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Method for preparing iron oxide particles having controllable morphology and size

A technology of iron oxide particles and size, applied in the field of preparation of iron oxide particles, can solve the problems of inability to realize the regulation of particle size and morphology, inability to regulate particle size and morphology, and no very successful examples, and achieve good results. The effect of biocompatibility, low production cost and high yield

Inactive Publication Date: 2018-01-26
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composition and appearance of the particles obtained in the above patents are consistent. To change the particle size, appearance and composition, different synthesis methods are required to synthesize iron oxide nanomaterials with different appearances, but none of them can realize the adjustment of particle size and appearance. control
[0006] Patent CN102659191 B reports a method for controlling the morphology and properties of ferric oxide. By adjusting the molar ratio of ferric chloride hexahydrate and urea, different temperatures and reaction times, the shape of spherical, microporous and hollow structures is realized. appearance control, but the urea used in this method will decompose and generate a large amount of ammonia gas during the solvothermal process, which will cause the pressure in the reactor to be too high and damage the reaction device, and the change of urea amount is not sensitive to the appearance control; patent CN103058283 A is disclosed A method of regulating the morphology of iron ferric oxide particles by controlling the dosage relationship between iron salt and sodium bicarbonate, and controlling the particle size by adjusting the dosage ratio of organic solvents and organic amines and heat treatment conditions, etc., this method also has regulation The mechanism is complex and the regulation is not sensitive, and efficient regulation cannot be achieved
[0007] To sum up, most current synthesis methods of magnetic nanoparticles cannot control the size and shape of the particles in a simple and efficient way, and there are relatively few studies on this problem, and there are no very successful examples so far.

Method used

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  • Method for preparing iron oxide particles having controllable morphology and size
  • Method for preparing iron oxide particles having controllable morphology and size
  • Method for preparing iron oxide particles having controllable morphology and size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Add 40mL of ethylene glycol into a 200mL beaker, start stirring, add 0.5g of dodecylbenzenesulfonic acid and 1.0g of polyvinyl alcohol (M.W.18000), and stir for 12h;

[0031] (2) Add 2.5g ferric chloride hexahydrate FeCl 3 ·6H 2 O and 0.35g sodium hydroxide, stirred for 4h;

[0032] (3) Transfer the above 40mL solution into a hydrothermal reaction kettle, and react at 190°C for 36h;

[0033] (4) After the reaction, the precipitate was separated by centrifugation, washed three times with ethanol and deionized water, and vacuum-dried at 50° C. to obtain magnetic ferric oxide nanoparticles. It can be seen from TEM characterization that the particle diameter is at ~ 20nm, the particle size distribution is uniform, and the monodispersity is good; the particle morphology is nanoparticle; XRD characterization shows that the particle is ferric oxide with high crystallinity; the product yield is ~ 87%.

Embodiment 2

[0035] Add 40mL of ethylene glycol into a 200mL beaker, start stirring, add 0.5g of dodecylbenzenesulfonic acid and 1.0g of polyvinyl alcohol (M.W.18000), and stir for 12h;

[0036] (2) Add 2.5g ferric chloride hexahydrate FeCl 3 ·6H 2 O and 1.35g sodium hydroxide, stirred for 4h;

[0037] (3) Transfer the above 40mL solution into a hydrothermal reaction kettle, and react at 190°C for 36h;

[0038] (4) After the reaction, the precipitate was separated by centrifugation, washed three times with ethanol and deionized water, and vacuum-dried at 50° C. to obtain magnetic ferric oxide nanoparticles. It can be seen from the TEM characterization that the particle diameter is at ~ 200nm, the particle size distribution is uniform, and the monodispersity is good; the particle morphology is a nano-cluster; the XRD characterization shows that the particle is ferric oxide with high crystallinity; the product yield is ~85%.

Embodiment 3

[0040] (1) Add 40mL of ethylene glycol and 20mL of diethylene glycol into a 200mL beaker, start stirring, add 0.5g of dodecylbenzenesulfonic acid and 1.0g of polyvinyl alcohol (M.W.18000), and stir for 12h;

[0041] (2) Add 2.5g ferric chloride hexahydrate FeCl 3 ·6H 2 O and 2.42g sodium hydroxide, stirred for 4h;

[0042] (3) Transfer the above 40mL solution into a hydrothermal reaction kettle, and react at 200°C for 36h;

[0043] (4) After the reaction, the precipitate was separated by centrifugation, washed three times with ethanol and deionized water, and vacuum-dried at 50° C. to obtain magnetic ferric oxide nanoparticles. The particle size distribution is uniform, the monodispersity is good, and the particle shape is regular octahedron; the product yield is ~88%.

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Abstract

The invention relates to a method for preparing iron oxide particles having controllable morphology and size. The method comprises the following steps: 1, adding a surfactant into an organic solvent,fully stirring the surfactant and the organic solvent to obtain a uniformly dispersed suspension, adding an inorganic alkali and a soluble iron salt into the suspension, and fully stirring the inorganic alkali, the soluble iron salt and the suspension until the inorganic alkali and the soluble iron salt are completely dissolved; 2, pouring a solution prepared in step 1 into a closed heating container, and carrying out a thermal reaction; and 3, separating a precipitate in the obtained reaction solution through a centrifuging or magnet process, repeatedly washing the precipitate with ethanol and deionized water, and carrying out vacuum drying to obtain a black solid which is the final product. The accurate and highly-efficient regulation of the size and the morphology of nano-particles is realized through adjusting the proportion of the reaction solvent and the addition amount of the inorganic alkali under same reaction conditions, the size of the obtained particles is 20-400 nm, and solid particles, nano-clusters, triangular prisms, regular octahedrons and other various morphologies can be obtained. The preparation method has the advantages of simplicity, and green and environmentally-friendly raw materials and technology, the product has the advantages of high crystallinity, stable structure, uniform size and gram level reaching yield, and the preparation method is of great guidance significance to preparing magnetic nano-particles.

Description

technical field [0001] The patent of the invention belongs to the technical field of metal oxide nanomaterial preparation technology, specifically a preparation method of iron oxide particles with controllable shape and size. Background technique [0002] In recent years, with the continuous development of nanoscience and technology, the research and application fields of magnetic nanomaterials have been greatly expanded. As a very representative class of magnetic nanomaterials, ferroferric oxide nanoparticles are very significantly different from bulk materials with the same composition in terms of macroscopic and microscopic properties, such as particle surface atoms The proportion increases, showing many special properties such as interface effect, small size effect, quantum size effect and macroscopic quantum tunneling effect, which has attracted the attention of many materials and physics researchers at home and abroad, and has been widely used in catalysis, magnetic fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82Y40/00
Inventor 赵凌云谢文升高飞高琴郭振虎王丹
Owner TSINGHUA UNIV
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