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Ferroferric oxide rhombic dodecahedron particles and preparation method thereof

A rhombic dodecahedron, ferric tetroxide technology, applied in the direction of iron oxide/iron hydroxide, ferrous oxide, inorganic material magnetism, etc. Activity and magnetic recycling, uniform size distribution, good superparamagnetic effect

Inactive Publication Date: 2014-05-07
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the lack of technology for preparing ferric ferric oxide rhombohedral particles in the prior art and the deficiency that rhombohedral dodecahedron disappears easily in the synthesis process, the present invention provides A method for preparing superparamagnetic ferric iron tetraoxide rhombohedral dodecahedron by solvothermal method and the obtained product

Method used

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  • Ferroferric oxide rhombic dodecahedron particles and preparation method thereof
  • Ferroferric oxide rhombic dodecahedron particles and preparation method thereof
  • Ferroferric oxide rhombic dodecahedron particles and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 1.1 Dissolve 0.162 g of ferric chloride (anhydrous), 0.127 g of ferrous chloride (anhydrous) and 0.067 g of polyvinylpyrrolidone in 10 mL of DMF, and stir for 20 minutes.

[0035] 1.2 Mix 9 mL of DMF and 1.5 mL of 80wt% hydrazine hydrate, then slowly add the mixture dropwise to the solution described in Example 1.1 at a dropping rate of 0.2 mL / min, and stir for 40 minutes.

[0036] 1.3 Seal the mixed solution described in Example 1.2 in a high-pressure reactor and keep it warm at 200°C for 20 hours. After the reaction, cool it down to room temperature naturally. The product after the reaction is black and can be collected by magnetic separation (such as with a magnet). , indicating that the product has strong magnetic properties and is ferric oxide. The product after separation is washed 3 times with water and ethanol to obtain ferric oxide particles, which are scanned by an electron microscope, and the obtained scanning electron microscope photos are as follows: figu...

Embodiment 2

[0039] 2.1 Dissolve 0.162 g of ferric chloride (anhydrous), 0.127 g of ferrous chloride (anhydrous) and 0.067 g of polyvinylpyrrolidone in 10 mL of DMF and stir for 20 minutes.

[0040] 2.2 Add solution B (1.5 mL hydrazine hydrate diluted with 8 mL DMF) dropwise to the solution described in Example 2.1 at a rate of 1 mL / min, and stir for 60 minutes.

[0041] 2.3 Seal the mixed solution described in Example 2.2 in a high-pressure reactor, and keep it warm at 200° C. for 20 hours. After the reaction, cool down to room temperature naturally, and collect a black product by magnetic separation. After washing with water and ethanol for 3 times, magnetic ferric ferric oxide rhombohedral particles were obtained. image 3 , Rhombic dodecahedral morphology standard, smooth surface, rhombus side length 200-400nm.

Embodiment 3

[0043]3.1 Dissolve 0.162 g of ferric chloride (anhydrous), 0.127 g of ferrous chloride (anhydrous) and 0.13 g of polyvinylpyrrolidone in 10 mL of DMF, and stir for 20 minutes.

[0044] 3.2 Slowly add solution B (1.5 mL hydrazine hydrate diluted with 10 mL DMF) dropwise to the solution described in Example 3.1 at a rate of 0.2 mL / min, and stir for 30 minutes.

[0045] 3.3 Seal the mixed solution described in Example 3.2 in a high-pressure reactor, and keep it warm at 200°C for 20 hours. After the reaction, cool it down to room temperature naturally, and collect the black product by magnetic separation. After washing with water and ethanol for 3 times, magnetic ferric ferric oxide rhombohedral particles were obtained. Figure 4 , Rhombic dodecahedral morphology standard, smooth surface, rhombus side length 200-400nm.

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Abstract

The invention discloses ferroferric oxide rhombic dodecahedron particles and a preparation method thereof. The preparation method comprises the following steps: adding a pyrrolidone stabilizing agent and an iron source to an organic solvent, uniformly stirring, then adding a hydrazine hydrate-containing N,N-dimethyl formamide (DMF) solution, and stirring so as to obtain a precursor solution; carrying out heat preservation on the precursor solution at the temperature of 140-240 DEG C for growing magnetic ferroferric oxide rhombic dodecahedron particles; and carrying out aftertreatment on the solution so as to obtain the magnetic ferroferric oxide rhombic dodecahedron particles. The preparation method has the advantages that the ferroferric oxide rhombic dodecahedron particles which are difficult to synthesize at present and have exposed surfaces with high surface energy are prepared by using a solvothermal method, the preparation process is simple to operate, the inert gas shielding is not needed, the preparation method is good in repeatability and easy to control, and the ferroferric oxide particles are regular and intact in shape and uniform in size distribution, have smooth particle surfaces, also have superstrong magnetism, very good superparamagnetism and enormous potential application in terms of catalytic activity improvement and magnetism recycling.

Description

technical field [0001] The present invention relates to a preparation method of rhombic dodecahedral particles, which is a new shape of ferric iron tetroxide, in particular to a method for preparing superparamagnetic ferric ferric oxide rhombohedral dodecahedral particles by solvothermal method and the obtained product The invention belongs to the technical field of magnetic material preparation. Background technique [0002] Due to the potential applications of magnetic ferroferric oxide particles with different morphologies in magnetic fluids, drug loading, medical diagnosis, data storage, catalysis, etc., rational and precise control of the morphology of ferroferric oxide particles has always been a research hotspot. . So far, scientists have successfully synthesized a series of ferric oxide particles with different shapes, the main shapes include irregular particles, cubes, wires, tubes, rods, sheets, rings, octahedrons, etc. But there is no report about the preparat...

Claims

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Application Information

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IPC IPC(8): C01G49/08H01F1/11
Inventor 杨萍赵杰王丹王俊鹏
Owner UNIV OF JINAN
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