CN101898251A - Template-free method for realizing preparation of metalliccobalt nanowire - Google Patents
Template-free method for realizing preparation of metalliccobalt nanowire Download PDFInfo
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- CN101898251A CN101898251A CN 201010255509 CN201010255509A CN101898251A CN 101898251 A CN101898251 A CN 101898251A CN 201010255509 CN201010255509 CN 201010255509 CN 201010255509 A CN201010255509 A CN 201010255509A CN 101898251 A CN101898251 A CN 101898251A
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Abstract
The invention relates to a template-free method for realizing preparation of a metalliccobalt nanowire in the technical field of nano materials, which utilizes the induction of a magnetic field, takes the mixing solution of ethylene glycol or water and ethanol as solvent and divalent cobalt salt as major salt, utilizes the sodium hydroxide to regulate the pH value of the solution, takes hydrazine hydrate as reducing agent, and enables cobalt ions to grow into one-dimensional cobalt nanowire under the induction of the applied magnetic field. In the invention, the cheap and nontoxic chemical reagent and simple and feasible preparation process are adopted to prepare the one-dimensional cobalt nanowire under the induction of the magnetic field, and the method has low cost, no pollution, simple equipment and process condition and can realize mass preparation.
Description
Technical field
That the present invention relates to is a kind of preparation method of technical field of nano material, specifically is a kind of method that template realizes the metalliccobalt nanowire preparation of not having.
Background technology
The cobalt nano material has performances such as unique magnetic, light, electricity, catalysis, is mainly used in carbide alloy, battery, catalyst, permanent magnet and ceramic industry.The preparation of the more concern cobalts of early stage research nano-powder and in the application in fields such as catalyst, coating material and carbide alloy bonding agent.For example as the carbide alloy binding agent, super-fine cobalt powder can not only obtain high-quality carbide alloy, and can reduce the ball milling incorporation time in the process and reduce sintering temperature.In recent years, it is found that regularization of nanometer cobalt form is very big to the influence of its characterisitic parameter, the especially successful preparation of 1-dimention nano cobalt is further expanded its application.Optical property exploitation as the cobalt nano-tube array has the important use potentiality in fields such as Ultrahigh-Density Data Storage and biological anticancer medicines.
Performances such as the crystallite dimension of nano metal material, pattern, surface state and micro-structural directly have influence on the character and the purposes of nano metal.As particle diameter is that the nanometer cobalt of 7nm has the superparamagnetism characteristic, and particle diameter is that the nanometer cobalt of 60nm then has very high coercivity.The structure of present various nanostructureds is to all having higher requirement as pattern, structure and the size of the nanoparticle that makes up primitive, and therefore, pattern control, synthesis technique and the application study etc. of nano metal are present research focuses.Yet, because the restriction of conditions such as technology of preparing and technology, the pattern of nano metal material, size, structure etc. are carried out controlled preparation, and still there are a lot of problems in the aspects such as re-assemble of nano molecular structure, need further further investigation.At present, the ultra-fine cobalt nano magnetic material of China mainly relies on import, therefore, is necessary to develop the preparation method and the technology of the cobalt nano magnetic material with independent intellectual property right, thereby advances the development of China's nanometer cobalt technology.
The main preparation methods of cobalt nano material has high-pressure water spray method, precipitation reducing process, electrolysis, high-temperature cracking method, radiation method, reducing process etc. at present.One dimension cobalt preparation of nanomaterials has electro-deposition template, polyol reduction method, microemulsion method, hydrazine reducing process etc., can reduce hard template method and soft template method.
Find through retrieval prior art, Yang Peixia etc. have delivered " prepared by electrodeposition cobalt nanowire array in the ionic liquid " on 1501 pages to 1504 pages of " Chinese Journal of Inorganic Chemistry " 2007 the 9th phases, adopt hard template method to prepare cobalt nanowire, be specially: be equipped with porous alumina formwork with the anodic anodization legal system earlier, electro-deposition cobalt nanowire array in template obtains end product after the dissolving template then.There are many weak points in this method owing to adopt prefabricated hard template method, and is few such as the amount of early-stage preparations process complexity, experimental provision complexity, especially product, can not a large amount of preparations.
