CN-116692921-B - Al (aluminum) alloy2O3/CeO2Synthesis method of hexagonal biconic particles and obtained product

Abstract

The invention discloses a synthesis method of Al 2 O 3 /CeO 2 hexagonal biconical particles and an obtained product, which comprises the steps of dissolving soluble cerium salt and 2-methylimidazole in methanol, standing, washing and drying a precipitate to obtain Ce-MOF, adding aluminum nitrate nonahydrate (Al (NO 3 ) 3 ·9H 2 O), ce-MOF, tetra-N-octylammonium bromide and L-lysine into a mixed solution of N, N-dimethylformamide, methanol, ethylene glycol and neopentyl glycol, heating in a water bath, irradiating by an ultraviolet lamp, carrying out hydrothermal reaction on the obtained uniform solution, centrifuging, drying and calcining the product to obtain the Al 2 O 3 /CeO 2 hexagonal biconical structure.

Inventors

• MA QIAN
• WANG XUEYING
• WANG YI
• ZHANG QI
• LI LINGYU
• ZHAO DONGHENG

Assignees

• 济南大学

Dates

Publication Date

20260508

Application Date

20230403

Claims (2)

1. 1. The synthesis method of the Al 2 O 3 /CeO 2 hexagonal biconical particles is characterized by comprising the following steps of: (1) Dropwise adding a methanol solution containing cerium nitrate hexahydrate (Ce (NO 3 ) 3 ·6H 2 O) into an equal volume of a methanol solution of 2-methylimidazole at room temperature, continuously stirring for 2h, forming a flocculent complex, and standing for 24 h at room temperature to form a precipitate, wherein the concentration of the Ce (NO 3 ) 3 ·6H 2 O/methanol solution is 0.1-0.5 mol/L and the concentration of the 2-methylimidazole/methanol solution is 0.6-1.2 mol/L; then centrifugally washing the product, drying at 60 ℃ for 5h to obtain Ce-MOF, adding aluminum nitrate nonahydrate (Al (NO 3 ) 3 ·9H 2 O), ce-MOF, tetra-N-octyl ammonium bromide and L-lysine into a mixed solution of N, N-dimethylformamide, methanol, ethylene glycol and neopentyl glycol, wherein the concentration of Al (NO 3 ) 3 ·9H 2 O in the mixed solution is 0.03-0.05 mol/L, the volume ratio of N, N-dimethylformamide, methanol, ethylene glycol and neopentyl glycol is 1:0.25-0.30:0.02-0.10:0.04-0.06, the mass ratio of Al (NO 2-MOF, tetra-N-octyl ammonium bromide and L-lysine is 1:0.2-0.3:0.01-0.02:0.005-0.010, heating and stirring the mixed solution in an ultraviolet lamp auxiliary water bath, wherein the wavelength of the ultraviolet light is 120-150/ 2 , the temperature of the ultraviolet light is 120-150/ 2 , the temperature of the water bath is between 50 ℃ and 60 ℃, the heat transfer time is between 24-150 ℃ and the heat transfer reaction kettle is carried out in a sealed condition of between 150 ℃ and 24 ℃ and 150 ℃ under the conditions of the reaction kettle, centrifugally drying the product at a drying temperature of 60 ℃ for a drying time of 5h to obtain precursor particles; (2) And (3) calcining the precursor at high temperature in a muffle furnace to obtain the Al 2 O 3 /CeO 2 composite material, wherein the calcining system is that the temperature is raised to 600-700 ℃ according to the heating rate of 1-5 ℃ per minute in the air atmosphere, and the temperature is kept for 2-4 h, so that the Al 2 O 3 /CeO 2 is hexagonal biconical particles.
2. 2. The synthesis method according to claim 1, wherein the obtained Al 2 O 3 /CeO 2 hexagonal biconic particles have a size of 0.5-5.0 μm, and have a hexagonal biconic structure at both ends and a short column size of 0.2-2.5 μm in the middle region.

