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Direct synthesis method of nanometer oxide powder

A technology of nano-scale oxides and nano-powders, which is applied in the preparation of ferrous oxides, titanium oxide/hydroxides, oxides/hydroxides, etc., can solve the problem of high decomposition temperature and particle size of nano-powders Large size, expensive equipment, etc., to achieve the effect of uniform particle size, narrow particle distribution, and avoid grain growth and agglomeration

Inactive Publication Date: 2010-08-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage of this method is that the process is simple and easy to control, but the equipment is expensive, the decomposition temperature is high, and the particle size of the nano-powder is large.

Method used

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  • Direct synthesis method of nanometer oxide powder
  • Direct synthesis method of nanometer oxide powder
  • Direct synthesis method of nanometer oxide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Disperse and dissolve 68 g of tetrabutyl titanate into 500 ml of absolute ethanol by stirring to obtain liquid A. 63.1 g of Ba(OH) 2 ·8H 2 O was dispersed and dissolved in 500 ml of 60°C water by stirring to obtain liquid B. Slowly add 2 grams of dodecyl alcohol and liquid A into liquid B while stirring. After the dropwise addition was completed, the solid and liquid were separated. Dry the solid part at 20-100°C to directly obtain BaTiO 3 nanoparticles. XRD shows that the obtained powder is BaTiO with perovskite structure 3 Micronized. SEM showed that the micropowder was nearly spherical crystalline particles with a uniform size and a particle diameter of ~50 nm.

Embodiment 2

[0031] Dispersed and dissolved 34 g of tetrabutyl titanate into 50 ml of n-butanol to obtain liquid A. 31.6 g Ba(OH) 2 ·8H 2 O was added to a ball mill jar with a volume of 250 milliliters, and 100 milliliters of n-butanol was used as a dispersant, and ball milled at a speed of 200 rpm for 4 hours to obtain liquid B. Add liquid A into the ball mill tank containing liquid B, and add 1 gram of dodecyl alcohol as a surfactant at the same time, and ball mill at a speed of 200 rpm for 4 hours. After ball milling, ventilate and dry at room temperature to directly obtain BaTiO 3 nanoparticles. XRD shows that the obtained powder is BaTiO with perovskite structure 3 Micronized. SEM showed that the micropowder was nearly spherical crystalline particles with a uniform size and a particle diameter of ~10 nm.

Embodiment 3

[0033] 29.1 g Co(NO 3 ) 2 ·6H 2 O and 80.8 g Fe(NO 3 ) 3 9H 2 O was dispersed in 100 ml of absolute ethanol to obtain liquid A. Add 32 grams of NaOH into a ball milling jar with a capacity of 250 milliliters, use 100 milliliters of absolute ethanol dispersant, and ball mill at a speed of 200 rpm for 4 hours to obtain liquid B. Add liquid A into the ball mill tank containing liquid B, and add 1 gram of dodecyl alcohol as a surfactant at the same time, and ball mill at a speed of 200 rpm for 4 hours. After ball milling, wash repeatedly with water for 5 times, and then dry at 20-100°C to directly obtain CoFe 2 o 4 nanoparticles. XRD shows that the obtained powder is CoFe with cubic structure 2 o 4 Micronized. SEM showed that the micropowder was nearly spherical crystalline particles with a uniform size and a particle diameter of ~5 nm.

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Abstract

The invention relates to a synthesis method of nanometer oxide powder, which belongs to the technical field of ultra fine powder preparation. The method comprises the following steps: respectively adding acid substances and alkaline substances into proper dispersing agents and surface active agents; carrying out mixing reaction again on two mixtures under a certain mixing condition at the proper temperature after being uniformly dispersed under a certain dispersing condition; and thus, directly synthesizing the required oxide nanometer powder. The synthesis method does not need high-temperature calcination, and inhibits the generation of the glomeration and the excessive growth of crystal grains, and the oxide powder with the grain diameter between 5 and 100 nm, uniform grain granular size, narrow grain distribution and uniform and stable ingredient can be directly prepared from the solution. The powder prepared by the synthesis method has high chemical activity and wide application range.

Description

technical field [0001] The invention relates to the preparation technology of ultrafine nano-powder, in particular to a synthesis method of nano-scale oxide powder. Background technique [0002] The particle size of nanoparticles is extremely small, but the specific surface area is extremely large, so they exhibit new optical, electrical, magnetic and chemical properties. At present, new materials composed of nanoparticles have been widely used in the fields of catalysis, luminescent materials, magnetic materials, semiconductor materials and fine ceramic materials. Nano-oxides are an important class of materials, and the research on their preparation methods has broad prospects. [0003] According to the material state, the preparation of nano oxides can be divided into solid phase method, precipitation method, sol-gel method, hydrothermal method, evaporation-condensation method and gas phase reaction method. [0004] Because the solid-phase method is based on the principl...

Claims

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Application Information

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IPC IPC(8): C01B13/14C01G23/00C01G51/00C01G25/02C01G49/00C01G53/00C01G49/08C01G23/053
Inventor 齐建全孙黎马振伟彭韬刘佰博李龙土
Owner TSINGHUA UNIV
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