CN103464775A - Method for adopting magnetic-field self-assembling method to prepare cobalt nanowire - Google Patents
Method for adopting magnetic-field self-assembling method to prepare cobalt nanowire Download PDFInfo
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- CN103464775A CN103464775A CN2013103723370A CN201310372337A CN103464775A CN 103464775 A CN103464775 A CN 103464775A CN 2013103723370 A CN2013103723370 A CN 2013103723370A CN 201310372337 A CN201310372337 A CN 201310372337A CN 103464775 A CN103464775 A CN 103464775A
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Abstract
The invention discloses a chemical preparation method of a metal cobalt nanowire and relates to cobalt nanowire preparation, in particular to a method for adopting a magnetic-field self-assembling method to prepare the cobalt nanowire under the premise that no template is used. The method is characterized in that by utilizing constraint action of an applied magnetic field on magnetic cobalt particles, self-assembling is realized to enable the magnetic cobalt particles to grow in a uniquely-oriented manner, and the cobalt nanowire is prepared in a pure water phase. The diameter of the cobalt nanowire prepared by the method is 100-1000 nanometers, the length of the cobalt nanowire is 10.0-80.0 micrometers, the length-diameter ratio reaches 10-200, and the cobalt nanowire is composed of pure cobalt. The method has the advantages of needlessness of template pre-preparation, mild reaction condition, easy-to-get material, simple technological process and neat product shape.
Description
Technical field
The present invention relates to prepare the 1-dimention nano wire material with the magnetic field self-assembly method, particularly relate to the preparation of cobalt nanowire.
Background technology
One-dimensional nano line (rod) material is for nano-powder material, due to its particular geometric pattern, having the excellent properties such as mechanical strength as superelevation, thermoelectricity capability, luminous efficiency, catalytic performance, magnetic property, is an important field in nanoscale science and technology to the research of its preparation, character and application.
At present, the preparation method of metal cobalt nanowire is template.According to " Science " 2001,291:2115～2117 reports, adopting TOPO (TOPO) and oleic acid intermixture is surfactant (soft template), o-dichlorohenzene is solvent, at 182 ℃ of lower thermal decomposition Co
2(CO)
8prepare cobalt nanorod, its diameter is 4～25nm.Raw material TOPO and Co that the method is used
2(CO)
8comparatively expensive, and reaction temperature is higher, has limited its suitability for industrialized production and application.According to " SCI " 2006,27:1708～1710; " Nanjing University of Chemical Technology's journal " 2000,22:69～71; " Chinese Journal of Inorganic Chemistry " 2007,23:1501～1504 reports such as paper such as grade, all adopt electrodepositing in porous alumina template to prepare cobalt nanowire.The defect of this class methods maximum is that preparation process complexity and the product later stage of template is comparatively difficult with separating of template, has limited its practical application.In the Chinese invention patent that is CN101698234A at publication number, the employing ethylene glycol such as the grandson of University of Science & Technology, Beijing winter sun and surfactant form soft template jointly, make the cobalt nucleus oriented growth that is reduced out in solution, obtain the cobalt nanowire of wire.The deficiency of the method is that the reaction solution preparation is comparatively complicated, product pattern regularity is poor.And there is not yet report both at home and abroad, there is the simple liquid phase chemical reduction method of employing to prepare cobalt nanowire under the prerequisite without template.
Summary of the invention
The object of the present invention is to provide a kind of magnetic field self-assembly method that adopts to prepare the method for cobalt nanowire under the prerequisite without template, be characterized in utilizing the effect of contraction of externally-applied magnetic field to the magnetic cobalt granule, realize self assembly, make its one dimension oriented growth, prepare cobalt nanowire at pure water in mutually, have advantages of without previously prepared template, reaction condition is gentle, raw material is easy to get, technical process is simple, the product pattern is regular.
Implementation process of the present invention is as follows:
1. the preparation of reaction initial soln
Using deionized water as solvent, by concentration of cobalt ions 0.01～0.3 molL
-1, complexing agent concentration 0.01～0.3molL
-1obtain solution, fully mix rear with NaOH solution regulator solution pH value to 9～13.
Wherein cobalt ions is by cobalt salt CoCl
2, CoSO
4or Co (NO
3)
2among one or more mixture provide.
Wherein complexing agent is the EDTA(ethylenediamine tetra-acetic acid), the EDTA-2Na(disodium ethylene diamine tetraacetate), the EDTA-4Na(tetrasodium ethylenediamine tetraacetate), one or more the mixture among trisodium citrate, sodium tartrate.
2. the preparation of cobalt nanowire
The reaction initial soln prepared as stated above is placed in to additional uniform magnetic field, is heated to 50～100 ℃, add reducing agent, react 30～90 minutes; To reacting complete, with permanent magnet or centrifuge separation solution and cobalt nanowire, wash successively cobalt nanowire 2 times with deionized water, absolute ethyl alcohol and acetone respectively, vacuum drying, collect product.
Wherein the intensity of externally-applied magnetic field is 5～500mT.
