CN101498050B - Preparation of nickel zinc alloy nano-wire array material - Google Patents
Preparation of nickel zinc alloy nano-wire array material Download PDFInfo
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- CN101498050B CN101498050B CN200910076993XA CN200910076993A CN101498050B CN 101498050 B CN101498050 B CN 101498050B CN 200910076993X A CN200910076993X A CN 200910076993XA CN 200910076993 A CN200910076993 A CN 200910076993A CN 101498050 B CN101498050 B CN 101498050B
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Abstract
The invention discloses a method of preparing coronite nanometer wire array material, which comprises the following steps: 1, preparing an alumina template; 2, carrying out the depressed modification of the alumina template; and 3, carrying out the direct current sedimentation preparation of the coronite nanometer wire. The invention needs to curry out the depressed modification of the prepared alumina template, can directly carry out the direct current sedimentation preparation of the coronite nanometer wire after the modification and simplifies a preparation process. The method can control the structure of a coronite nanometer wire structure by controlling electrodeposit pressure and can control the coronite nanometer wire structure.
Description
Technical field
The present invention relates to a kind of preparation method of one-dimensional nano line array material, more particularly say, be meant a kind of nickel zinc alloy nano-wire array material preparation method.
Background technology
Nano material is because grain-size is little, specific area is big, quantum effect is obvious and the adjustability of surface microstructure on nanoscale, makes it have the excellent physical chemistry that is different from traditional material.Have broad application prospects in fields such as magneticsubstance, catalytic material, electrode materialss.
The research of monodimension nanometer material is the basis of other low-dimensional materials of research, and is closely related with nano electron device and microsensor again, is the forward position of studying both at home and abroad in recent years.Its preparation method mainly contains solution method, vapor phase process, template etc.Template prepares monodimension nanometer material and has advantages such as simple and generally suitable, is the most directly method of preparation monodimension nanometer material.Alumina formwork has that hole is arranged in order, hole density height, pore size distribution are wide, parameter is easy to advantages such as control, prepares in template to have obtained application widely in the monodimension nanometer material.
Because the dc electrodeposition template can be by the length of how much controlling prepared monodimension nanometer material of control metal deposition amount, simultaneously can be by control galvanic deposit parameter change nano material's structure, so the dc electrodeposition template has consequence in the preparation of monodimension nanometer material and performance study.
The method that present dc electrodeposition template prepares one-dimensional nano line array mainly comprises three processes: 1. the preparation of porous alumina formwork; 2. remove unoxidized aluminum substrate and blocking layer, spray the conductive metal layer in a side; With the alumina formwork of step 2 preparation as negative electrode, dc electrodeposition is realized the preparation of nano-wire array.The alumina formwork thickness of the through hole of using in this method preparation process is extremely thin, has only tens microns, and a little less than being highly brittle, it is improper a little to operate, and can cause film breaks.And in order to make the oxide film conduction, must deposit layer of conductive material, preparation process complex operation, cost are increased as electrode.
The compound of ferromagnetic metal and non-ferromagnetic metal can give material new magnetic behavior, and the structure of magneticsubstance also can influence the performance of material greatly.Nickel is ferromagnetic substance, and zinc is nonferromugnetic material, and nickel zinc alloy is expected to have the excellent magnetism performance." material engineering " 2008 (10): 158-160 report has been realized the preparation of nickel zinc alloy nano-wire array in the hole of alumina formwork.But alumina formwork need be made through hole and after a side sprays copper metal layer, realize galvanic deposit, and not have the research of nickel zinc alloy nano-wire structure and galvanic deposit voltage relationship.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nickel zinc alloy nano-wire array, be characterized in alumina formwork being carried out the step-down modification, modify the back and in single nickel salt and zinc sulfate are the plating bath of main salt, can directly realize the preparation of nickel zinc alloy nano-wire, can realize the control of nickel zinc nano thread structure by control galvanic deposit voltage.Simplified preparation process, the method for control nickel zinc alloy nano-wire structure is provided.
Technical scheme of the present invention is as follows:
1, the preparation of alumina formwork
Adopt the two-step anodization method to realize the preparation of alumina formwork, its preparation process is identical with common alumina formwork method.
2, the step-down of alumina formwork is modified
Alumina formwork is after two-step anodization is finished, and adjusting the anodic oxidation temperature is 30 ℃, keeps other anodic oxidation condition constant, with 2～3Vs
-1Velocity step ladder reduce anodic oxidation voltage, when voltage is reduced to less than 2.5V, stop step-down, the flushing.
3, the dc electrodeposition of nickel zinc alloy nano-wire preparation
The modification rear oxidation aluminum alloy pattern plate that obtains with step 2 is a negative electrode, and stereotype is an anode, realizes the prepared by electrodeposition of nickel zinc alloy nano-wire array in electroplate liquid with 35～45 ℃ of temperature ranges.
