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Preparation method of one-dimensional mesoporous Co nanowire array

A nanowire array and mesoporous technology, applied in the field of inorganic nanomaterial synthesis, can solve the problems of inability to prepare one-dimensionally oriented mesoporous nanostructures, inability to obtain one-dimensional magnetic Co nanostructures, and inability to obtain SBA structures, etc. The preparation process is easy to operate, small mesopore size, and the effect of large specific surface

Inactive Publication Date: 2010-01-20
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

Although the preparation of Co nanowire arrays by electrochemical deposition in AAO templates has been reported in the literature, 1D magnetic Co nanostructures with mesoporous structures cannot be obtained by this method.
British "Nature" (Nature 2004, No. 3, page 816) and American "Nano Letters" (Nano Letter 2004, No. 4, page 2337) respectively reported the use of sol-gel (Sol-Gel) method in macroporous AAO. Obtained SiO with hexagonal mesoporous structure 2 Fiber (SBA), by controlling the addition ratio of surfactants, structure-directing agents, and silicon sources, helical and layered SiO can be obtained 2 fiber, but the SBA structure parallel to the AAO template pore wall cannot be obtained
Therefore, the electrochemical deposition of this AAO-SBA composite template can only obtain point-like particles distributed in the SBA mesoporous channels, and it is impossible to prepare mesoporous nanostructures with one-dimensional orientation.

Method used

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  • Preparation method of one-dimensional mesoporous Co nanowire array
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  • Preparation method of one-dimensional mesoporous Co nanowire array

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Preparation of porous alumina template by one-step anodic oxidation method

[0023] The annealed aluminum sheet was put into an electrolytic cell, 0.36 mol / mL phosphoric acid was used as the electrolyte, and an oxidation voltage of 120V was applied at 0-5°C for oxidation, and the oxidation time was 60 hours. Then the prepared alumina template is immersed in 0.36 mol / mL phosphoric acid solution for 2-3 hours. This step is used to expand the pore size of the porous alumina template.

[0024] 2) Preparation of AAO-SBA composite mesoporous template with mesoporous channels parallel to AAO channels

[0025] At room temperature, 0.6 g of P123 and 40 ml of ethanol were mixed uniformly. Then, 0.93 g of tetraethyl orthosilicate and 0.4 g of hydrochloric acid (38 wt%) were added dropwise, and stirring was continued to make the solution uniformly mixed to obtain a precursor solution. At room temperature, the prepared porous alumina template was immersed in the precursor solution for...

Embodiment 2

[0036] 1) Prepare porous alumina template by one-step anodic oxidation method (same as Example 1)

[0037] 2) Preparation of AAO-SBA composite mesoporous template with mesoporous channels parallel to AAO channels

[0038] At room temperature, mix 0.5 g of P123 and 40 ml of ethanol. Then, 0.93g of tetraethylorthosilicate and 0.4g of hydrochloric acid (38wt%) were added dropwise, and stirring was continued to make the solution evenly mixed, and the prepared AAO template was soaked in the precursor solution for 20h. After that, the alumina template was taken out and dried at 50°C for 13 hours, and then kept at 400°C for 5 hours.

[0039] 3) Removal of SiO on the surface of the composite mesoporous template 2 Oxide layer (same as Example 1)

[0040] 4) Preparation of one-dimensional mesoporous Co nanowires

[0041] Weigh 2 g of cobalt acetate and 2 g of boric acid and dissolve in 100 mL of distilled water, and stir until the cobalt acetate and boric acid are all dissolved and mixed unifor...

Embodiment 3

[0043] 1) Prepare porous alumina template by one-step anodic oxidation method (same as Example 1)

[0044] 2) Preparation of AAO-SBA composite mesoporous template with mesoporous channels parallel to AAO channels

[0045] At room temperature, 0.7g of P123 and 40ml of ethanol were mixed uniformly. Then, 0.93g of tetraethylorthosilicate and 0.4g of hydrochloric acid (38wt%) were added dropwise respectively, and stirring was continued to make the solution evenly mixed, and the prepared AAO template was soaked in the precursor solution for 22h. Then it was dried at 70°C for 15 hours, and then kept at 500°C for 6 hours.

[0046] 3) Removal of SiO on the surface of the composite mesoporous template 2 Oxide layer (same as Example 1)

[0047] 4) Preparation of one-dimensional mesoporous Co nanowires

[0048] Weigh 2 g of cobalt acetate and 3 g of boric acid and dissolve in 100 mL of distilled water, and stir until the cobalt acetate and boric acid are all dissolved and mixed uniformly. Contr...

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Abstract

The invention discloses a preparation method of a one-dimensional mesoporous Co nanowire array, which comprising the following steps: preparing a precursor solution at room temperature by mixing 0.5-0.7g of PEP-POO-PEP (P123) which is an addition polymer of polypropylene glycol and ethylene oxide, 0.9-3g of tetraethyl orthosilicate and 0.4g of 38 wt% muriatic acid together; in an AAO (anodised aluminium) template, synthesizing SBA (mesoporous silica) nanofibers, wherein the mesoporous canals of the SBA (mesoporous silica) nanofibers are parallel to AAO canals; preparing electrodeposit liquid in the ratio of 2-4g of Co(CH3COO)2 : 1-3g of H3BO3; taking an aluminium base AAO-SBA composite mesoporous template as a working electrode and taking graphite as an auxiliary electrode, and controlling electrode density between 0.5-1.5 mA / cm2 and electrodepositing for 1.0-1.5h to obtain a Co nanowire with the width of about 200nm, wherein the Co nanowire consists of 4-6mn mesoporous Co nano rods. The invention adopts a simple electrochemical method to generate Co nano structures in AAO-SBA composite mesopores for the first time; and the growth direction of the crystals of the nano structures is controlled by the mesoporous canals. The invention has simple equipment, can be operated easily and is suitable to the industrial production.

Description

Technical field [0001] The invention relates to a method for preparing a one-dimensional mesoporous Co nanowire array, which belongs to the field of inorganic nano material synthesis. Background technique [0002] With the continuous development of new technologies, the structure and performance requirements of nanomaterials are getting higher and higher. One-dimensional mesoporous materials have been widely concerned by researchers because of their narrow pore size distribution, diverse pore shapes, high specific surface area, and high pore volume. One-dimensional mesoporous SiO using electrochemical deposition method 2 Compared with solid nanowires, the novel mesoporous nanowire materials synthesized in the pores have many obvious characteristics: (1) Higher specific surface area; (2) Periodically adjustable morphology, metal surface morphology It affects the cytoplasmic gene resonance on the metal surface and expands the application of metals in the field of spectroscopy; (3)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B30/02C30B29/02C30B29/62C25D1/04C25D1/10
Inventor 姬广斌龚志红高婷婷
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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