Further retrieval is found, and is relative with hard template method, adopts hole in the surfactant method for preparing nano material that leads mutually to be called soft template method.Qian Yitai etc. have delivered " Synthesis of ferromagnetic single-crystalline cobalt nanobelts via a surfactant-assisted hydrothermal reduction process " (the surfactant water thermal reduction prepares the magnetic mono crystal cobalt nanowire) on 2958 pages to 2962 pages of nanotechnology (nanometer technology) 2005 the 12nd phases, this article adopts the soft template method that adds surfactant SDBS (neopelex) to prepare the cobalt nano chain, its weak point is to react and must carries out in autoclave, and the reaction solution preparation is complicated, and product purity is lower.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of method that template realizes the metalliccobalt nanowire preparation of not having is provided, by adopting the chemical reagent of non-toxic inexpensive, simple preparation technology, preparation one dimension cobalt nano material under induced by magnetic field, the method cost is low, pollution-free, equipment and process conditions are simple, can realize a large amount of preparations.
The present invention is achieved by the following technical solutions, the present invention utilizes the inducing action in magnetic field, mixed solution with ethylene glycol or water and ethanol is a solvent, with divalent cobalt is main salt, with sodium hydrate regulator solution pH value, with the hydrazine hydrate is reducing agent, makes the cobalt ions reduction grow into the one dimension cobalt nanowire under the inducing of externally-applied magnetic field.
Described divalent cobalt is meant the CoSO of 0.005～0.3mol/L
4, Co (CH
3COO)
2, Co (NO
3)
2, and CoCl
2In any;
Described NaOH is meant the NaOH of 0.1～1mol/L
Described hydrazine hydrate is meant: weight percent concentration is the aqueous solution of 85% hydrazine hydrate;
The consumption of described reducing agent and the volume ratio of described solvent are 1: 0.1～1: 0.6;
Inducing of described externally-applied magnetic field is meant: 0.05～0.52T adds uniform magnetic field;
Described reduction growth is meant: reducing agent is added stir the back in the solvent that contains main salt be heated to 50～90 ℃ and reacted 15～120 minutes under the inducing of externally-applied magnetic field, obtain the one dimension cobalt nanowire through drying after the magnetic washing.
Described magnetic washing is meant: down auxiliary at permanent magnet, spend the deionised water cobalt nanowire earlier 2～3 times, and wash cobalt nanowire 2～3 times with absolute ethyl alcohol or acetone again;
Described drying is meant: following about 50 ℃ dry the collections or freeze-drying collection in freeze drier of vacuum.
Compared with prior art, the present invention does not need to prepare template in advance, and is reflected under the normal pressure and carries out, and equipment is simple, and technical process is simple, and the cycle is short, and preparation cost is low, can realize a large amount of preparations.Adopting the present invention can prepare diameter is 800～3044nm, and length can reach 15～80 μ m, and draw ratio is 10～81 cobalt nanowire.
Description of drawings
Fig. 1 is the cobalt nanowire SEM photo of embodiment 1 preparation.
The specific embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
1, the preparation of reaction precursor solution:
With ethylene glycol solution in following ratio obtain solution:
CoCl
2 0.01mol/L
NaOH 0.75mol/L
In the solution for preparing, added the aqueous solution of the hydrazine hydrate of 85% (w/w), stirring reaction under the room temperature, 5 minutes reaction time in 1: 0.1 by volume;
2, the preparation of cobalt nanowire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.4T;
2. be heated to 60 ℃;
3. react and finished until reaction in 60 minutes;
4. down auxiliary at permanent magnet, with deionized water and absolute ethyl alcohol or acetone washing cobalt nanowire;
5. following about 50 ℃ dry collections of vacuum, or freeze-drying collection in freeze drier.
Obtaining average length is 80 μ m, and average diameter is 980nm, and draw ratio is 81 cobalt nanowire.
Embodiment 2:
1, the preparation of reaction precursor solution:
With the mixed solution of water and ethanol in following ratio obtain solution:
Co(CH
3COO)
2 0.01mol/L
NaOH 0.75mol/L
In the solution for preparing, added the aqueous solution of the hydrazine hydrate of 85% (w/w), stirring reaction under the room temperature, 10 minutes reaction time in 1: 0.3 by volume;
2, the preparation of cobalt nanowire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.52T;
2. be heated to 90 ℃;
3. react and finished until reaction in 60 minutes;
4. down auxiliary at permanent magnet, with deionized water and absolute ethyl alcohol or acetone washing cobalt nanowire;
5. following about 50 ℃ dry collections of vacuum, or freeze-drying collection in freeze drier.
Obtaining average length is 44 μ m, and average diameter is 2405nm, and draw ratio is 18 cobalt nanowire.