Wherein reducing agent is one or more the mixture in hydrazine hydrate, sodium borohydride or inferior sodium phosphate.
Wherein the consumption of reducing agent is to be 1:3～5:1 with the mol ratio of cobalt ions.
Compared with prior art, the present invention, without previously prepared template, reaction condition are gentle, raw material is easy to get, technical process is simple, the product pattern is regular, can realize a large amount of preparations.The cobalt nanowire diameter that adopts the present invention to prepare is 100～1000nm, and length is 10.0～80.0 μ m, and draw ratio reaches 10～200.
The accompanying drawing explanation
The cobalt nanowire SEM photo that Fig. 1 is embodiment 1 preparation (low multiplication factor)
The cobalt nanowire SEM photo (than high-amplification-factor) that Fig. 2 is embodiment 1 preparation
The product XRD collection of illustrative plates that Fig. 3 is embodiment 1 preparation.
The specific embodiment
The present embodiment be take technical solution of the present invention and is implemented as prerequisite, 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 initial soln
By 4.76g CoCl
26H
2o is dissolved in 200 mL deionized waters, adds 7.44g EDTA-2Na, fully mixes rear 0.5 molL that uses
-1naOH solution regulator solution pH value to 12.
2. the preparation of cobalt nanowire
The reaction initial soln prepared as stated above is placed in to the additional uniform magnetic field of 25mT, heating water bath to 70 ℃, add the hydrazine hydrate 6mL that content is 80%, reacts 60 minutes; To reacting complete, with permanent magnet separation solution and cobalt nanowire, wash successively cobalt nanowire 2 times with deionized water, absolute ethyl alcohol and acetone respectively, 50 ℃ of vacuum drying, collect product.
The acquisition average diameter is 500nm, and average length is 40 μ m, the cobalt nanowire that draw ratio is 80.Its pattern is shown in accompanying drawing 1.Its constituent analysis the results are shown in accompanying drawing 2, is pure cobalt.
Embodiment 2:
1. the preparation of reaction initial soln
By 5.62g CoSO
47H
2o is dissolved in 200 mL deionized waters, adds the 8.82g trisodium citrate, fully mixes rear 0.5 molL that uses
-1naOH solution regulator solution pH value to 10.
2. the preparation of cobalt nanowire
The reaction initial soln prepared as stated above is placed in to the additional uniform magnetic field of 50mT, heating water bath to 60 ℃, add inferior sodium phosphate 4.30g, reacts 45 minutes; To reacting complete, with centrifuge separation solution and cobalt nanowire, wash successively cobalt nanowire 2 times with deionized water, absolute ethyl alcohol and acetone respectively, 50 ℃ of vacuum drying, collect product.
Embodiment 3:
1. the preparation of reaction initial soln
By 7.14g CoCl
26H
2o is dissolved in 200 mL deionized waters, adds 7.45g EDTA-2Na and 5.88g sodium tartrate, fully mixes rear 1 molL that uses
-1naOH solution regulator solution pH value to 12.
2. the preparation of cobalt nanowire
The reaction initial soln prepared as stated above is placed in to the additional uniform magnetic field of 75mT, heating water bath to 50 ℃, add hydrazine hydrate 4mL and sodium borohydride 0.76g that content is 80%, reacts 40 minutes; To reacting complete, with permanent magnet separation solution and cobalt nanowire, water, absolute ethyl alcohol and acetone wash cobalt nanowire 2 times successively, and product is collected in 50 ℃ of vacuum drying.
Embodiment 4:
1. the preparation of reaction initial soln
By 7.14g CoCl
26H
2o is dissolved in 200 mL deionized waters, adds 11.40g EDTA-4Na, fully mixes rear 1 molL that uses
-1naOH solution regulator solution pH value to 10.
2. the preparation of cobalt nanowire
The reaction initial soln prepared as stated above is placed in to the additional uniform magnetic field of 150mT, heating water bath to 50 ℃, add sodium borohydride 2.28g, reacts 30 minutes; To reacting complete, with permanent magnet separation solution and cobalt nanowire, water, absolute ethyl alcohol and acetone wash cobalt nanowire 2 times successively, and product is collected in 50 ℃ of vacuum drying.
The cobalt nanowire SEM photo that accompanying drawing 1 is embodiment 1 preparation (low multiplication factor), the cobalt nanowire SEM photo (than high-amplification-factor) that accompanying drawing 2 is embodiment 1 preparation.Cobalt nanowire pattern in figure is regular, and average diameter is 500nm, and average length is 40 μ m, and draw ratio is 80.
The product XRD collection of illustrative plates that accompanying drawing 3 is embodiment 1 preparation.The diffraction maximum occurred in figure, with the indicated XRD data consistent of the powder diffraction standard card of cobalt, the composition that the product obtained is described is metallic cobalt.
