Method for preparing magnetic metal nanotubes by controlling electrodeposition conditions

A magnetic metal nano and electrodeposition technology, which is applied in the direction of nanotechnology, nanotechnology, metal material coating technology, etc., can solve the problems of affecting material performance, poor regularity, poor uniformity, etc., to achieve increased generation rate, good regularity, Good uniformity of length and wall thickness

Active Publication Date: 2019-05-21
NINGBO ZHETIE JIANGNING CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] However, this series of metal nanotubes are prepared by traditional electrochemical deposition methods, which either have relatively high requirements on the conductive layer, or introduce impurities that se

Method used

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  • Method for preparing magnetic metal nanotubes by controlling electrodeposition conditions
  • Method for preparing magnetic metal nanotubes by controlling electrodeposition conditions
  • Method for preparing magnetic metal nanotubes by controlling electrodeposition conditions

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preparation example Construction

[0062] (b-1) Preparation of salt bridge: 95-105 parts by weight of distilled water and 2.5-3.5 parts by weight of agar are added to the container, heated in a water bath until completely dissolved; then 25-35 parts by weight of KCl is added to fully dissolve it, and finally Pour it into a U-shaped thin glass tube while it is hot, and get a salt bridge after the agar solidifies.

[0063] (b-2) Sputtering conductive layer: a layer of copper film is sputtered on the anodized aluminum template: the conditions for sputtering the conductive layer are: the argon flow rate is 10-30 sccm, and the air pressure is 3-5×10 -4 Pa, the self-bias voltage is 150-200Pa. After copper plating, place the electrolyte and anodized aluminum template under a nitrogen atmosphere for 1-3 hours, and then deposit a layer of Cu nanorods on the bottom channel of the anodized aluminum template in the Cu electrodeposition solution. The deposition conditions are: voltage 0.7-0.9V, time 8-12min; component conc...

Embodiment 1

[0074] Embodiment 1 (magnetic metal Ni nanotube)

[0075] (1) Template preparation

[0076] (1-1) Select high-quality and high-purity (purity 99.999%) aluminum sheets and anneal at 500°C for 4 hours, then sonicate in acetone for 10 minutes, then soak in 5% (wt) sodium hydroxide for 5 minutes, and finally Sonicate in acetone for 3 minutes to complete the pretreatment of the aluminum sheet.

[0077] (1-2) The first oxidation: corrode the pretreated aluminum sheet at 40V voltage and 0°C for 4 hours, and the electrolyte concentration is 0.3mol / L oxalic acid.

[0078] (1-3) Removal of the primary oxide film: After taking it out, soak it in a mixed solution of 65°C, 6% (wt) phosphoric acid and 1.5% (wt) chromic acid for 12 hours to remove the primary oxide film, and clean it with deionized water .

[0079](1-4) Second oxidation: place the aluminum sheet from which the primary oxide film has been removed in 0.3mol / L oxalic acid aqueous solution, electrochemically corrode it for 8 ...

Embodiment 2

[0087] Embodiment 2 (magnetic metal Fe nanotube)

[0088] (1) Template preparation

[0089] (1-1) Select high-quality and high-purity (purity 99.999%) aluminum sheets and anneal at 500°C for 4 hours, then sonicate in acetone for 10 minutes, then soak in 5% (wt) sodium hydroxide for 5 minutes, and finally Sonicate in acetone for 3 minutes to complete the pretreatment of the aluminum sheet.

[0090] (1-2) The first oxidation: corrode the pretreated aluminum sheet at 40V voltage and 0°C for 4 hours, and the electrolyte concentration is 0.3mol / L oxalic acid.

[0091] (1-3) Removal of the primary oxide film: After taking it out, soak it in a mixed solution of 65°C, 6% (wt) phosphoric acid and 1.5% (wt) chromic acid for 12 hours to remove the primary oxide film, and clean it with deionized water .

[0092] (1-4) Second oxidation: place the aluminum sheet from which the primary oxide film has been removed in 0.3mol / L oxalic acid aqueous solution, electrochemically corrode it for 8...

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Abstract

The invention relates to the field of nano materials and discloses a method for preparing magnetic metal nanotubes by controlling electrodeposition conditions. The method comprises the following stepsof (a) preparing a template; (b) performing constant-potential deposition of the nanotubes, wherein (b-1) a salt bridge is prepared; (b-2) a conductive layer is applied in a spattering mode, namely,a layer of copper film is sputtered on an anodic aluminum oxide template; and (b-3) constant-potential electrodeposition is carried out, wherein an anodic aluminum oxide template sputtered with the copper film, a platinum sheet and a saturated calomel electrode are used as a working electrode, a counter electrode and a saturated calomel electrode in a three-electrode system correspondingly, an auxiliary electrode is soaked in a saturated KCl solution, and a saturated KCl solution is connected with electrolyte through the salt bridge, wherein deposition conditions are as follows: the pH value is 2-3, the deposition potential is-1-3V, and the deposition time is 300-600s; and (c) releasing the magnetic metal nanotubes, wherein the anodic aluminum oxide template obtained in the step (b) is soaked in a post-treatment solution to remove the aluminum oxide template and the copper film.

Description

technical field [0001] The invention relates to the field of nanometer materials, in particular to a method for preparing magnetic metal nanotubes by controlling electrodeposition conditions. Background technique [0002] Nanotubes have become a research hotspot in academia since electron microscope expert Iijima accidentally discovered carbon nanotubes, which are one-dimensional magnetic nanomaterials with hollow tubular structures. As a member of the nanotube family, magnetic nanotubes not only have the characteristics of nanotubes such as low density, high surface energy, excellent adsorption performance, and inner and outer double-layer active surfaces, but also have their own characteristics as one-dimensional magnetic materials. Such as excellent coercive force and remanence ratio, special magnetic reversal mode, small stable magnetic domain structure, magnetic nanotubes will not appear head-to-head domain walls, etc. [0003] Due to various novel properties, magnetic...

Claims

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Application Information

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IPC IPC(8): C25D3/12C25D3/20C25D11/10C25D11/12C25D11/16C23C28/00B82Y30/00B82Y40/00
Inventor 毛正余胡新跃胡军
Owner NINGBO ZHETIE JIANGNING CHEM
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