CN101342598A - Method for preparing metallic nickel nano-wire - Google Patents
Method for preparing metallic nickel nano-wire Download PDFInfo
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- CN101342598A CN101342598A CNA2008100421664A CN200810042166A CN101342598A CN 101342598 A CN101342598 A CN 101342598A CN A2008100421664 A CNA2008100421664 A CN A2008100421664A CN 200810042166 A CN200810042166 A CN 200810042166A CN 101342598 A CN101342598 A CN 101342598A
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Abstract
The invention discloses a chemical preparation method of nickel nano-wire which belongs to the field of the nanometer technology. The invention utilizes the mixed solution of water and ethanol to prepare the nickel ion solution which reacts with sodium hydroxide solution to generate nickel hydroxide precipitation, then utilizes hydrazine hydrate to dissolve precipitation and reduces the nickel ion under the heating condition and in the applied uniform magnetic field, finally the nickel nano-wire is assembled. Compared with the prior art, using the invention can prepare the nickel nano-wire which is 217 to 1900 nanometer in diameter, 15 to 69 micrometer in length, 20 to 300 in length-diameter ratio and has the composition of pure nickel. The invention has the advantages that the beforehand preparation process of formwork is not required, the chemical process is simple, the preparation cycle is short, the preparation cost is low and the mass preparation can be realized.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of nano material, specifically, what relate to is a kind of chemical preparation process of metal nickel nano-line.
Background technology
The crystallite dimension of nano metal material and 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 nickel of 15nm has the superparamagnetism characteristic, and particle diameter is that the nanometer nickel of 85nm 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, the pattern control of nano metal is synthetic still to be in the starting stage with application study, and carrying out the preparation of the controlled nano metal material of pattern, size and structure and the re-assemble of nano molecular structure is the research focus of the present and the future's a period of time.There is abundant nickel resources in China, for making full use of resource, increases economic efficiency, and advances China's nanometer nickel Progress in technique, and the preparation research that carries out the controlled nanometer nickel of pattern, size and structure is significant.
The main method for preparing the metal nickel nano material has sol-gal process, electrochemical deposition method, chemical vapour deposition technique, chemical reduction method, hydrothermal reduction method, microemulsion method, radiation method etc. at present.And the method for traditional preparation process nickel nano wire is the porous alumina formwork method.Relative with hard template method, adopt lead the mutually method of growth of nano material of hole in the surfactant to be called soft template method.
Through the retrieval of prior art is found, " preparation and the hysteresis curve thereof of Ni nano-wire array in order " that Pan Gu equality was delivered on 675 pages to 679 pages of " Chinese Journal of Chemical Physics " 1999 the 6th phases.Propose to adopt hard template method to prepare the nickel nano wire in this article, be specially: prepare porous alumina formwork with anodizing earlier, then under direct current on template the nickel deposited nano-wire array, dissolve template then and obtain end product.This method is classified as hard template method owing to adopt prefabricated rigid template.Its deficiency is: early-stage preparations process complexity, the amount of experimental provision complexity, especially product is few, can not a large amount of preparations." Magneticnanochains of metal formed by assembly of small nanoparticles " (magnetic nano chain that little nano particle self assembly forms) that Liu Chengming etc. deliver in 2726 pages to 2727 pages of " Chemicalcommunications " (chemical communications) 2004, propose in this article to prepare the nickel nano chain with soft template method, its deficiency is that the reaction solution preparation is complicated, and controllable product shape is relatively poor.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of chemical preparation process of metal nickel nano-line is provided, adopt no template, prepare the nickel nano wire, can realize a large amount of preparations by induced by magnetic field.
The present invention is achieved by the following technical solutions, the present invention is an inducing action of utilizing magnetic field, is solvent with water and ethanol and mixed solution, is main salt with divalent nickel salt, with the hydrazine hydrate is reducing agent, nickel ion is reduced and assemble to form the nickel nano wire under the inducing that adds uniform magnetic field.
The inventive method comprises the steps:
The first step, the preparation of reaction precursor solution:
Mixed solution with water and ethanol is that solvent is in following ratio obtain solution.
Nickel salt 0.006～0.3mol/L
NaOH 0.1～1mol/L
The aqueous solution of 1: 0.2 by volume～1: 0.6 adding hydrazine hydrate in the solution for preparing, stirring reaction under the room temperature;
Described nickel salt can be NiSO
4, Ni (CH
3COO)
2, Ni (NO
3)
2, and NiCl
2In any.
The mixed solution of described water and ethanol, wherein water and ethanol mass ratio are 1: 0～19.
The aqueous solution of described hydrazine hydrate, its weight percent concentration are 85%.
Stirring reaction under the described room temperature, its reaction time is 5～10 minutes.
