Method for preparing nano spinel ferrite with equal grain size

The technology of spinel ferrite and nano-spinel is applied in the field of preparation of nano-spinel ferrite, which can solve the problems of environmental pollution, difficult operation and high preparation cost, and achieves reduction of energy consumption and particle size distribution. Uniform, controllable preparation results

Inactive Publication Date: 2008-04-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing nano spinel ferrite with uniform particle size, which solves the problems of difficult operation, high preparation cost and serious environmental pollution, and realizes the controllable preparation of particle size under low temperature conditions. Uniform nano-spinel ferrite

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0018] Accurately weigh Co(NO 3 ) 3 ·6H 2 O, Fe (NO 3 ) 3 ·9H 2 O, prepared into a mixed salt solution with deionized water, the concentrations of metal ions in the solution are: [Co 2+ ]=0.2M, [Fe 3+ ]=0.4M, put this mixed solution into a beaker. Separately prepared NaBH 4 and polyvinylpyrrolidone (PVP) mixed solution, in which [NaBH 4 ]=1.5M, [PVP]=1.8g / L. Mix equal volume of mixed salt solution with NaBH 4 Pour the mixed solution with PVP into a rapidly rotating colloid mill (6000 rpm), and stir vigorously for 5 minutes. After that, the nano metal particles obtained by reduction were transferred to an autoclave with a polytetrafluoroethylene liner, and hydrothermally crystallized at 120° C. for 12 hours. After naturally cooling to room temperature, the obtained precipitate was washed with deionized water until neutral. Dry at 40°C for 12 hours to obtain CoFe with an average particle size of 18nm 2 O 4 Spinel nanoparticles.

Embodiment 2

[0020] Accurately weigh Ni (NO 3 ) 3 ·6H 2 O, Fe (NO 3 ) 3 ·9H 2 O, prepared into mixed salt solution with deionized water, the concentrations of metal ions in the solution are: [Ni 2+ ]=0.25M, [Fe 3+ ]=0.5M, put this mixed solution into a beaker. Separately prepared NaBH 4 and polyvinyl alcohol (PVA) mixed solution, in which [NaBH 4 ]=1.0M, [PVA]=3.2g / L. Mix equal volume of mixed salt solution with NaBH 4 Pour into a rapidly rotating colloid mill (4500 rpm) together with the mixed solution of PVA, and stir vigorously for 5 minutes. After that, the nano metal particles obtained by reduction were transferred to an autoclave with a polytetrafluoroethylene liner, and hydrothermally crystallized at 200° C. for 24 hours. After naturally cooling to room temperature, the obtained precipitate was washed with deionized water until neutral. Dry at 40°C for 12 hours to obtain NiFe with an average particle size of 52nm 2 O 4 Spinel nanoparticles.

Embodiment 3

[0022] Accurately weigh Co(NO 3 ) 3 ·6H 2 O, Fe (NO 3 ) 3 ·9H 2 O, Cu(NO 3 ) 2 ·3H 2 O was prepared into a mixed salt solution with deionized water, and the concentrations of metal ions in the solution were: [Co 2+ ]=0.4M, [Fe 3+ ]=1.0M, [Cu 2+ ]=0.1M This mixed solution was placed in a beaker. Separately prepared NaBH 4 and polyvinylpyrrolidone (PVP) mixed solution, in which [NaBH 4 ]=1.2M, [PVP]=4.0g / L. Mix equal volume of mixed salt solution with NaBH 4 Pour the mixed solution with PVP into a rapidly rotating colloid mill (3000 rpm), and stir vigorously for 7 minutes. After that, the nano-metal particles obtained by reduction were transferred to an autoclave with a polytetrafluoroethylene liner, and hydrothermally crystallized at 150° C. for 6 hours. After naturally cooling to room temperature, the obtained precipitate was washed with deionized water until neutral. Dry at 40°C for 12 hours to obtain Co with a particle size of 27nm 0.8 Cu 0.2 Fe 2 O 4 Spine...

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Abstract

The invention relates to a preparation method of particle size homogeneous nanometer spinel ferrite, which belongs to the art of the metal oxides preparation. Metallic ion is first deoxidized into highly scattered nanometer metallics in a colloid mill, and then the blended solution containing the nanometer metallics is transferred into a Teflon gallbladder for water hot crystallization under high-pressured reaction so as to form the spinel ferrite particle with a diameter of 5 to 200 nanometers. The invention has the advantages that the high-speed shearing action of the colloid mill ensures that the deoxidized metallics are highly dispersed, thereby enabling the particle size homogeneous nanometer spinel ferrite. The reaction is carried in the solution, and the diameter of the nanometer particle can be controlled through adjusting the reactant density, the reaction temperature and the reaction time; since no need for high-temperature roasting process in the reaction, the operation becomes quite easy. Moreover, the invention has low cost and low energy consumption, thereby being favorable for industrialized application.

Description

technical field [0001] The invention belongs to the technical field of metal oxide preparation, and in particular relates to a preparation method of nano spinel ferrite with uniform particle size, and the particle size can be controllably prepared under low temperature conditions. Background technique [0002] Ferrite is a composite oxide composed of iron and one or more other metals, which is widely used in various fields such as communication broadcasting, radar navigation, astronautics, medical biology and so on. In recent years, with the continuous development of materials science, the development and research of nanomaterials are used to prepare ferrite materials, so that the performance of ferrite materials has been greatly improved and improved. Due to the specific surface effect, small size effect, interface effect and macroscopic quantum effect of nanomaterials, they exhibit different physical properties such as light, electricity, heat, and magnetism from conventio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/26C04B35/626
Inventor 李峰顾智军项顼
Owner BEIJING UNIV OF CHEM TECH
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