CN100390046C - Synthesis method of iron nanotube array - Google Patents
Synthesis method of iron nanotube array Download PDFInfo
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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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- Prior art keywords
- electrolyte
- iron
- conducting film
- power supply
- ferrous sulfate
- Prior art date
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 32
- 239000002071 nanotube Substances 0.000 title claims description 24
- 238000001308 synthesis method Methods 0.000 title 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 32
- 239000003792 electrolyte Substances 0.000 claims abstract description 22
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 16
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 16
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 13
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 13
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 235000010338 boric acid Nutrition 0.000 claims abstract description 5
- 238000004070 electrodeposition Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- 238000010189 synthetic method Methods 0.000 claims description 5
- 238000007581 slurry coating method Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 4
- 239000010931 gold Substances 0.000 abstract 4
- 229910052737 gold Inorganic materials 0.000 abstract 4
- 238000003491 array Methods 0.000 abstract 2
- 229960002645 boric acid Drugs 0.000 abstract 2
- 229960001781 ferrous sulfate Drugs 0.000 abstract 2
- 230000002194 synthesizing effect Effects 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000004377 microelectronic Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/10—Reduction of greenhouse gas [GHG] emissions
- Y02P10/134—Reduction of greenhouse gas [GHG] emissions by avoiding CO2, e.g. using hydrogen
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a synthesizing method for iron nanometer pipe arrays, which relates to a preparation technology of metal nanometer materials. In the method, ferrous sulfate, boracic acid and ascorbic acid are used as raw materials; at room temperature, a water solution comprising ferrous sulfate, boracic acid and ascorbic acid is prepared as an electrolyte; the electrolyte is placed in an electrolytic tank; a gold conducting film or a silver conducting film is prepared as a cathode of electrochemical reaction in the method that one surface of a porous alumina film is sprayed with gold or is spread with silver pulp; the gold conducting film or the silver conducting film is connected with a negative electrode of a power supply, and the other surface of the gold conducting film or the silver conducting film comes into contact with the electrolyte; one end of a metal iron rod as an anode of electrochemical reaction is inserted in the electrolyte, and the other end is connected with a positive electrode of the power supply; the power supply is switched on, the current strength of the constant power supply is from 10 milliamperes to 20 milliamperes, and metal iron nanometer pipe arrays are obtained. The method has the advantages of convenient and simple technology and easy raw material obtainment, and the method can be used for synthesizing iron nanometer pipes with an outer diameter of 80 nm to 100 nm, an inner diameter of 30 nm to 50 nm and maximum total length of 60 nanometers. The method can be applied to the fields of microelectronic devices, magnetic records, etc.
Description
Technical field
The present invention relates to a kind of preparation of metal nano material, particularly relate to a kind of synthesis technique and method of iron nanotube array.
Background technology
Iron is a kind of metal material commonly used.Very important use is arranged in fields such as magnetic recording, electron transport.Iron nanotube array belongs to a kind of metallic conduction and with bigger coercitive magnetic material, no matter in academic research or in application facet, all has great importance.The synthetic patent report that iron nanotube array is not arranged at present as yet.
Summary of the invention
The object of the present invention is to provide the method for the synthetic iron nanotube array of a kind of easy preparation.The present invention is achieved through the following technical solutions: a kind of synthetic method of iron nanotube array is characterized in that this method undertaken by following step:
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 or silver slurry coating and obtain golden film or silverskin, 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, connect power supply and control electric current and be (scope can at the 10-20 milliampere), certain hour (scope can at 10-110 minute) can obtain iron nanotube array.
Raw materials used being easy to get in the synthetic method of the present invention, technology is easy, can synthesize the about 80-100 nanometer of external diameter, the about 30-50 nanometer of internal diameter, the longest iron nanotube that reaches 60 microns of length.
Description of drawings
Fig. 1: be the iron nanotube electron scanning micrograph of embodiment 1:
A---multiplication factor is 1,000 times;
B---multiplication factor is 1,000 times;
C---multiplication factor is 8,000 times;
D---multiplication factor is 20,000 times, promptly 20,000 times;
E---multiplication factor is 2,000 times;
F---multiplication factor is 10,000 times, promptly 10,000 times.
Fig. 2: be the iron nanotube X-ray diffractogram of embodiment 2.
Fig. 3: be the iron nanotube X-ray diffractogram of embodiment 3.
The specific embodiment
Below by specific embodiment the present invention further is illustrated.
Embodiment 1:
---with ferrous sulfate (FeSO
47H
2O) (14g/100ml), boric acid (H
3BO
3) (5g/100ml), ascorbic acid (0.1g/100ml) is raw material, at room temperature, the preparation sulfur acid is ferrous, the aqueous solution of boric acid, ascorbic acid is as electrolyte.
---multiaperture pellumina is simultaneously dried the negative electrode that reacts as electrochemical deposition then with silver slurry coating;
---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;
---at room temperature, connecting power supply and controlling electric current is 10 milliamperes, and the time is about 1 hour 45 minutes, can obtain iron nanotube array.
By 60 microns of visible this nanotube length of Fig. 1 a, by Fig. 1 c, d, visible this nanotube external diameter of f is about the 80-100 nanometer, and internal diameter is about the 30-50 nanometer, and this nanotube presents array as seen from Figure 1.
