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Method for preparing nano zirconium oxide by internal gel method

A nano-zirconia and zirconium oxychloride technology, applied in the field of material science, can solve the problems of easy agglomeration of zirconia powder and narrow particle size distribution, and achieve the effects of easy reaction, uniform size and good dispersion.

Active Publication Date: 2020-09-11
宁德三祥纳米新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 2) The particle size distribution range is narrow;
[0007] The preparation methods of nano zirconia powder are mainly divided into solid phase method, wet chemical method (precipitation method, sol-gel method, hydrothermal method, emulsion method) and chemical vapor phase method, etc. Zirconia powder has the problem that it is easy to agglomerate. How to eliminate the agglomeration of nano-zirconia powder by simplifying steps is a technical problem that needs to be solved urgently

Method used

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  • Method for preparing nano zirconium oxide by internal gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Weigh 171.2g of zirconium oxychloride (containing crystal water) and 11.85g of yttrium nitrate hexahydrate in the ratio of 3Y, and dissolve them in 250ml of deionized water; weigh 33g of urea and dissolve them in the zirconium solution; weigh 70g of organic monomer : acrylamide, and 3g of cross-linking agent: N, N'-methylenebisacrylamide, dissolved in the above mixed solution; take 5g ammonium persulfate, 2ml tetramethylethylenediamine, add to the solution, stir Evenly and heat to 80°C, wait for 30min, after it is completely gelled, take it out and cut it into small squares of about 0.5mm; soak the small gel pieces in distilled water to wash-filter, repeat several times until the filtrate The chloride ion content is less than 20ppm, and then the colloidal particles are filtered and dried (90°C—110°C); the dried colloid is calcined at a high temperature of 800°C for 4 hours to obtain nano-zirconia powder with good dispersion; The specific surface area of ​​the powder mea...

Embodiment 2

[0040] Weigh 171.2g of zirconium oxychloride (containing crystal water), 5.2g of magnesium chloride, and dissolve them in 250ml of deionized water; weigh 33g of urea and dissolve them in the zirconium solution; weigh 70g of organic monomers: acrylamide, and 3g of Cross-linking agent: N, N'-methylenebisacrylamide, dissolved in the above mixed solution; take 5g of ammonium persulfate and 2ml of tetramethylethylenediamine, add them to the solution, stir evenly and heat to 80°C, Wait for 30 minutes, after it is completely gelled, take it out and cut it into small squares of about 0.5mm; soak the small gel pieces in distilled water to clean-filter, repeat several times until the chloride ion content of the filtrate is less than 20ppm, Then filter and dry the colloidal particles (90°C—110°C); place the dried colloid at a high temperature of 800°C for 4 hours to obtain nano-zirconia powder with good dispersion; measure the powder with a specific surface area meter The specific surfac...

Embodiment 3

[0042] A kind of method for preparing nano zirconia by inner gel technology, is characterized in that, comprises the following steps:

[0043] Step 1: Mix soluble zirconium source and soluble yttrium source, mix with deionized water, and prepare solution A of 0.5-2.0mol / L, the total weight of zirconium source and yttrium source is M1, and the molar ratio zirconium: urea is 1: 1.1 Weigh urea and add it to solution A to obtain solution B; the soluble yttrium source is any one or two of yttrium chloride, yttrium oxalate, yttrium nitrate, and yttrium acetate; the soluble zirconium source is oxychloride Any one or both of zirconium oxide and zirconium acetate; the molar ratio of zirconium and yttrium in the reaction solution A is 97:6;

[0044] Step 2: Weigh acrylamide with a weight of M2 and N, N'-methylenebisacrylamide with a weight of M3, and put them into solution A for dissolution to obtain solution C, wherein M2:M1 is 1:4-1:3 , M3:M2 is 1:30-1:15;

[0045] Step 3: adding am...

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Abstract

The invention belongs to the technical field of material science, and particularly relates to a method for preparing nano zirconium oxide by an internal gel method. The method comprises the followingsteps of: carrying out in-situ curing on a zirconium source and a urea solution through chemical gel, continuously heating to urea decomposition to convert the colloid into a precursor of zirconium oxide, drying the colloid and calcining at 800 DEG C for 4 hours to obtain high-quality composite nanometer zirconium oxide. The reaction is a uniform reaction, the nucleation granularity is uniform, sothat the composite nano zirconium oxide powder with uniform size and good dispersity is obtained; and compared with a traditional gel method process, the method has the advantages of small colloidalparticles, easiness in reaction, convenience in cleaning, loading and transportation, and elimination of agglomeration of the nano zirconium oxide powder while operation steps are simplified.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a method for preparing nanometer zirconia by an internal gel method. Background technique [0002] Nano zirconia powder helps to optimize the performance of zirconia ceramics, and the preparation of nano zirconia powder has always been a research hotspot. The manufacture of high-performance ceramic materials has high requirements for the powder used. In addition to the requirements for accurate, uniform chemical composition and phase composition of the powder, and low impurity content, there are strict requirements for the shape and size of the particles in the powder. It can be roughly summarized as follows: [0003] 1) The particle size is small; [0004] 2) The particle size distribution range is narrow; [0005] 3) The particle shape is preferably spherical or equiaxed; [0006] 4) There is no agglomeration or a small degree of agglomeration among the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y30/00B82Y40/00
CPCC01G25/02B82Y30/00B82Y40/00C01P2002/72C01P2004/64C01P2006/12
Inventor 周志永姜波骆兵
Owner 宁德三祥纳米新材料有限公司
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