Second step, the preparation of nickel nano wire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.015～0.52T;
2. be heated to 50～85 ℃;
3. finish until reaction;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire earlier, again with absolute ethyl alcohol or acetone washing nickel nano wire;
6. dry the collection.
Second the step 3. in, described reaction, its time is 15～60 minutes.
Second step 5. in, spend deionised water nickel nano wire 2～3 times earlier, again with absolute ethyl alcohol or acetone washing nickel nano wire 2～3 times.
Compared with prior art, the present invention does not need to prepare template in advance, 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 91～1044nm, and length can reach 8.7～69 μ m, and draw ratio is 40～300 nickel nano wire.
Description of drawings
Fig. 1 is the nickel nano wire SEM photo of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of nickel nano wire.
The specific embodiment
Below in conjunction with accompanying drawing 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 water and 1: 1 mixed solution of ethanol mass ratio in following ratio obtain solution.
NiSO
4 0.006mol/L
NaOH 1mol/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: 0.6 by volume;
2, the preparation of nickel nano wire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.37T;
2. be heated to 50 ℃;
3. react and finished until reaction in 30 minutes;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire 2 times earlier, wash the nickel nano wire 2 times with absolute ethyl alcohol or acetone again;
6. dry the collection.
Obtaining average length is 69 μ m, and average diameter is 217nm, and draw ratio is 318 nickel nano powder.
Embodiment 2:
1, the preparation of reaction precursor solution:
With water and 1: 0 mixed solution of ethanol mass ratio in following ratio obtain solution.
Ni(CH
3COO)
2 0.006mol/L
NaOH 0.1mol/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: 0.6 by volume;
2, the preparation of nickel nano wire:
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 85 ℃;
3. react and finished until reaction in 60 minutes;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire 2 times earlier, wash the nickel nano wire 2 times with absolute ethyl alcohol or acetone again;
6. dry the collection.
Obtaining average length is 44 μ m, and average diameter is 724nm, and draw ratio is 61 nickel nano wire.
Embodiment 3:
1, the preparation of reaction precursor solution:
With water and 1: 1 mixed solution of ethanol mass ratio in following ratio obtain solution.
Ni(NO
3)
2 0.006mol/L
NaOH 1mol/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 nickel nano wire:
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 15 minutes;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire 3 times earlier, wash the nickel nano wire 3 times with absolute ethyl alcohol or acetone again;
6. dry the collection.
Obtaining average length is 15 μ m, and average diameter is 235nm, and draw ratio is 64 nickel nano wire.
Embodiment 4:
1, the preparation of reaction precursor solution:
With water and 1: 19 mixed solution of ethanol mass ratio in following ratio obtain solution.
NiCl
2 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 nickel nano wire:
The reaction precursor solution that 1. will prepare as stated above places the uniform magnetic field that adds of 0.015T;
2. be heated to 70 ℃;
3. react and finished until reaction in 30 minutes;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire 3 times earlier, wash the nickel nano wire 3 times with absolute ethyl alcohol or acetone again;
6. dry the collection.
Obtaining average length is 36 μ m, and average diameter is 641nm, and draw ratio is 56 nickel nano wire.
Embodiment 5:
1, the preparation of reaction precursor solution:
With water and 1: 1 mixed solution of ethanol mass ratio in following ratio obtain solution.
NiCl
2 0.3mol/L
NaOH 1mol/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 nickel nano wire:
The reaction precursor solution that 7. will prepare as stated above places the uniform magnetic field that adds of 0.015T;
8. be heated to 50 ℃;
9. react and finished until reaction in 30 minutes;
10. use magnetic field separation solution and nickel nano wire;
Obtaining average length is 40 μ m, and average diameter is 1.9 μ m, and draw ratio is 21 nickel nano wire.
Accompanying drawing 1 is the scanning electron microscope diagram of the nickel nano wire of preparation among the embodiment 1.Nickel nanowire surface among the figure is comparatively level and smooth, and average length is 69 μ m, and average diameter is 217nm, and draw ratio is 318.
Accompanying drawing 2 is X-ray diffraction (XRD) collection of illustrative plates of the nickel nano wire of preparation among the embodiment 1.Demonstrated diffraction maximum as we can see from the figure near the angle of diffraction is 45 °, 52 °, 76 °, these three peaks correspond respectively to the diffraction of 111,200 and 220 crystal faces of metallic nickel, with the indicated XRD data consistent of the powder diffraction card standard card of nickel.Thereby the composition that can confirm the product that obtains is a nickel.The broadening phenomenon has appearred in diffraction maximum simultaneously, can illustrate that prepared product crystallite dimension is in the nanoscale scope.Simultaneously in the collection of illustrative plates except the diffraction maximum of metallic nickel, do not find the diffraction maximum of the compound of other nickel, it can be said that in the bright course of reaction that because the existence of the hydrazine hydrate of excessive reproducibility, the nanometer nickel of generation can be not oxidized, can obtain pure nickel nano wire.