Embodiment 2:
---with ferrous sulfate (FeSO
47H
2O) (14g/100ml), boric acid (H
3BO
3) (5g/100ml), ascorbic acid (0.1g/100ml) is raw material, at room temperature, the preparation sulfur acid is ferrous, the aqueous solution of boric acid, ascorbic acid is as electrolyte.
---with metal spraying of multiaperture pellumina, as the negative electrode of electrochemical deposition reaction;
---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;
---at room temperature, connecting power supply and controlling electric current is 10 milliamperes, and the time is about 15 minutes, can obtain iron nanotube array.
The constituent of this nanotube belongs to iron as seen from Figure 2.
Embodiment 3:
---with ferrous sulfate (FeSO
47H
2O) (14g/100ml), boric acid (H
3BO
3) (5g/100ml), ascorbic acid (0.1g/100ml) is raw material, at room temperature, the preparation sulfur acid is ferrous, the aqueous solution of boric acid, ascorbic acid is as electrolyte.
---with metal spraying of multiaperture pellumina, as the negative electrode of electrochemical deposition reaction;
---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;
---at room temperature, connecting power supply and controlling electric current is 10 milliamperes, and the time is about 18 minutes, can obtain iron nanotube array.
The constituent of this nanotube belongs to iron as seen from Figure 3.
Embodiment 4:
---with ferrous sulfate (FeSO
47H
2O) (20g/100ml), boric acid (H
3BO
3) (6g/100ml), ascorbic acid (0.5g/100ml) is raw material, at room temperature, preparation electrolyte comprises the aqueous solution of ferrous sulfate, boric acid, ascorbic acid.
---with metal spraying of multiaperture pellumina, as the negative electrode of electrochemical deposition reaction;
---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;
---at room temperature, connecting power supply and controlling electric current is 20 milliamperes, and the time is about 10 minutes, can obtain 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100989462A CN100390046C (en) | 2004-12-17 | 2004-12-17 | Synthesis method of iron nanotube array |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100989462A CN100390046C (en) | 2004-12-17 | 2004-12-17 | Synthesis method of iron nanotube array |
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| Publication Number | Publication Date |
|---|---|
| CN1621338A CN1621338A (en) | 2005-06-01 |
| CN100390046C true CN100390046C (en) | 2008-05-28 |
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|---|---|---|---|
| CNB2004100989462A Expired - Fee Related CN100390046C (en) | 2004-12-17 | 2004-12-17 | Synthesis method of iron nanotube array |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432304C (en) * | 2006-12-22 | 2008-11-12 | 南京大学 | Electric method for quick preparation for nanotube |
| CN101692364B (en) * | 2009-10-12 | 2012-09-05 | 钢铁研究总院 | One-dimensional permanent magnetic nano-material, in which hard magnetic tubes are coated with soft magnetic wires and preparation method thereof |
| CN102021654B (en) * | 2010-12-06 | 2012-04-25 | 皖南医学院 | Method for preparing magnetic nanotube |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300713A (en) * | 1999-12-22 | 2001-06-27 | 南京大学 | Process for synthesizing nm carbon tubes containing nm metal wires |
| JP2004161571A (en) * | 2002-11-14 | 2004-06-10 | National Institute For Materials Science | Boron/carbon/nitrogen nanotube and its production process |
-
2004
- 2004-12-17 CN CNB2004100989462A patent/CN100390046C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1300713A (en) * | 1999-12-22 | 2001-06-27 | 南京大学 | Process for synthesizing nm carbon tubes containing nm metal wires |
| JP2004161571A (en) * | 2002-11-14 | 2004-06-10 | National Institute For Materials Science | Boron/carbon/nitrogen nanotube and its production process |
Non-Patent Citations (8)
| Title |
|---|
| Boron nitride nanotubes and nanowires. F.L.Deepak,et al.Chemical Physics Letters,Vol.353 No.5-6. 2002 |
| Boron nitride nanotubes and nanowires. F.L.Deepak,et al.Chemical Physics Letters,Vol.353 No.5-6. 2002 * |
| Coaxial nanocables:Fe nanowires encapasulated in BNnanotubes with intermediate C layers. Renzhi Ma,et al.Chemical Physics Letters,Vol.350 No.1-2. 2001 |
| Coaxial nanocables:Fe nanowires encapasulated in BNnanotubes with intermediate C layers. Renzhi Ma,et al.Chemical Physics Letters,Vol.350 No.1-2. 2001 * |
| Synthesis of Eu2O3 nanotube arrays through a facile sol-geltemplate approach. Guosheng Wu,et al.Journal of the American Chemical Society,Vol.126 No.19. 2004 |
| Synthesis of Eu2O3 nanotube arrays through a facile sol-geltemplate approach. Guosheng Wu,et al.Journal of the American Chemical Society,Vol.126 No.19. 2004 * |
| 新型交流电沉积法制备多种金属氧化物纳米材料并对其形貌进行控制. 王翠英.第四届中国功能材料及其应用学术会议论文集. 2001 |
| 新型交流电沉积法制备多种金属氧化物纳米材料并对其形貌进行控制. 王翠英.第四届中国功能材料及其应用学术会议论文集. 2001 * |
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| CN1621338A (en) | 2005-06-01 |
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