CN100390046C - A kind of synthetic method of iron nanotube array - Google Patents

Abstract

The invention discloses a method for synthesizing an iron nanotube array, which relates to a preparation process of metal nanomaterials. The method uses ferrous sulfate, boric acid and ascorbic acid as raw materials, and prepares an aqueous solution comprising ferrous sulfate, boric acid and ascorbic acid as an electrolyte at room temperature. The electrolyte is placed in an electrolytic cell, and the porous aluminum oxide film is sprayed with gold or silver paste on one side to prepare a gold conductive film or a silver conductive film as the cathode of the electrochemical reaction, which is connected to the negative electrode of the power supply, and the other side is in contact with the electrolyte. , and insert one end of the metal iron rod as the anode of the electrochemical reaction into the electrolyte, the other end is connected to the positive pole of the power supply, and the power supply is turned on. The current intensity of the constant power supply is 10-20 milliamps, and the metal iron nanotube array can be obtained . The method has simple process and easy-to-obtain raw materials, and can synthesize iron nanotubes with an outer diameter of 80-100 nanometers, an inner diameter of 30-50 nanometers and a total length of up to 60 micrometers. The invention is expected to be applied in the fields of microelectronic devices, magnetic recording and the like.

Description

A kind of synthetic method of iron nanotube array

technical field

The invention relates to the preparation of a metal nanometer material, in particular to a synthesis process and method of an iron nanotube array.

Background technique

Iron is a commonly used metal material. It has very important applications in the fields of magnetic recording and electron transport. The iron nanotube array is a kind of magnetic material with metal conduction and large coercive force, which is of great significance in both academic research and application. At present, there is no patent report on the synthesis of iron nanotube arrays.

Contents of the invention

The purpose of the present invention is to provide a method for easily preparing and synthesizing iron nanotube arrays. The present invention is achieved through the following technical solutions: a method for synthesizing an iron nanotube array, characterized in that the method is carried out according to the following steps:

a. Take ferrous sulfate (FeSO ₄ 7H ₂ O), boric acid (H ₃ BO ₃ ), and ascorbic acid as raw materials, at room temperature, prepare an aqueous solution containing ferrous sulfate, boric acid, and ascorbic acid as the electrolyte, and ferrous sulfate ( The concentration of FeSO ₄ 7H ₂ O) can be in the range of 14-20 g/100 ml, the concentration of boric acid (H ₃ BO ₃ ) can be in the range of 5-6 g/100 ml, and the concentration of ascorbic acid can be in the range of 0.1-0.5 g/100 ml .

b. One side of the porous aluminum oxide film is coated with gold or silver paste and then dried to obtain a gold film or a silver film, which is used as the cathode of the electrochemical deposition reaction;

c. placing the above-mentioned porous aluminum oxide film after the above-mentioned treatment in the electrolytic cell, placing the electrolytic solution on the other side of the film, and inserting an iron sheet into the electrolytic solution as the anode of the electrochemical reaction;

d. At room temperature, turn on the power supply and control the current to be (in the range of 10-20 milliamps), and for a certain period of time (in the range of 10-110 minutes), the iron nanotube array can be obtained.

The raw materials used in the synthesis method of the present invention are easy to obtain and the process is simple, and the iron nanotubes with an outer diameter of about 80-100 nanometers, an inner diameter of about 30-50 nanometers and a length of up to 60 microns can be synthesized.

Description of drawings

Fig. 1: is the iron nanotube scanning electron microscope photograph of embodiment 1:

a——The magnification is 1000 times;

b——The magnification is 1000 times;

c - the magnification is 8 thousand times;

d——The magnification is 20 thousand times, that is, 20,000 times;

e - the magnification is 2 thousand times;

f——The magnification is 10 thousand times, that is, 10,000 times.

Fig. 2: is the X-ray diffraction pattern of the iron nanotube of embodiment 2.

Fig. 3: is the X-ray diffraction pattern of the iron nanotube of embodiment 3.

Detailed ways

The present invention will be further described below through specific examples.

Example 1:

——Using ferrous sulfate (FeSO ₄ 7H ₂ O) (14g/100ml), boric acid (H ₃ BO ₃ ) (5g/100ml) and ascorbic acid (0.1g/100ml) as raw materials, prepare sulfuric acid containing The aqueous solution of ferrous iron, boric acid and ascorbic acid is used as electrolyte.