Claims (7)
1, a kind of chemical preparation process of metal nickel nano-line is characterized in that, comprises the steps:
The first step, the preparation of reaction precursor solution
With the mixed solution of water and ethanol is solvent in following ratio obtain solution:
Nickel salt 0.006～0.3mol/L
NaOH 0.1～1mol/L
The aqueous solution of 1: 0.2 by volume～1: 0.6 adding hydrazine hydrate in the solution for preparing, stirring reaction under the room temperature;
Second step, the preparation of nickel nano wire
1. the reaction precursor solution that the first step is prepared places the uniform magnetic field that adds of 0.015～0.52T;
2. be heated to 50～85 ℃;
3. finish until reaction;
4. use magnetic field separation solution and nickel nano wire;
5. spend deionised water nickel nano wire earlier, again with absolute ethyl alcohol or acetone washing nickel nano wire;
6. dry the collection.
2, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, in the first step, and the mixed solution of described water and ethanol, wherein water and ethanol mass ratio are 1: 0～19.
3, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, in the first step, described nickel salt is NiSO
4, Ni (CH
3COO)
2, Ni (NO
3)
2Or NiCl
2In any.
4, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, in the first step, and the aqueous solution of described hydrazine hydrate, its weight percent concentration is 85%.
5, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, in the first step, and stirring reaction under the described room temperature, its reaction time is 5～10 minutes.
6, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, second the step 3. in, described reaction, its time is 15～60 minutes.
7, the chemical preparation process of metal nickel nano-line as claimed in claim 1 is characterized in that, second step 5. in, spend deionised water nickel nano wire 2～3 times earlier, again with absolute ethyl alcohol or acetone washing nickel nano wire 2～3 times.
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|---|---|---|---|
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|---|---|---|---|
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| CN101871122A (en) * | 2010-06-10 | 2010-10-27 | 同济大学 | Preparation method of Pt-endpoint FeNi nano rod |
| CN101898251A (en) * | 2010-08-17 | 2010-12-01 | 上海交通大学 | Template-free method for realizing preparation of metalliccobalt nanowire |
| CN102145388A (en) * | 2011-03-25 | 2011-08-10 | 中北大学 | Method for synthesizing nano nickel powder at room temperature |
| CN102174709A (en) * | 2011-03-08 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Three-dimensional metallic nickel nano tapered body array structure and preparation method thereof |
| CN102605357A (en) * | 2012-03-23 | 2012-07-25 | 惠州学院 | Preparation method of magnetic metal or alloy film with nano-structure |
| CN102631924A (en) * | 2011-03-14 | 2012-08-15 | 江苏康恒化工有限公司 | Preparation method of o-phenylenediamine catalyst-nano nickel by hydrogenation |
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| CN101898251A (en) * | 2010-08-17 | 2010-12-01 | 上海交通大学 | Template-free method for realizing preparation of metalliccobalt nanowire |
| CN102174709A (en) * | 2011-03-08 | 2011-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Three-dimensional metallic nickel nano tapered body array structure and preparation method thereof |
| CN102174709B (en) * | 2011-03-08 | 2013-03-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Three-dimensional metallic nickel nano tapered body array structure and preparation method thereof |
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| CN102145388A (en) * | 2011-03-25 | 2011-08-10 | 中北大学 | Method for synthesizing nano nickel powder at room temperature |
| CN102605357A (en) * | 2012-03-23 | 2012-07-25 | 惠州学院 | Preparation method of magnetic metal or alloy film with nano-structure |
| CN103586479A (en) * | 2012-08-14 | 2014-02-19 | 南京大学 | Large-scale preparation method for precisely regulating and controlling sizes of nanocrystalline nickel wires |
| CN103170649A (en) * | 2013-04-15 | 2013-06-26 | 南京理工大学 | Preparation method of magnetic nickel nano material |
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| CN105522167A (en) * | 2015-12-28 | 2016-04-27 | 江苏理工学院 | Synthetic method for bead-like nickel microparticles |
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| CN105688914A (en) * | 2016-01-19 | 2016-06-22 | 上海交通大学 | Method for preparing recyclable nickel nanowire-cuprous oxide multiplex photo-catalyst |
| CN109732097A (en) * | 2018-12-14 | 2019-05-10 | 珠海启尼亚生物技术有限公司 | A kind of preparation method of the one-dimensional magnetic nano wire for biochemical analysis |
| CN109732097B (en) * | 2018-12-14 | 2021-11-16 | 珠海启尼亚生物技术有限公司 | Preparation method of one-dimensional magnetic nanowire for biochemical analysis |
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Open date: 20090114 |