Preparation method of rare-earth-based fluorite type high-entropy oxide powder material

A technology of oxide powder and fluorite type, applied in the direction of rare earth metal oxides/hydroxides, rare earth metal compounds, chemical instruments and methods, etc., can solve the problem of high reaction temperature, high pressure, complex reaction equipment and preparation process, etc. problem, to achieve the effect of low production cost and low energy consumption

Active Publication Date: 2018-12-07
内蒙古广禾元纳米高科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent of China Authorized Notice No. CN105905935B proposes a method for preparing rare earth oxides or composite oxides with large specific surface area by pyrolysis spraying method. This method has complex reaction equipment and preparation process and high reaction temperature; Compounds are used as raw materials, and HCl gas will be generated durin

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  • Preparation method of rare-earth-based fluorite type high-entropy oxide powder material
  • Preparation method of rare-earth-based fluorite type high-entropy oxide powder material
  • Preparation method of rare-earth-based fluorite type high-entropy oxide powder material

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 43.42g of Ce(NO 3 ) 3 .6H 2 O, 43.30g of La(NO 3 ) 3 .6H 2 O, 43.50g of Pr(NO 3 ) 3 .6H 2 O, 33.64g of Sm(NO 3 ) 3 .6H 2 O and 38.30g of Y (NO 3 ) 3 .6H 2 O was dissolved in 50mL of distilled water, stirred evenly to obtain a mixed solution containing rare earth nitrate; then 90.09g urea was weighed and added to the above mixed solution, after stirring evenly, the pH of the mixed solution was adjusted to be 7 with ammonia water to obtain a transparent sol; The above-mentioned transparent sol was heated in an oil bath at 130°C to remove the solvent water, and a loose, foamy gel was obtained; finally, the above-mentioned gel was placed in a muffle furnace at 350°C for 30 minutes to obtain a crystal structure of fluorite type ( Such as figure 1 shown), the fluorite-type (CeLaPrSmY)O high-entropy oxide powder material with an average particle size of 35nm (such as figure 2 shown).

Embodiment 2

[0028] Weigh 65.13g of Ce(NO 3 ) 3 .6H 2 O, 67.70g of Gd(NO 3 ) 3 .6H 2 O, 64.95g of La(NO 3 ) 3 .6H 2 O, 62.25g of Pr(NO 3 ) 3 .6H 2 O, 50.46g of Sm(NO 3 ) 3 .6H 2 O and 57.45g of Y (NO 3 ) 3 .6H 2 O was dissolved in 100mL of distilled water, and stirred evenly to obtain a mixed solution containing rare earth nitrates; then 180.15g of acetic acid and 54.02g of oxalic acid were weighed and added to the above mixed solution, and after stirring evenly, the pH of the mixed solution was adjusted to 6 with ammonia water to obtain transparent sol; then heat the above transparent sol in an oil bath at 180°C to remove the solvent water to obtain a loose, foamy gel; finally place the above gel in a muffle furnace at 500°C for 15 minutes to obtain an average Fluorite-type (CeGaLaPrSmY)O high-entropy oxide powder material with a particle size of 80nm (such as image 3 shown).

Embodiment 3

[0030] Weigh 43.42g of Ce(NO 3 ) 3 .6H 2 O, 45.14g of Gd(NO 3 ) 3 .6H 2 O, 43.30g of La(NO 3 ) 3 .6H 2 O, 43.84g of Nd(NO 3 ) 3 .6H 2 O, 43.50g of Pr(NO 3 ) 3 .6H 2 O, 33.64g of Sm(NO 3 ) 3 .6H 2 O and 38.30g of Y (NO 3 ) 3 .6H 2 O was dissolved in 100mL of distilled water, and stirred evenly to obtain a mixed solution containing rare earth nitrate; then 42.04g of urea and 42.00g of acetic acid were weighed and added to the above mixed solution, and after stirring evenly, the pH of the mixed solution was adjusted to 8 with ammonia water. Obtain a transparent sol; then heat the above transparent sol in an oil bath at 130°C to remove the solvent water to obtain a loose, foamy gel; finally place the above gel in a microwave oven with a microwave power of 600W for 5 minutes to obtain Fluorite-type (CeGaLaNdPrSmY)O high-entropy oxide powder materials with an average particle size of 120nm (such as Figure 4 shown).

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Abstract

The invention discloses a preparation method of a rare-earth-based fluorite type high-entropy oxide powder material and belongs to the field of rare earth oxide powder materials. The method is a low-temperature combustion synthesis method and specifically comprises the following steps: taking rare earth nitride as a metal source and one or a mixture of more of urea, acetic acid, ammonium acetate,oxalic acid and glycine as fuel; and controlling the concentration of metal salt raw materials, types and adding amounts of the fuel, types and adding amounts of a combustion improver and an ignitionmanner to regulate and control properties including granularity, shapes and the like of rare-earth-based fluorite type high-entropy oxide powder. According to the preparation method disclosed by the invention, liquid-phase ingredients are adopted to ensure that a molecular level of the raw materials is uniform and a stoichiometric proportion of a product is realized; meanwhile, the preparation method has the advantages of energy source saving, high production efficiency, greenness and environment protection, no need of complicated post-treatment and the like; and the prepared rare earth oxidepowder has the advantages of high purity, small granularity and uniformity in distribution.

Description

technical field [0001] The invention belongs to the field of rare earth oxide powder materials, and in particular relates to a method for synthesizing a rare earth-based high-entropy oxide powder material with a fluorite structure by low-temperature combustion. Background technique [0002] In recent years, rare earth composite oxides have been widely used in catalysts and catalyst supports, thermal barrier coatings, functional ceramics, oxygen ion conductors, solid fuel cells, optics and magnetism and other fields. The preparation methods of rare earth oxides mainly include precipitation method, homogeneous precipitation method, hydrothermal method, sol-gel method and spray pyrolysis method. The precursor prepared by the precipitation method is prone to agglomeration in the subsequent drying and calcination process; it is difficult to synthesize a pure-phase rare earth composite oxide powder material by the hydrothermal method, which requires harsh reaction conditions such ...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y30/00
CPCB82Y30/00C01F17/206C01P2002/72C01P2004/03C01P2004/64Y02P20/10
Inventor 冒爱琴权峰俞海云郑翠红檀杰
Owner 内蒙古广禾元纳米高科技有限公司
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