Embodiment 3:
1, the preparation of reaction precursor solution:
With ethylene glycol solution in following ratio obtain solution:
Co(NO
3)
2 0.01mol/L
NaOH 0.8mol/L
In the solution for preparing, added the aqueous solution of the hydrazine hydrate of 85% (w/w), stirring reaction under the room temperature, 7 minutes reaction time in 1: 0.4 by volume;
2, the preparation of cobalt nanowire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.4T;
2. be heated to 60 ℃;
3. react and finished until reaction in 15 minutes;
4. down auxiliary at permanent magnet, with deionized water and absolute ethyl alcohol or acetone washing cobalt nanowire;
5. following about 50 ℃ dry collections of vacuum, or freeze-drying collection in freeze drier.
Obtaining average length is 15 μ m, and average diameter is 1534nm, and draw ratio is 10 cobalt nanowire.
Embodiment 4:
1, the preparation of reaction precursor solution:
With ethylene glycol solution in following ratio obtain solution:
CoSO
4 0.06mol/L
NaOH 0.5mol/L
In the solution for preparing, added the aqueous solution of the hydrazine hydrate of 85% (w/w), stirring reaction under the room temperature, 10 minutes reaction time in 1: 0.2 by volume;
2, the preparation of cobalt nanowire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.05T;
2. be heated to 50 ℃;
3. react and finished until reaction in 120 minutes;
4. down auxiliary at permanent magnet, with deionized water and absolute ethyl alcohol or acetone washing cobalt nanowire;
5. following about 50 ℃ dry collections of vacuum, or freeze-drying collection in freeze drier.
Obtaining average length is 60 μ m, and average diameter is 1045nm, and draw ratio is 57 cobalt nanowire.
Embodiment 5:
1, the preparation of reaction precursor solution:
With the mixed solution of water and ethanol in following ratio obtain solution:
CoCl
2 0.01mol/L
NaOH 0.75mol/L
In the solution for preparing, added the aqueous solution of the hydrazine hydrate of 85% (w/w), stirring reaction under the room temperature, 10 minutes reaction time in 1: 0.2 by volume;
2, the preparation of cobalt nanowire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.52T;
2. be heated to 60 ℃;
3. react and finished until reaction in 60 minutes;
4. down auxiliary at permanent magnet, with deionized water and absolute ethyl alcohol or acetone washing cobalt nanowire;
5. following about 50 ℃ dry collections of vacuum, or freeze-drying collection in freeze drier.
Obtaining average length is 69 μ m, and average diameter is 2.7 μ m, and draw ratio is 25 cobalt nanowire.
As shown in Figure 1, be the scanning electron microscope image of cobalt nanowire of preparation among the embodiment 1.Cobalt nanowire surface among the figure is comparatively level and smooth, and average length is 69 μ m, and average diameter is 980nm, and draw ratio is 81.
Claims (10)
1. one kind is not had the method that template realizes the metalliccobalt nanowire preparation, it is characterized in that, utilize the inducing action in magnetic field, mixed solution with ethylene glycol or water and ethanol is a solvent, with divalent cobalt is main salt, with sodium hydrate regulator solution pH value, be reducing agent with the hydrazine hydrate, under the inducing of externally-applied magnetic field, make the cobalt ions reduction grow into the one dimension cobalt nanowire.
2. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that described divalent cobalt is meant the CoSO of 0.005～0.3mol/L
4, Co (CH
3COO)
2, Co (NO
3)
2, and CoCl
2In any.
3. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that described NaOH is meant the NaOH of 0.1～1mol/L.
4. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that described hydrazine hydrate is meant: weight percent concentration is the aqueous solution of 85% hydrazine hydrate.
5. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that the consumption of described reducing agent and the volume ratio of described solvent are 1: 0.1～1: 0.6.
6. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that inducing of described externally-applied magnetic field is meant: 0.05～0.52T adds uniform magnetic field.
7. realize the method that metalliccobalt nanowire prepares according to claim 1 or 6 described no templates, it is characterized in that, described reduction growth is meant: reducing agent is added stir the back in the solvent that contains main salt be heated to 50～90 ℃ and reacted 15～120 minutes under the inducing of externally-applied magnetic field, obtain the one dimension cobalt nanowire through drying after the magnetic washing.
8. no template according to claim 7 realizes the method for metalliccobalt nanowire preparation, it is characterized in that, described magnetic washing is meant: down auxiliary at permanent magnet, spend the deionised water cobalt nanowire earlier 2～3 times, and wash cobalt nanowire 2～3 times with absolute ethyl alcohol or acetone again.
