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Solvothermal synthesis method of nickel cobaltate nano particles

A nanoparticle and synthesis method technology, applied in cobalt compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of poor dispersion, difficult dispersion, uneven particle distribution, etc., and achieve difficult agglomeration, uniform size, high The effect of dispersion

Inactive Publication Date: 2011-01-19
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Mechanochemical synthesis introduces a lot of strain and defects during the ball milling process, and the product has high surface activity, but the particle distribution is uneven and the dispersion is not good
The liquid-phase chemical precipitation method mainly includes two steps of chemical co-precipitation to prepare precursors and roasting and decomposition of the precursors. The process of crystal nucleation and growth is separated, which can refine the crystal grains, but the structure of the product is incomplete, and some metastable phase formation
The sol-gel method can obtain particles with small particle size and uniform distribution by adding a surface dispersant, but it is easy to introduce impurities and the phase purity is not high
The hydrothermal method is simple to operate, has the advantages of being environmentally friendly, low temperature, directly obtaining the product in solution without calcination, and low cost. However, the current hydrothermal method to obtain nickel cobaltate nanoparticles is generally only carried out in aqueous solution, and the agglomeration phenomenon is serious. Difficult to disperse

Method used

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  • Solvothermal synthesis method of nickel cobaltate nano particles
  • Solvothermal synthesis method of nickel cobaltate nano particles

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Experimental program
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Effect test

Embodiment 1

[0021] Mix 2ml 0.5mol / L nickel acetate and 4ml 0.5mol / L cobalt acetate solution, add it to 10ml n-propanol, then add 28% (weight) concentrated ammonia water to adjust pH=9, and the solvent will be at 220℃ After 6h of thermal reaction, nickel cobaltate nanoparticles can be obtained. Such as figure 1 As shown in the middle curve 1, all the diffraction peaks can correspond to the standard spinel peaks at the bottom. It can be seen that the obtained nickel cobaltate particles are cubic phase pure spinel structure, according to the Scherer formula D=κ ·Λ / βcosθ,κ is the Scherrer constant, generally taken as 0.89; λ is the X-ray wavelength, which is 0.154056nm in this embodiment; β is the half-width of the diffraction peak, that is, half the height from the top to the bottom of the peak The width of the place is measured and converted into radians; θ is the diffraction angle. It can be estimated that the grain size D is about 10 nm. Since the particle size of the material is smalle...

Embodiment 2

[0023] Mix 2ml 0.5mol / L nickel acetate and 2ml 1.0mol / L cobalt acetate solution, add them to 12ml n-butanol, then add 28% concentrated ammonia to adjust pH=9, and solvothermally react at 220℃ for 6h , You can get nickel cobaltate nanoparticles. Such as figure 1 As shown in the middle curve 2, all diffraction peaks can correspond to the standard spinel peaks at the bottom. It can be seen that the obtained nickel cobalt oxide particles are cubic phase pure spinel structure. According to the Scherer formula, the crystal structure can be estimated. The particle size is about 11 nm.

Embodiment 3

[0025] Mix 2ml 1.0mol / L nickel acetate and 4ml 1.0mol / L cobalt acetate solution, add it to 10ml n-propanol, add 20% concentrated ammonia to adjust pH=10, and solvothermally react at 200℃ for 24h , You can get nickel cobaltate nanoparticles. Such as figure 1 As shown in the middle curve 3, all diffraction peaks can correspond to the standard spinel peaks at the bottom. It can be seen that the obtained nickel cobaltate particles are cubic phase pure spinel structure, and the crystal structure can be estimated according to the Scherer formula. The particle size is about 10 nm. figure 2 It is a transmission electron micrograph of the prepared nickel cobaltate nanoparticles (JEOL 2010 high-resolution transmission electron microscope scanner, 100kV). Such as figure 2 As shown, the nickel cobaltate nanoparticles obtained in this embodiment are relatively uniform, have a narrow particle size distribution, basically about 10 nm, and have good dispersibility.

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Abstract

The invention discloses a solvothermal synthesis method of nickel cobaltate nano particles, which comprises the steps of mixing aqueous solutions of nickel acetate with the concentration of 0.5-2 mol / L and cobalt acetate with the concentration of 0.5-2 mol / L, wherein the mol ratio of nickel acetate and cobalt acetate is 1:2; adding normal butanol or normal propyl alcohol as an organic solvent; leading the volume ratio of water and the organic solvent to be 0.5-2:1; adding aqua ammonia and stirring till even mix; adjusting the pH of the solution to be 9-10; and carrying out solvothermal reaction for 6-72h at the temperature of 180-220 DEG C. The method has simple operation, environmental friendliness and low temperature, and can directly obtain products from the solution without calcination; the obtained nickel cobaltate particles have high purity, even size, narrow particle size distribution and good dispersivity, are spinelle-type cubic phase nano particles, and can be used without further superficial treatment; and the size of the particles is smaller than 12nm.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a solvothermal synthesis method of nickel cobaltate nanoparticles. Background technique [0002] Nickel cobalt oxide (NiCo 2 o 4 ) is AB with spinel structure 2 o 4 type composite oxides. Due to its structural characteristics, it can be used as a magnetic material to manufacture electronic components and as a wave-absorbing material. In a reducing atmosphere, obvious Co 2+ and oxygen vacancies, therefore, in the petroleum industry NiCo 2 o 4 It can be used as a catalyst with deep oxidation activity, has high catalytic activity for oxygen precipitation, and can be used as an excellent catalytic material for reducing oxygen evolution potential, improving electrode stability, and reducing energy consumption and cost. Relevant studies have also found that the composite oxide nickel cobaltate can replace precious metals platinum, rhodium and p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/00
Inventor 田俐吴明娒扶雄辉
Owner SUN YAT SEN UNIV