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

A kind of synthetic method of iron nanotube array Download PDF

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CN100390046C
CN100390046C CNB2004100989462A CN200410098946A CN100390046C CN 100390046 C CN100390046 C CN 100390046C CN B2004100989462 A CNB2004100989462 A CN B2004100989462A CN 200410098946 A CN200410098946 A CN 200410098946A CN 100390046 C CN100390046 C CN 100390046C
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曹化强
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Abstract

一种铁纳米管阵列的合成方法,涉及一种金属纳米材料的制备工艺。该方法是以以硫酸亚铁、硼酸、抗坏血酸为原料,在室温下,配制包括硫酸亚铁、硼酸、抗坏血酸的水溶液作为电解液。将该电解液放置一个电解槽内,将多孔氧化铝膜一面喷金或涂银浆方式制备金导电膜或银导电膜作为电化学反应的阴极,与电源的负极相连,另一面与电解液接触,并将金属铁棒作为电化学反应的阳极一端插入电解液中,另一端与电源的正极相连,接通电源,恒定电源的电流强度为10-20毫安培,即可得到金属铁纳米管阵列。该方法工艺简便,原料易得,可合成外径为80-100纳米,内径为30-50纳米,总长度最长可达到60微米的铁纳米管。本发明可望在微电子器件、磁记录等领域中得到应用。

Figure 200410098946

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.

Figure 200410098946

Description

一种铁纳米管阵列的合成方法 A kind of synthetic method of iron nanotube array

技术领域 technical field

本发明涉及一种金属纳米材料的制备,特别是涉及一种铁纳米管阵列的合成工艺及方法。The invention relates to the preparation of a metal nanometer material, in particular to a synthesis process and method of an iron nanotube array.

背景技术 Background technique

铁是一种常用的金属材料。在磁记录、电子输运等领域中有很重要的应用。铁纳米管阵列属于一种金属导电及兼具有较大矫顽力的磁性材料,无论在学术研究还是在应用方面,均具有重要的意义。目前尚未有铁纳米管阵列的合成专利报道。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.

发明内容 Contents of the invention

本发明的目的在于提供一种简便制备合成铁纳米管阵列的方法。本发明是通过如下技术方案实现的:一种铁纳米管阵列的合成方法,其特征是该方法按如下的步骤进行: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.以硫酸亚铁(FeSO4·7H2O)、硼酸(H3BO3)、抗坏血酸为原料,在室温下,配制含有硫酸亚铁、硼酸、抗坏血酸的水溶液作为电解液,硫酸亚铁(FeSO4·7H2O)浓度可在14-20克/100毫升范围,硼酸(H3BO3)浓度可在5-6克/100毫升范围,抗坏血酸浓度可在0.1-0.5克/100毫升范围。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.将多孔氧化铝膜一面用喷金或银浆涂层然后烘干得到金膜或银膜,作为电化学沉积反应的阴极;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.将上述经上述处理后的多孔氧化铝膜置于电解槽内,将电解液置于膜的另一面上,并将一铁片插入电解液中作为电化学反应的阳极;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.在室温下,接通电源并控制电流为(范围可在10-20毫安),一定时间(范围可在10-110分钟),可得到铁纳米管阵列。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.

本发明合成方法中所用原料易得,工艺简便,可合成出外径约80-100纳米,内径约30-50纳米,长度最长可达60微米的铁纳米管。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.

附图说明 Description of drawings

图1:为实施例1的铁纳米管扫描电子显微镜照片:Fig. 1: is the iron nanotube scanning electron microscope photograph of embodiment 1:

a——放大倍数为1千倍;a——The magnification is 1000 times;

b——放大倍数为1千倍;b——The magnification is 1000 times;

c——放大倍数为8千倍;c - the magnification is 8 thousand times;

d——放大倍数为20千倍,即2万倍;d——The magnification is 20 thousand times, that is, 20,000 times;

e——放大倍数为2千倍;e - the magnification is 2 thousand times;

f——放大倍数为10千倍,即1万倍。f——The magnification is 10 thousand times, that is, 10,000 times.

