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Pure iron based surface Fe3O4 nano-column array and preparation method thereof

A nano-column array, fe3o4 technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of difficult control of product shape and size, high decomposition temperature, environmental pollution, etc., to achieve The production efficiency is environmentally friendly, the composition is uniform, and the process parameters are precise and controllable.

Inactive Publication Date: 2014-10-29
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Each of these methods has advantages and disadvantages: the co-precipitation method has the advantages of mild reaction conditions and simple equipment, but the shape and size of the prepared product are difficult to control; although the thermal decomposition method has great advantages in controlling the crystal shape, shape and size of the product However, the precursors used in this method are often highly toxic metal-organic compounds, such as Fe(CO)5, Fe(cup)2, Fe( acac)2, etc., and the decomposition temperature of metal-organic compounds is very high; although the microemulsion method can well control the size, particle size distribution and morphology of nanoparticles, this method requires the use of a large amount of organic matter , easy to cause environmental pollution

Method used

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  • Pure iron based surface Fe3O4 nano-column array and preparation method thereof

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Experimental program
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Embodiment 1

[0021] A pure iron-based surface Fe 3 o 4 Nanopillar arrays and methods of making them. The pure iron after surface pretreatment is anodized in the ammonium fluoride-water-ethylene glycol system electrolyte; take it out, clean it, and blow it dry. Then, in a hydrogen atmosphere, the temperature was raised from room temperature to 400-600 °C at a rate of 5-8 °C / min, kept for 3-5 hours, and naturally cooled with the furnace to obtain pure iron-based surface Fe. 3 o 4 array of nanopillars.

[0022] The technical parameters of the anodizing treatment are: the voltage of the anodizing treatment is 20-30V, the temperature of the anodizing treatment is 45-60°C, and the time of the anodizing treatment is 0.05-0.5h.

[0023] The mass fraction of ammonium fluoride in the ammonium fluoride-water-ethylene glycol system electrolyte is 0.2-0.35%, and the volume fraction of water is 1.5-2%.

[0024] The pure iron-based surface Fe obtained in this embodiment 3 o 4 The layer thickness o...

Embodiment 2

[0026] A pure iron-based surface Fe 3 o 4 Nanopillar arrays and methods of making them. The pure iron after surface pretreatment is anodized in the ammonium fluoride-water-ethylene glycol system electrolyte; take it out, clean it, and blow it dry. Then, in a hydrogen atmosphere, the temperature was raised from room temperature to 550-700 °C at a rate of 8-12 °C / min, kept for 4-7 hours, and naturally cooled with the furnace to obtain pure iron-based surface Fe. 3 o 4 array of nanopillars.

[0027] The technical parameters of the anodizing treatment are: the voltage of the anodizing treatment is 30-45V, the temperature of the anodizing treatment is 35-50°C, and the time of the anodizing treatment is 0.1-0.8h.

[0028] The mass fraction of ammonium fluoride in the ammonium fluoride-water-ethylene glycol system electrolyte is 0.3-0.45%, and the volume fraction of water is 2.0-2.5%.

[0029] The pure iron-based surface Fe obtained in this embodiment 3 o 4 The layer thickness...

Embodiment 3

[0031] A pure iron-based surface Fe 3 o 4 Nanopillar arrays and methods of making them. The pure iron after surface pretreatment is anodized in the ammonium fluoride-water-ethylene glycol system electrolyte; take it out, clean it, and blow it dry. Then, in a hydrogen atmosphere, the temperature was raised from room temperature to 600-800°C at a heating rate of 12-15°C / min, kept for 6-8 hours, and cooled naturally with the furnace to obtain pure iron-based surface Fe. 3 o 4 array of nanopillars.

[0032]The technical parameters of the anodizing treatment are: the voltage of the anodizing treatment is 45-60V, the temperature of the anodizing treatment is 20-40°C, and the time of the anodizing treatment is 0.5-1.0h.

[0033] The mass fraction of ammonium fluoride in the ammonium fluoride-water-ethylene glycol system electrolyte is 0.4-0.5%, and the volume fraction of water is 2.5-3.0%.

[0034] The pure iron-based surface Fe obtained in this embodiment 3 o 4 The layer thic...

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Abstract

The invention particularly relates to a pure iron based surface Fe3O4 nano-column array and a preparation method thereof. The technical scheme of the invention is as follows: the method comprises the steps: carrying out anodic oxidation treatment on pure iron, which is subjected to surface pretreatment, in an ammonium fluoride-water-ethanediol system electrolyte; taking out, cleaning and drying through blowing; heating to the temperature of 400-800 DEG C from room temperature in a hydrogen atmosphere at the heating rate of 5-15 degrees centigrade per minute, carrying out heat preservation for 3-8 hours, and carrying out furnace cooling naturally, thereby preparing the pure iron based surface Fe3O4 nano-column array. The method is characterized in that in the ammonium fluoride-water-ethanediol system electrolyte, the mass percentage of ammonium fluoride is 0.2-0.5%, and the volume percentage of water is 1.5-3%; the anodic oxidation treatment is carried out under the conditions that the voltage is 20-60 voltage, the temperature is 20-60 DEG C and the time is 0.05-1 hour. The preparation method has the characteristics of simple process, environmental friendliness and low cost; the prepared pure iron based surface Fe3O4 nano-column array has the advantages that the structure is regular and orderly, the composition is uniform, the density of nano-columns is high, the specific surface area is large, the bonding with substrates is tight, and other impurity elements are not involved.

Description

technical field [0001] The invention belongs to Fe 3 o 4 The technical field of nanopillar arrays. Specifically related to a pure iron-based surface Fe 3 o 4 Nanopillar arrays and methods of making them. Background technique [0002] There are three types of iron oxides: ferrous oxide, ferric oxide and ferric oxide. The chemical formula of ferric oxide is Fe 3 o 4 . X-ray diffraction experiments showed that Fe 3 o 4 It has a trans-spinel structure, and there is no metaferrate ion in the crystal. In addition, Fe 3 o 4 is still a conductor, because in ferromagnetic ore due to Fe 2+ with Fe 3+ The octahedral position is basically disordered, and electrons can be transferred rapidly between the two oxidation states of iron. Fe 3 o 4 The basic physical properties are: crystalline black solid, insoluble in water, magnetic, and solid with excellent electrical conductivity. Fe 3 o 4 The basic chemical properties of iron are: oxidizing and reducing, when heated at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/34B82Y30/00B82Y40/00
Inventor 倪红卫张超张博威詹玮婷陈荣生
Owner WUHAN UNIV OF SCI & TECH
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