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Method for preparing transition nanometer oxide with uniform grain size by coprecipitation method

A technology of nano-oxide and co-precipitation method, applied in the field of preparation of inorganic nano-compounds, can solve the problems of poor crystallinity, large particle size distribution of products, uneven product morphology, etc., and achieve narrow particle size distribution, perfect shape, good biocompatibility

Inactive Publication Date: 2014-03-19
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of large product particle size distribution, uneven product appearance and poor crystallinity in the prior art, the present invention proposes an improved co-precipitation method, specifically by precisely controlling various reaction parameters, so that various reactions Conditions, ligand types and quantities work together to achieve the technical effects of uniform particle growth, uniform particle size, controllable morphology, and high crystallinity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get 2 moles of ferrous chloride and 4 moles of ferric chloride, mix and add 400ml of water and 200ml of pyrrolidone mixed solution to dissolve. Add complex ligand 4 moles of sodium citrate, 4 moles of glycerin, 4 moles of glycine, 4 moles of mercaptoethanol, mix well, add ammonia water for precipitation, stir at high speed during the precipitation process, control the temperature at 40°C, and control the pH at 8.5-8.6 , and centrifuged after the precipitation was complete. The product precipitate is dispersed in water, the weight ratio is product: water = 1:10, and the mixed liquid is heated to 120-130°C in a sealed kettle to react for 30-60min, cooled and filtered to obtain the product. The product was detected by XRD to be ferric oxide nanoparticles. For the average particle size, 200 particles in the same area in the TEM photo were selected for counting, the average particle size was 23 nm, and the standard deviation / average particle size was 3%. The vibrating hyst...

Embodiment 2

[0026] Take 6 moles of ferric chloride, mix and add 400ml of water and 400ml of pyrrolidone mixture to dissolve. Add complex ligands 6 moles of sodium citrate, 4 moles of glycine, and 6 moles of mercaptoethanol. After mixing evenly, add ammonia water for precipitation. During the precipitation process, stir at high speed, control the temperature at 45°C, and control the pH at 8.5-8.6. After the precipitation is complete, centrifuge separate. The product precipitate is dispersed in water, the weight ratio is product: water = 1:10, and the mixed liquid is heated to 120-130°C in a sealed kettle to react for 30-60min, cooled and filtered to obtain the product. The product was detected by XRD to be ferric oxide nanoparticles. For the average particle size, 200 particles in the same area in the TEM photo were selected for counting, the average particle size was 25 nm, and the standard deviation / average particle size was 4%. It is detected by a hysteresis loop instrument and is sup...

Embodiment 3

[0028] Take 2 moles of cobalt dichloride and 4 moles of ferric chloride, mix and add 400ml of water and 200ml of pyrrolidone mixed solution to dissolve. Add complex ligand 4 moles of sodium citrate, 4 moles of glycerin, 4 moles of glycine, 4 moles of mercaptoethanol, mix well, add ammonia water for precipitation, stir at high speed during the precipitation process, control the temperature at 40°C, and control the pH at 8.5-8.6 , and centrifuged after the precipitation was complete. The product precipitate is dispersed in water, the weight ratio is product: water = 1:10, and the mixed liquid is heated to 120-130°C in a sealed kettle to react for 30-60min, cooled and filtered to obtain the product. The product was detected as CoFe by XRD 2 o 4 nanoparticles. For the average particle size, 200 particles in the same area in the TEM photo were selected for counting, the average particle size was 25 nm, and the standard deviation / average particle size was 3%.

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Abstract

The invention discloses a method for preparing a transition nanometer oxide with a uniform grain size by a coprecipitation method. The method comprises the steps of selecting a soluble metal salt as a raw material; dissolving in a water-organic mixed solvent phase; adding a composite ligand, and then adding a precipitator to carry out coprecipitation reaction; simultaneously controlling the pH value within a range of 7-9 at any time; filtering to obtain a sediment product. Various reaction conditions and ligand variety and quantity are synergistic, so as to achieve the technical effects of uniform growth, uniform particle size, controllable morphology and high crystallinity of particles by using the composite ligand and accurately controlling a plurality of reaction parameters. The obtained oxide nanoparticles have narrower particle size distribution and higher crystallinity, and are applicable to the fields such as biomedicine detection and the like.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, relates to a preparation method of an inorganic nanometer compound, and is suitable for fields including biomedical detection and the like. Background technique [0002] The precipitation method is usually to mix substances with different chemical compositions in a solution state, add an appropriate precipitant to the mixed solution to prepare a precursor precipitate, and then dry or calcinate the precipitate to obtain the corresponding powder particles. [0003] The co-precipitation method refers to the solution containing two or more cations, which exist in the solution in a homogeneous phase, adding a precipitant, and after a precipitation reaction, a uniform precipitation of various components can be obtained. It is a preparation containing two Or an important method of composite oxide ultrafine powder of two or more metal elements. [0004] The co-precipitation method is to add a suitable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/36C01G49/06C01G49/08C01G51/00B82Y30/00
Inventor 董彬孙长艳常志东李文军周花蕾刘世香
Owner UNIV OF SCI & TECH BEIJING
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