CN101695994B - Carbon nano tube-doped ferric oxide three-dimensional nanometer material and preparation method thereof - Google Patents
Carbon nano tube-doped ferric oxide three-dimensional nanometer material and preparation method thereof Download PDFInfo
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- CN101695994B CN101695994B CN2009102334487A CN200910233448A CN101695994B CN 101695994 B CN101695994 B CN 101695994B CN 2009102334487 A CN2009102334487 A CN 2009102334487A CN 200910233448 A CN200910233448 A CN 200910233448A CN 101695994 B CN101695994 B CN 101695994B
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Abstract
The invention discloses a carbon nano tube-doped ferric oxide three-dimensional nanometer material and a preparation method thereof, which relate to the technical field of the preparation of nanometer material. In the method, 1, 4 butylene glycol is used as a solvent, an acidified carbon nano tube is used as a doped phase, soluble trivalent ferric salt and ethylene diamine are used as raw materials, the materials are mixed at room temperature to form a uniform suspension, the uniform suspension is transferred into a mixed system to a stainless steel reaction liner, and stainless steel reaction liner is sealed for the uniform suspension to react in a baking oven at 150 to 200 degrees centigrade for 10 to 20 hours to obtain carbon nano tube-doped ferric oxide powder. The nano powder has a cuboid structure assembled by nano particles, and the cuboid has a length of between 0.1 and 0.5 mu m and a width of between 0.05 and 0.2 mu m. The method of the invention is simple. A solvent heating method is used for the first time to prepare a cuboid material assembled by doped ferric oxide nano particles of the three-dimensional carbon nano tube, thereby expanding the preparation field of the ferric oxide material.
Description
Technical field
The present invention relates to the preparing technical field of nano material, be specifically related to the preparation method of carbon nano tube-doped ferric oxide three-dimensional nano structural material.
Background technology
CNT has caused the extensive concern of scientific circles with its excellent magnetic, electricity, mechanical property, microwave absorbing property and unique hollow structure.Ferriferrous oxide nanometer material is widely used in the high density magnetic recording material, is used for storage, and is used to prepare absorbing material, xerography ink, wide band transformer, noise filter, communication with transformer etc.To show excellent magnetism, electrical and microwave absorbing property more with the carbon nano tube-doped ferric oxide nano material, have application prospect widely.
Patent (CN 1743387A) discloses a kind of preparation method of magnetic compound material of ferric oxide cladded carbon nanotube, and it adopts, and the ferric iron particle adheres in the acidifying carbon nano tube surface, hydrolysis, dehydration prepare the di-iron trioxide coated carbon nanotube.The di-iron trioxide coated carbon nanotube of its preparation belongs to one-dimentional structure, and magnetic induction intensity is lower, and in addition, this preparation process adopts the dehydration of high temperature inert atmosphere protection not only to increase the cost of product, and makes the preparation process complicated.
Compare with the nano structural material of peacekeeping two dimension, the 3-D nano, structure material has excellent more electricity, optics, catalysis and magnetic performance.At present, 3-D nano, structure is mainly through the template preparation, and still poor through the nano material crystallinity of template preparation, template is removed relatively difficulty simultaneously, has increased cost, is unfavorable for the heavy industrialization of material.
Summary of the invention
A kind of simple unformed method provided by the present invention prepares the carbon nano tube-doped ferric oxide three-dimensional nano structural material, to remedy the deficiency of prior art, satisfies the needs of producing with the development of relevant field.
A kind of preparation method of carbon nano tube-doped ferric oxide three-dimensional nanometer material; It is characterized in that may further comprise the steps: with 1 of solubility trivalent iron salt; 1,4 butanediol solution and the acidifying CNT of 4 butanediol solutions, ethylenediamine at room temperature mix the suspension that forms homogeneous, then suspension are transferred in the container; The sealing back in 150-220 ℃ of reaction 10-20h, can obtain the carbon nano tube-doped ferric oxide powder in baking oven; 1,4 butanediol solution of solubility trivalent iron salt, 1,4 butanediol solution of ethylenediamine are pressed equal-volume and are added, and the molar concentration of 1,4 butanediol solution of solubility trivalent iron salt is 0.1-0.5M, and the molar concentration of ethylenediamine 1,4 butanediol solution is 0.5-1.0M; The addition of acidifying CNT is the 1/1000-1/100 of trivalent iron salt amount of substance.This nano-powder has the rectangular structure that nano particle is assembled into, and cuboid is long to be 0.1-0.5 μ m, and wide is 0.05-0.2 μ m.