Claims (6)
1. the chemical preparation process of a metal cobalt nanowire, is characterized in that, concrete steps are:
Using deionized water as solvent, by concentration of cobalt ions 0.01～0.3 molL
-1, complexing agent concentration 0.01～0.3molL
-1obtain solution, fully mix rear with NaOH solution regulator solution pH value to 9～13; The reaction initial soln prepared as stated above is placed in additional uniform magnetic field, is heated to 50～100 ℃, adds reducing agent, reacts 30～90 minutes; To reacting complete, with permanent magnet or centrifuge separation solution and cobalt nanowire, wash successively cobalt nanowire 2 times with deionized water, absolute ethyl alcohol and acetone respectively, vacuum drying, collect product.
2. preparation method as claimed in claim 1, is characterized in that, described cobalt ions is by cobalt salt CoCl
2, CoSO
4or Co (NO
3)
2among one or more mixture provide.
3. preparation method as claimed in claim 1, it is characterized in that, described complexing agent is the EDTA(ethylenediamine tetra-acetic acid), the EDTA-2Na(disodium ethylene diamine tetraacetate), the EDTA-4Na(tetrasodium ethylenediamine tetraacetate), one or more the mixture among trisodium citrate, sodium tartrate.
4. preparation method as claimed in claim 1, is characterized in that, the magnetic field intensity of described externally-applied magnetic field is 5～500mT.
5. preparation method as claimed in claim 1, is characterized in that, described reducing agent is one or more the mixture in hydrazine hydrate, sodium borohydride or inferior sodium phosphate.
6. preparation method as claimed in claim 5, is characterized in that, the consumption of described reducing agent is to be 1:3～5:1 with the mol ratio of cobalt ions.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105598469A (en) * | 2016-03-18 | 2016-05-25 | 西北师范大学 | Preparation method of transition metal alloy material of ordered controllable three-dimensional grading structure |
| CN105947971A (en) * | 2016-05-26 | 2016-09-21 | 清华大学深圳研究生院 | Preparation method of ferromagnetic nanowire array |
| WO2017107999A1 (en) * | 2015-12-25 | 2017-06-29 | 李�浩 | Method for preparing copper oxide nanowire |
| CN106966439A (en) * | 2017-03-15 | 2017-07-21 | 四川大学 | A kind of preparation method of battery electrode cobaltosic oxide nano line |
| CN107201600A (en) * | 2017-07-19 | 2017-09-26 | 清华大学深圳研究生院 | A kind of non-woven fabrics and preparation method thereof |
| CN110218345A (en) * | 2019-05-08 | 2019-09-10 | 广东石油化工学院 | A kind of flexible extensible electromagnetic wave shield film and preparation method thereof |
| CN110449597A (en) * | 2019-09-06 | 2019-11-15 | 哈尔滨工业大学 | A kind of chain Fe nanowire and preparation method thereof |
| CN110976898A (en) * | 2019-12-12 | 2020-04-10 | 沈阳工业大学 | Soft magnetic metal iron porous micron wire and preparation method thereof |
| CN111729132A (en) * | 2020-06-18 | 2020-10-02 | 四川大学 | Polyether-ether-ketone bone repair material with antibacterial property and preparation method thereof |
| CN114905049A (en) * | 2022-05-11 | 2022-08-16 | 江南大学 | Chiral cobalt super particle and preparation method 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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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017107999A1 (en) * | 2015-12-25 | 2017-06-29 | 李�浩 | Method for preparing copper oxide nanowire |
| CN105598469A (en) * | 2016-03-18 | 2016-05-25 | 西北师范大学 | Preparation method of transition metal alloy material of ordered controllable three-dimensional grading structure |
| 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 |
| CN106966439A (en) * | 2017-03-15 | 2017-07-21 | 四川大学 | A kind of preparation method of battery electrode cobaltosic oxide nano line |
| CN107201600B (en) * | 2017-07-19 | 2019-07-05 | 清华大学深圳研究生院 | A kind of non-woven fabrics and preparation method thereof |
| CN107201600A (en) * | 2017-07-19 | 2017-09-26 | 清华大学深圳研究生院 | A kind of non-woven fabrics and preparation method thereof |
| CN110218345A (en) * | 2019-05-08 | 2019-09-10 | 广东石油化工学院 | A kind of flexible extensible electromagnetic wave shield film and preparation method thereof |
| CN110218345B (en) * | 2019-05-08 | 2021-12-24 | 广东石油化工学院 | Flexible stretchable electromagnetic shielding film and preparation method thereof |
| CN110449597A (en) * | 2019-09-06 | 2019-11-15 | 哈尔滨工业大学 | A kind of chain Fe nanowire and preparation method thereof |
| CN110976898A (en) * | 2019-12-12 | 2020-04-10 | 沈阳工业大学 | Soft magnetic metal iron porous micron wire and preparation method thereof |
| CN111729132A (en) * | 2020-06-18 | 2020-10-02 | 四川大学 | Polyether-ether-ketone bone repair material with antibacterial property and preparation method thereof |
| CN111729132B (en) * | 2020-06-18 | 2021-06-29 | 四川大学 | Polyether-ether-ketone bone repair material with antibacterial property and preparation method thereof |
| CN114905049A (en) * | 2022-05-11 | 2022-08-16 | 江南大学 | Chiral cobalt super particle and preparation method 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: 20131225 |