032] (4) After the reaction is over, after the high-pressure hydrothermal reactor is naturally cooled to room temperature, wash with absolute ethanol, centrifuge at 10,000rpm for 15min to remove the supernatant, then wash with deionized water, and centrifuge at 10,000rpm Centrifuge for 15 minutes to remove the supernatant, repeat this cycle 3 times, finally wash with absolute ethanol, centrifuge at 10,000 rpm for 15 minutes to ob...

Embodiment 2

[0035] (1) Weigh 0.16g of hafnium tetrachloride powder and dissolve it in 10mL of deionized water to form a hafnium oxychloride solution;

[0036] (2) Weigh 4.0 g of sodium hydroxide and dissolve it in 10 mL of deionized water, then drop the alkali solution into the hafnium oxychloride solution to obtain a mixed solution;

[0037] (3) Transfer the obtained mixed solution to a high-pressure hydrothermal reactor with a polytetrafluoroethylene liner of 100 mL, then tighten the reactor, place it in a blast drying oven, and react at 120° C. for 24 hours.

[0038] (4) After the reaction is over, after the high-pressure hydrothermal reactor is naturally cooled to room temperature, wash with absolute ethanol, centrifuge at 10,000rpm for 15min to remove the supernatant, then wash with deionized water, and centrifuge at 10,000rpm Centrifuge for 15 minutes to remove the supernatant, repeat this cycle 3 times, finally wash with absolute ethanol, centrifuge at 10,000 rpm for 15 minutes to ...

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Abstract

The invention relates to a method of preparing nanometer hafnium oxide particles of different crystal forms by adjusting alkali concentration. The method includes the steps that at the room temperature, an alkaline solution is added into a hafnium oxide solution dropwises to obtain a mixed solution; the mixed solution is subjected to reaction at the constant temperature of 100-130 DEG C, and the nanometer hafnium oxide particles are obtained through washing, centrifuging and drying. The method has the advantages of being simple in operation method, high in repeatability, low in temperature requirement and free of calcinations, and reaction conditions are easy to control; the crystal form of the product can be controlled by controlling the alkali concentration in the solution; the prepared good nanometer hafnium oxide particles are uniform in particle size distribution and high in dispersity and have good application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of nano hafnium dioxide materials, in particular to a method for preparing nano hafnium dioxide particles of different crystal forms by adjusting the concentration of alkali. Background technique [0002] Hafnium dioxide is a ceramic material with wide bandgap and high dielectric constant, especially in the field of microelectronics, which has attracted extreme attention. In addition, it can also be used as refractory materials, anti-radiation coatings and catalysts. [0003] Currently, about nano-HfO 2 There are many preparation methods, mainly hydrothermal method, sol-gel method, microemulsion method, co-precipitation method and so on. The sol-gel method is a powder material preparation method developed in the 1960s. The advantages of this method are low reaction temperature, easy control, and high purity of the obtained powder, but the required raw materials are usually expensive and not easy to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G27/02
CPCC01G27/02C01P2002/72C01P2004/04C01P2004/64
Inventor 周兴平万盈盈
Owner DONGHUA UNIV
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