Among the above-mentioned preparation method, the solubility trivalent iron salt is ferric nitrate, iron chloride or ferric sulfate.
Among the above-mentioned preparation method, container refers to polytetrafluoroethylene bushing, and compactedness is 80%.
The present invention adopts solvent thermal method to prepare the cuboid material of the ferric oxide nanometer particle assembling of three dimensional carbon nanotubes doping first, has widened the preparation field of iron oxide material.
Description of drawings
Fig. 1 is the low power stereoscan photograph of prepared carbon nano tube-doped ferric oxide in the embodiment of the invention 1.
Fig. 2 is the high power stereoscan photograph of prepared carbon nano tube-doped ferric oxide in the embodiment of the invention 1.
Fig. 3 is the XRD curve of prepared carbon nano tube-doped ferric oxide in the embodiment of the invention 1, and through contrasting with the standard spectrogram, the iron oxide of generation is a tri-iron tetroxide.
The specific embodiment
Embodiment 1:
With the acidifying CNT of 0.05g add to 24ml 0.3M ferric nitrate 1,4 butanediol solution of 1,4 butanediol solution and 24ml 0.5M ethylenediamine in; After evenly mixing, the capacity of pouring into is in the 60ml polytetrafluoroethylene bushing, and compactedness is 80%; The polytetrafluoroethylene bushing that sealing is good is put into 200 ℃ of reactions of water heating kettle 12 hours, be cooled to room temperature after, filter; Drying, obtaining being about is 0.25 μ m, the wide cuboid carbon nano tube-doped ferric oxide that is about 0.15 μ m.
Embodiment 2:
With the acidifying CNT of 0.01g add to 24ml 0.4M iron chloride 1,4 butanediol solution of 1,4 butanediol solution and 24ml 0.7M ethylenediamine in; After evenly mixing, the capacity of pouring into is in the 60ml polytetrafluoroethylene bushing, and compactedness is 80%; The polytetrafluoroethylene bushing that sealing is good is put into 200 ℃ of reactions of water heating kettle 10 hours, be cooled to room temperature after, filter; Drying, obtaining being about is 0.3 μ m, the wide carbon nano tube-doped ferric oxide that is about the rectangular shape of 0.1 μ m.
Embodiment 3:
With the acidifying CNT of 0.01g add to 24ml 0.5M ferric sulfate 1,4 butanediol solution of 1,4 butanediol solution and 24ml 0.8M ethylenediamine in; After evenly mixing, the capacity of pouring into is in the 60ml polytetrafluoroethylene bushing, and compactedness is 80%; The polytetrafluoroethylene bushing that sealing is good is put into 180 ℃ of reactions of water heating kettle 15 hours, be cooled to room temperature after, filter; Drying, obtaining being about is 0.1 μ m, the wide carbon nano tube-doped ferric oxide that is about the rectangular shape of 0.08 μ m.
Embodiment 4:
With the acidifying CNT of 0.03g add to 24ml 0.3M ferric nitrate 1,4 butanediol solution of 1,4 butanediol solution and 24ml 0.6M ethylenediamine in; After evenly mixing, the capacity of pouring into is in the 60ml polytetrafluoroethylene bushing, and compactedness is 80%; The polytetrafluoroethylene bushing that sealing is good is put into 150 ℃ of reactions of water heating kettle 15 hours, be cooled to room temperature after, filter; Drying, obtaining being about is 0.3 μ m, the wide carbon nano tube-doped ferric oxide that is about the rectangular shape of 0.2 μ m.
Claims (4)
1. carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material; It is characterized in that: said nano material has the rectangular structure that nano particle is assembled into, and said cuboid is long to be 0.1-0.5 μ m, and wide is 0.05-0.2 μ m; Said preparation of nanomaterials is following: with 1 of solubility trivalent iron salt; 1,4 butanediol solution and the acidifying CNT of 4 butanediol solutions, ethylenediamine at room temperature mix the suspension that forms homogeneous, then suspension are transferred in the container; The sealing back in 150-220 ℃ of reaction 10-20h, can obtain carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material in baking oven; 1,4 butanediol solution of solubility trivalent iron salt and 1,4 butanediol solution of ethylenediamine are pressed equal-volume and are added, and the molar concentration of 1,4 butanediol solution of solubility trivalent iron salt is 0.1-0.5M, and the molar concentration of ethylenediamine 1,4 butanediol solution is 0.5-1.0M; The addition of acidifying CNT is the 1/1000-1/100 of trivalent iron salt amount of substance.