图2:为实施例2的铁纳米管X射线衍射图。Fig. 2: is the X-ray diffraction pattern of the iron nanotube of embodiment 2.

图3:为实施例3的铁纳米管X射线衍射图。Fig. 3: is the X-ray diffraction pattern of the iron nanotube of embodiment 3.

具体实施方式 Detailed ways

以下通过具体实施例对本发明进一步加以说明。The present invention will be further described below through specific examples.

实施例1:Example 1:

——以硫酸亚铁(FeSO4·7H2O)(14g/100ml)、硼酸(H3BO3)(5g/100ml)、抗坏血酸(0.1g/100ml)为原料,在室温下,配制含硫酸亚铁、硼酸、抗坏血酸的水溶液作为电解液。——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.

——将多孔氧化铝膜一面用银浆涂层然后烘干作为电化学沉积反应的阴极;- Coating one side of the porous aluminum oxide film with silver paste and then drying it as the cathode of the electrochemical deposition reaction;

——将上述经上述处理后的多孔氧化铝膜置于电解槽内,将电解液置于膜的另一面上,并将一铁片插入电解液中作为电化学反应的阳极;- 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;

——在室温下,接通电源并控制电流为10毫安,时间为约1小时45分钟,可得到铁纳米管阵列。——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.

由图1a可见该纳米管长度60微米,由图1c,d,f可见该纳米管外径约为80-100纳米,内径约为30-50纳米,由图1可见该纳米管呈现出阵列。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.

实施例2:Example 2:

——以硫酸亚铁(FeSO4·7H2O)(14g/100ml)、硼酸(H3BO3)(5g/100ml)、抗坏血酸(0.1g/100ml)为原料,在室温下,配制含硫酸亚铁、硼酸、抗坏血酸的水溶液作为电解液。——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.

——将多孔氧化铝膜一面喷金,作为电化学沉积反应的阴极;—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

——将上述经上述处理后的多孔氧化铝膜置于电解槽内,将电解液置于膜的另一面上,并将一铁片插入电解液中作为电化学反应的阳极;- 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;

——在室温下,接通电源并控制电流为10毫安,时间为约15分钟,可得到铁纳米管阵列。——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.

由图2可见该纳米管的结构成分属于铁。It can be seen from Figure 2 that the structural components of the nanotubes belong to iron.

实施例3:Example 3:

——以硫酸亚铁(FeSO4·7H2O)(14g/100ml)、硼酸(H3BO3)(5g/100ml)、抗坏血酸(0.1g/100ml)为原料,在室温下,配制含硫酸亚铁、硼酸、抗坏血酸的水溶液作为电解液。——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.

——将多孔氧化铝膜一面喷金,作为电化学沉积反应的阴极;—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

——将上述经上述处理后的多孔氧化铝膜置于电解槽内,将电解液置于膜的另一面上,并将一铁片插入电解液中作为电化学反应的阳极;- 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;

——在室温下,接通电源并控制电流为10毫安,时间为约18分钟,可得到铁纳米管阵列。——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.

由图3可见该纳米管的结构成分属于铁。It can be seen from Figure 3 that the structural components of the nanotubes belong to iron.

实施例4:Example 4:

——以硫酸亚铁(FeSO4·7H2O)(20g/100ml)、硼酸(H3BO3)(6g/100ml)、抗坏血酸(0.5g/100ml)为原料,在室温下,配制电解液包括硫酸亚铁、硼酸、抗坏血酸的水溶液。——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.

——将多孔氧化铝膜一面喷金,作为电化学沉积反应的阴极;—— Spray gold on one side of the porous aluminum oxide film as the cathode of the electrochemical deposition reaction;

——将上述经上述处理后的多孔氧化铝膜置于电解槽内,将电解液置于膜的另一面上,并将一铁片插入电解液中作为电化学反应的阳极;- 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;

——在室温下,接通电源并控制电流为20毫安,时间为约10分钟,可得到铁纳米管阵列。——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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CN102021654B (en) * 2010-12-06 2012-04-25 皖南医学院 A kind of preparation method of magnetic nanotube

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