- Coating one side of the porous aluminum oxide film with silver paste and then drying it as the cathode of the electrochemical deposition reaction;

- placing the above-mentioned porous aluminum oxide film after the above-mentioned treatment in the electrolytic cell, placing the electrolyte solution on the other side of the film, and inserting an iron sheet into the electrolyte solution as the anode of the electrochemical reaction;

——At room temperature, turn on the power supply and control the current to 10 mA for about 1 hour and 45 minutes to obtain the iron nanotube array.

It can be seen from Fig. 1a that the length of the nanotube is 60 microns. It can be seen from Fig. 1c, d, f that the outer diameter of the nanotube is about 80-100 nanometers, and the inner diameter is about 30-50 nanometers. It can be seen from Fig. 1 that the nanotube presents an array.

Example 2:

——Using ferrous sulfate (FeSO ₄ 7H ₂ O) (14g/100ml), boric acid (H ₃ BO ₃ ) (5g/100ml) and ascorbic acid (0.1g/100ml) as raw materials, prepare sulfuric acid containing The aqueous solution of ferrous iron, boric acid and ascorbic acid is used as electrolyte.

—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

- placing the above-mentioned porous aluminum oxide film after the above-mentioned treatment in the electrolytic cell, placing the electrolyte solution on the other side of the film, and inserting an iron sheet into the electrolyte solution as the anode of the electrochemical reaction;

——At room temperature, switch on the power supply and control the current to 10 mA for about 15 minutes to obtain the iron nanotube array.

It can be seen from Figure 2 that the structural components of the nanotubes belong to iron.

Example 3:

——Using ferrous sulfate (FeSO ₄ 7H ₂ O) (14g/100ml), boric acid (H ₃ BO ₃ ) (5g/100ml) and ascorbic acid (0.1g/100ml) as raw materials, prepare sulfuric acid containing The aqueous solution of ferrous iron, boric acid and ascorbic acid is used as electrolyte.

—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

- placing the above-mentioned porous aluminum oxide film after the above-mentioned treatment in the electrolytic cell, placing the electrolyte solution on the other side of the film, and inserting an iron sheet into the electrolyte solution as the anode of the electrochemical reaction;

——At room temperature, turn on the power supply and control the current to 10 mA for about 18 minutes to obtain the iron nanotube array.

It can be seen from Figure 3 that the structural components of the nanotubes belong to iron.

Example 4:

——Using ferrous sulfate (FeSO ₄ 7H ₂ O) (20g/100ml), boric acid (H ₃ BO ₃ ) (6g/100ml), and ascorbic acid (0.5g/100ml) as raw materials, prepare the electrolyte solution at room temperature Including ferrous sulfate, boric acid, ascorbic acid in water.

—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

- placing the above-mentioned porous aluminum oxide film after the above-mentioned treatment in the electrolytic cell, placing the electrolyte solution on the other side of the film, and inserting an iron sheet into the electrolyte solution as the anode of the electrochemical reaction;

——At room temperature, switch on the power supply and control the current to 20 mA for about 10 minutes to obtain the iron nanotube array.

Claims (2)

1. the synthetic method of an iron nanotube array is characterized in that, this method is carried out as follows:

A. with ferrous sulfate (FeSO ₄7H ₂O), boric acid (H ₃BO ₃), ascorbic acid is raw material, at room temperature, the aqueous solution that preparation contains ferrous sulfate, boric acid, ascorbic acid is as electrolyte, ferrous sulfate (FeSO ₄7H ₂O) concentration can restrain at 14-20/100 milliliters of scopes, boric acid (H ₃BO ₃) concentration can restrain at 5-6/100 milliliters of scopes, ascorbic acid concentrations can restrain at 0.1-0.5/100 milliliters of scopes;

B. the multiaperture pellumina one side is dried then with metal spraying and obtain golden film, as the negative electrode of electrochemical deposition reaction;

C. above-mentioned multiaperture pellumina after above-mentioned processing is placed in the electrolytic cell, electrolyte is placed on the another side of film, and an iron plate is inserted in the electrolyte anode as electrochemical reaction;

D. at room temperature, connecting power supply and controlling electric current is the 10-20 milliampere, and the time is 10-110 minute, promptly obtains iron nanotube array.

2. according to the synthetic method of the described a kind of iron nanotube array of claim 1, it is characterized in that step b obtains silverskin for multiaperture pellumina is simultaneously dried then with silver slurry coating, as the negative electrode of electrochemical deposition reaction.

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