2. the preparation method of a kind of carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material as claimed in claim 1; It is characterized in that may further comprise the steps: with 1 of solubility trivalent iron salt; 1,4 butanediol solution and the acidifying CNT of 4 butanediol solutions, ethylenediamine at room temperature mix the suspension that forms homogeneous, then suspension are transferred in the container; The sealing back in 150-220 ℃ of reaction 10-20h, can obtain carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material in baking oven; 1,4 butanediol solution of solubility trivalent iron salt and 1,4 butanediol solution of ethylenediamine are pressed equal-volume and are added, and the molar concentration of 1,4 butanediol solution of solubility trivalent iron salt is 0.1-0.5M, and the molar concentration of ethylenediamine 1,4 butanediol solution is 0.5-1.0M; The addition of acidifying CNT is the 1/1000-1/100 of trivalent iron salt amount of substance.
3. the preparation method of a kind of carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material as claimed in claim 2 is characterized in that: the solubility trivalent iron salt is ferric nitrate, iron chloride or ferric sulfate.
4. the preparation method of a kind of carbon nano tube-doped tri-iron tetroxide three-dimensional nanometer material as claimed in claim 2 is characterized in that: container refers to polytetrafluoroethylene bushing, and compactedness is 80%.
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| CN101695994B true CN101695994B (en) | 2012-08-15 |
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| CN103115947B (en) * | 2013-03-05 | 2014-04-23 | 济南大学 | Preparation method and application of carbon-doped mesoporous metal oxide acetone sensor |
| CN110127769A (en) * | 2019-05-21 | 2019-08-16 | 东北大学 | A method of iron-based negative electrode material is prepared based on hydro-thermal method |
Citations (5)
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| JP2004140259A (en) * | 2002-10-18 | 2004-05-13 | Osaka Gas Co Ltd | Magnetic fluid |
| CN1670251A (en) * | 2005-03-01 | 2005-09-21 | 东华大学 | Method for preparing magnetic compound material of ferric oxide cladded carbon nanotube |
| CN1778470A (en) * | 2005-09-29 | 2006-05-31 | 华东师范大学 | Production of iron oxide nanometer thin-membrane carried on carbon nanometer tubes |
| CN1794372A (en) * | 2005-10-31 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Magnetic composite powder for ferroferric oxide nanometer crystal modified carbon nanometer pipe and its preparation method |
| CN100999319A (en) * | 2006-12-31 | 2007-07-18 | 哈尔滨工业大学 | Preparation method of magnetic controlled ultra paramagnetism nanometer carbon pipe |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004140259A (en) * | 2002-10-18 | 2004-05-13 | Osaka Gas Co Ltd | Magnetic fluid |
| CN1670251A (en) * | 2005-03-01 | 2005-09-21 | 东华大学 | Method for preparing magnetic compound material of ferric oxide cladded carbon nanotube |
| CN1778470A (en) * | 2005-09-29 | 2006-05-31 | 华东师范大学 | Production of iron oxide nanometer thin-membrane carried on carbon nanometer tubes |
| CN1794372A (en) * | 2005-10-31 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Magnetic composite powder for ferroferric oxide nanometer crystal modified carbon nanometer pipe and its preparation method |
| CN100999319A (en) * | 2006-12-31 | 2007-07-18 | 哈尔滨工业大学 | Preparation method of magnetic controlled ultra paramagnetism nanometer carbon pipe |
Non-Patent Citations (2)
| Title |
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| 于华荣，等.碳纳米管负载纳米Fe2O3的研究.《无机化学学报》.2005,第21卷(第11期),1649-1654. * |
| 蒋峰景,等.Fe3O4包覆碳纳米管软磁性纳米复合微粒的制备及性能.《新型炭材料》.2007,第24卷(第4期),371-374. * |
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