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Preparation method and use of spherical ferric oxide nanoparticles with controllable size

A ferric tetroxide and nanoparticle technology, which is applied in ferrous oxides, ferric oxide/ferric hydroxide, electrochemical generators, etc., can solve the complex system and does not involve the regulation of spherical ferric tetroxide particle size. and other problems, to achieve the effect of uniform size distribution, controllable particle size and uniform morphology.

Inactive Publication Date: 2016-08-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the systems used in the above-mentioned preparation methods are relatively complex, and have certain requirements on the valence state of the iron salt, and at the same time, it does not involve the regulation of the particle size of spherical ferric ferric oxide

Method used

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  • Preparation method and use of spherical ferric oxide nanoparticles with controllable size
  • Preparation method and use of spherical ferric oxide nanoparticles with controllable size
  • Preparation method and use of spherical ferric oxide nanoparticles with controllable size

Examples

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Effect test

Embodiment 1

[0030] Weigh 0.8 g FeCl 3 ·6H 2 O and 1.6 g sodium oleate (C 17h 33 COONa) was dissolved in 30 mL of ethylene glycol, and magnetically stirred at room temperature for 2 hours to form a uniformly mixed orange-yellow solution; the mixed solution was added to a 50 mL polytetrafluoroethylene-lined reactor and sealed, and the reactor was placed in Constant temperature blast drying oven, 200 o C was kept warm for 24 hours; after the reaction kettle was naturally cooled to room temperature, the product was ultrasonically cleaned several times with absolute ethanol, and then placed in a vacuum oven for 80 o C drying to obtain black magnetic powder. The ferroferric oxide obtained under this condition is a spherical particle with a diameter of about 200 nm and a uniform particle size distribution.

[0031] Such as Figure 4 As shown, the ferric oxide nanocrystals prepared by the present invention have excellent cycle performance, and its specific capacity can still be stabilized a...

Embodiment 2

[0033] Weigh 0.8g FeCl 3 ·6H 2 O and 1.2 g sodium oleate (C 17 h 33 COONa) was dissolved in 30 mL of ethylene glycol, and magnetically stirred at room temperature for 2 hours to form a uniformly mixed orange-yellow solution; the mixed solution was added to a 50 mL polytetrafluoroethylene-lined reactor and sealed, and the reactor was placed in Constant temperature blast drying oven, 200 o C was kept warm for 24 hours; after the reaction kettle was naturally cooled to room temperature, the product was ultrasonically cleaned several times with absolute ethanol, and then placed in a vacuum oven for 80 o C drying to obtain black magnetic powder. The ferroferric oxide obtained under this condition is a spherical particle with a diameter of about 500 nm and a uniform particle size distribution.

Embodiment 3

[0035] Weigh 0.8 g FeCl 3 ·6H 2 O and 4.6 g sodium oleate (C 17 h 33 COONa) was dissolved in 30 mL of ethylene glycol, and magnetically stirred at room temperature for 2 hours to form a uniformly mixed orange-yellow solution; the mixed solution was added to a 50 mL polytetrafluoroethylene-lined reactor and sealed, and the reactor was placed in Constant temperature blast drying oven, 200 o C was kept warm for 24 hours; after the reaction kettle was naturally cooled to room temperature, the product was ultrasonically cleaned several times with absolute ethanol, and then placed in a vacuum oven for 80 o C drying to obtain black magnetic powder. The Fe3O4 obtained under this condition did not form a spherical structure, but was loose primary particles with a diameter of about 20 nm and a wide particle size distribution.

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Abstract

The invention discloses a preparation method of spherical ferriferrous oxide nano particles with controllable size, which is characterized in that sodium oleate is taken as a synthesis auxiliary agent and a surfactant, a hydrothermal method is used for one-step preparation in a glycol system. The method comprises the following steps: dissolving soluble ferric salt and a certain amount of sodium oleate in glycol, stirring for more than 2 hours; then sealing the mixed liquor in a polytetrafluoroethylene lined high-pressure reaction vessel, cooling and then centrifuging and washing to obtain the spherical ferriferrous oxide nano particles. According to the invention, the technology is more reliable and has the advantage of high repeatability, only sodium oleate used in a system is taken as a reaction auxiliary agent, and the particle size of the spherical ferriferrous oxide can be regulated and controlled by adjusting the addition of sodium oleate. The prepared ferriferrous oxide has a grading structure, the process is easily controlled and realized, and the preparation method has the advantage of friendly environment. The prepared spherical particles of ferriferrous oxide can be used as a lithium ion battery cathode material, the experiment shows that the spherical particles have excellent cycle performance and good application prospect.

Description

technical field [0001] The invention belongs to the field of preparation of nanometer metal oxide functional materials, and in particular relates to a preparation method of size-controllable spherical iron ferric oxide nanoparticles. Background technique [0002] Lithium-ion batteries are widely used in electronic products and electric vehicles due to their high voltage and energy density. Lithium-ion batteries are mainly composed of positive electrode, diaphragm, negative electrode and electrolyte. The current main commercial negative electrode material is graphite, but graphite material is due to its low specific capacity (372 mAhg -1 ), has become a factor limiting the energy density of lithium-ion batteries, so the development of a higher-capacity lithium-ion battery anode material has become a current research hotspot. Due to the high theoretical capacity of transition metal oxides (generally greater than 600 mAhg -1 ), higher safety, and no pollution have become an e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/1391H01M4/131C01G49/08
CPCC01G49/08H01M4/52H01M10/0525Y02E60/10
Inventor 王智宇任志敏钱国栋樊先平
Owner ZHEJIANG UNIV