9. no template according to claim 1 realizes the method for metalliccobalt nanowire preparation, it is characterized in that described drying is meant: following about 50 ℃ dry the collections or freeze-drying collection in freeze drier of vacuum.
10. an one dimension cobalt nanowire is characterized in that, prepares by the described method of claim 1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102366832A (en) * | 2011-06-30 | 2012-03-07 | 燕山大学 | Preparation method of anisotropic samarium-cobalt/cobalt nano-composite magnet |
| CN102941355A (en) * | 2012-12-05 | 2013-02-27 | 大连理工大学 | Solvothermal preparation method of cobalt nano-fibers |
| CN103464775A (en) * | 2013-08-24 | 2013-12-25 | 四川大学 | Method for adopting magnetic-field self-assembling method to prepare cobalt nanowire |
| CN105947971A (en) * | 2016-05-26 | 2016-09-21 | 清华大学深圳研究生院 | Preparation method of ferromagnetic nanowire array |
| CN107322007A (en) * | 2017-08-21 | 2017-11-07 | 南京师范大学 | A kind of preparation method of ultra-fine overlength Au nano wires |
| CN111033659A (en) * | 2017-09-25 | 2020-04-17 | 国立大学法人千叶大学 | Porous conductor having conductive nanostructure, and electricity storage device using same |
| CN115058735A (en) * | 2022-07-08 | 2022-09-16 | 东北大学 | Porous catalyst with high hydrogen evolution performance by external magnetic field and preparation and use methods thereof |
| CN115213394A (en) * | 2022-07-25 | 2022-10-21 | 同济大学 | Strong magnet-based metal nanowire and preparation method and application thereof |
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| CN101342598A (en) * | 2008-08-28 | 2009-01-14 | 上海交通大学 | Method for preparing metallic nickel nano-wire |
| CN101698234A (en) * | 2009-10-21 | 2010-04-28 | 北京科技大学 | Chemical preparation method of metal cobalt nanowire |
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Cited By (14)
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|---|---|---|---|---|
| CN102366832B (en) * | 2011-06-30 | 2013-07-03 | 燕山大学 | Preparation method of anisotropic samarium-cobalt/cobalt nano-composite magnet |
| CN102366832A (en) * | 2011-06-30 | 2012-03-07 | 燕山大学 | Preparation method of anisotropic samarium-cobalt/cobalt nano-composite magnet |
| CN102941355A (en) * | 2012-12-05 | 2013-02-27 | 大连理工大学 | Solvothermal preparation method of cobalt nano-fibers |
| CN102941355B (en) * | 2012-12-05 | 2014-12-24 | 大连理工大学 | Solvothermal preparation method of cobalt nano-fibers |
| CN103464775A (en) * | 2013-08-24 | 2013-12-25 | 四川大学 | Method for adopting magnetic-field self-assembling method to prepare cobalt nanowire |
| CN105947971B (en) * | 2016-05-26 | 2017-11-10 | 清华大学深圳研究生院 | A kind of preparation method of Ferromagnetic Nanowire Arrays |
| CN105947971A (en) * | 2016-05-26 | 2016-09-21 | 清华大学深圳研究生院 | Preparation method of ferromagnetic nanowire array |
| CN107322007A (en) * | 2017-08-21 | 2017-11-07 | 南京师范大学 | A kind of preparation method of ultra-fine overlength Au nano wires |
| CN107322007B (en) * | 2017-08-21 | 2019-04-02 | 南京师范大学 | A kind of preparation method of ultra-fine overlength Au nano wire |
| CN111033659A (en) * | 2017-09-25 | 2020-04-17 | 国立大学法人千叶大学 | Porous conductor having conductive nanostructure, and electricity storage device using same |
| CN111033659B (en) * | 2017-09-25 | 2023-01-03 | 国立大学法人千叶大学 | Porous conductor having conductive nanostructure, and electricity storage device using same |
| CN115058735A (en) * | 2022-07-08 | 2022-09-16 | 东北大学 | Porous catalyst with high hydrogen evolution performance by external magnetic field and preparation and use methods thereof |
| CN115058735B (en) * | 2022-07-08 | 2024-02-27 | 东北大学 | Porous catalyst with high hydrogen evolution performance by externally applied magnetic field and preparation and use methods thereof |
| CN115213394A (en) * | 2022-07-25 | 2022-10-21 | 同济大学 | Strong magnet-based metal nanowire and preparation method and application thereof |
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Application publication date: 20101201 |