Description

Synthesis method of Al 2O3/CeO2 hexagonal biconical particles and obtained product Technical Field The invention relates to a synthesis method of Al 2O3/CeO2 hexagonal bipyramid particles, in particular to a solvothermal synthesis method of an Al 2O3/CeO2 hexagonal bipyramid structure with adjustable growth size and controllable morphology. Background In recent years, oxide semiconductor materials have shown great application value in the fields of energy, photoelectricity, sensing and the like, and have attracted wide attention. By controlling the microstructure (such as size, crystal exposed surface, lattice defect, crystal phase composition, etc.) of the oxides, unique physical and chemical properties can be obtained, and the oxides have been widely applied to chemical, magnetic, mechanical, optical, electrical and other devices. Al 2O3 has the characteristics of large elastic modulus, good thermal stability, high hardness, friction resistance, corrosion resistance, good insulativity, rich raw material sources, low price and the like. Is widely applied to various fields such as catalyst carriers, automobile industry, chemical industry, cutting tools, aerospace and the like. With the rapid development of industries such as bioceramics, medical drugs, electronics, machinery, etc., the market demand for alumina is increasing, and the production and demand of Al 2O3 is further increasing. Common Al 2O3 materials are mainly synthesized by two modes of a chemical method and a physical method. CeO 2 is a rare earth metal oxide semiconductor material with rich reserves and low price, and the band gap is 2.7 eV, which is always paid attention to. CeO 2 has physical and chemical characteristics of adjustable oxygen vacancy concentration (Ce 3+ and Ce 4+ through reversible conversion), high oxygen storage capacity, high oxygen ion conductivity and the like, and has important application prospects in the fields of sensors, electrons, glass polishing materials and magnetic materials. For example, ceO 2 nano-particles can be used in the field of mechanical polishing solutions and can also be used as excellent photocatalyst degradation materials. The existing CeO 2 synthesis methods mainly comprise a calcination method, a hydrothermal (solvothermal) method, a sol-gel method and an electrochemical method. The precipitation method and the heat treatment method are often used for preparing the oxide-based composite material, and have the advantages of low energy consumption, simple equipment and the like, but the obtained Al 2O3 and the microstructure of the composite material are mainly sphere-like, and the process route for synthesizing the polyhedral micro-nano structure is not common. Up to now, no report on the size-adjustable and shape-controllable Al 2O3/CeO2 hexagonal biconical particles is found at home and abroad. In practice, by regulating and controlling water bath reaction and ultraviolet irradiation parameters, a novel reaction system is designed, the size regulation of Al 2O3/CeO2 hexagonal biconical particles can be obtained, the large-scale production of the Al 2O3/CeO2 composite material is realized, and the application of the Al 2O3/CeO2 composite material in the fields of mechanical polishing, industrial catalysis, automobile exhaust purification, fuel cells, precise ceramics, paint additives, gas-sensitive sensing, flame retardants, magnetic media, abrasives, catalytic reactions and the like is promoted. Disclosure of Invention Aiming at the situation that a method for preparing an Al 2O3/CeO2 polyhedral structure by combining a precipitation method and a heat treatment method is not used in the prior art, the invention provides a preparation method of Al 2O3/CeO2 hexagonal biconical particles, which comprises the steps of preparing Ce-MOF by the precipitation method, and synthesizing a final Al 2O3/CeO2 composite material by combining a subsequent hydrothermal and calcining technology. The invention provides a preparation method of Al 2O3/CeO2 hexagonal biconical particles, which comprises the following steps: (1) Dropwise adding a methanol solution containing Ce (NO 3)3·6H2 O) into an equal volume of a methanol solution of 2-methylimidazole at room temperature, continuously stirring for 2h to form flocculent complex, and standing for 24h at room temperature to form precipitate; (2) Centrifugally washing and drying the product of the step (1) to obtain Ce-MOF; (3) Adding Al (NO 3)3·9H2 O, ce-MOF in the step (2), tetra-N-octylammonium bromide and L-lysine into a mixed solution of N, N-dimethylformamide, methanol, ethylene glycol and neopentyl glycol; (4) Placing the mixed solution in the step (3) under irradiation of an ultraviolet lamp with the wavelength of 365 nm, heating and stirring in a water bath, and obtaining a uniform mixed solution after a certain time; (5) Transferring the mixed solution obtained in the step (4) into a reaction kettle, and performing solvothermal reaction under a closed co