Consisting of of electroplate liquid wherein: zinc sulfate 70-150g/l, single nickel salt 140-210g/l, boric acid 40-55g/l, citric acid 15-25g/l, PH:1～3, galvanic deposit voltage: 3-6V.
The diameter of nickel zinc alloy nano-wire can be controlled by the aperture of controlled oxidation aluminum alloy pattern plate, the length of nano wire can be controlled by the control electrodeposition time, structure can be controlled by galvanic deposit voltage, when galvanic deposit voltage more than or equal to 5V during smaller or equal to 6V, the nickel zinc alloy nano-wire that generates is along nickel [111] preferred orientation, when galvanic deposit voltage more than or equal to 4V during less than 5V, the nickel zinc alloy nano-wire of generation is along zinc [101] preferred orientation.
The invention has the advantages that: realized the preparation of nickel zinc alloy nano-wire array.Alumina formwork is carried out step-down modify, modify nickel zinc alloy nano-wire can directly be realized in the back in single nickel salt and zinc sulfate are the plating bath of main salt preparation, simplified preparation process.The composition of alloy nano-wire can be controlled by the ratio of zinc sulfate in the electroplate liquid and single nickel salt.Can realize the control of nickel zinc nano thread structure by control galvanic deposit voltage, the method for control nickel zinc alloy nano-wire structure is provided.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the nickel zinc alloy nano-wire of embodiment 1 preparation;
Fig. 2 is the XRD spectra of the nickel zinc alloy nano-wire array of embodiment 1 preparation;
Fig. 3 is the stereoscan photograph of the nickel zinc alloy nano-wire of embodiment 2 preparations;
Fig. 4 is the XRD spectra of the nickel zinc alloy nano-wire array of embodiment 2 preparations;
Fig. 5 is the XRD spectra of the nickel zinc alloy nano-wire array of embodiment 3 preparations;
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1
1, the preparation of alumina formwork
With the pure aluminum foil anode, identical pure aluminum foil is a negative electrode, places the oxalic acid of 0.3mol/l, heating in water bath, and temperature is controlled at 25 ℃, voltage 40V, anodic oxidation 3h.After aluminium foil after the oxidation rinsed well with deionized water, immerse mass ratio and be 6% phosphoric acid and 1.8% chromic acid mixing solutions, heating in water bath, temperature is controlled at 60 ℃, to remove irregular aluminum oxide rete.Then carry out the anodic oxidation second time, condition is with oxidizing condition is identical for the first time.
2, the step-down of alumina formwork is modified
After step 1 was finished, adjusting the anodic oxidation temperature was 30 ℃, keeps other anodic oxidation condition constant, with 2Vs
-1Velocity step ladder reduce anodic oxidation voltage, when voltage is reduced to 2V, stop step-down, the flushing.
3, the dc electrodeposition of nickel zinc alloy nano-wire preparation
The modification rear oxidation aluminum alloy pattern plate that obtains with step 2 is a negative electrode, and stereotype is an anode, realizes the prepared by electrodeposition of nickel zinc alloy nano-wire array in electroplate liquid with 40 ℃ of temperature ranges.
Consisting of of electroplate liquid wherein: zinc sulfate 90g/l, single nickel salt 180g/l, boric acid 50g/l, citric acid 20g/l, PH:2, galvanic deposit voltage: 4V.
Obtain nickel zinc solid solution alloy nano-wire array, its transmission electron microscope photo as shown in Figure 1; Nano-wire array has along the orientation of zinc [101], and its XRD photo as shown in Figure 2.
Embodiment 2
1, the preparation of alumina formwork
Identical with embodiment 1 step 1.
2, the step-down of alumina formwork is modified
After step 1 was finished, adjusting the anodic oxidation temperature was 30 ℃, keeps other anodic oxidation condition constant, with 2Vs
-1Velocity step ladder reduce anodic oxidation voltage, when voltage is reduced to 2.5V, stop step-down, the flushing.
3, the dc electrodeposition of nickel zinc alloy nano-wire preparation
The modification rear oxidation aluminum alloy pattern plate that obtains with step 2 is a negative electrode, and stereotype is an anode, realizes the prepared by electrodeposition of nickel zinc alloy nano-wire array in electroplate liquid with 40 ℃ of temperature ranges.
Consisting of of electroplate liquid wherein: zinc sulfate 70g/l, single nickel salt 210g/l, boric acid 50g/l, citric acid 20g/l, PH:2.5, galvanic deposit voltage: 5V.
Obtain nickel zinc solid solution alloy nano-wire array, its stereoscan photograph as shown in Figure 3; Nano-wire array has along the orientation of nickel [111], and its XRD photo as shown in Figure 4.
Embodiment 3
1, the preparation of alumina formwork
Identical with embodiment 1 step 1.
2, the step-down of alumina formwork is modified
After step 1 was finished, adjusting the anodic oxidation temperature was 30 ℃, keeps other anodic oxidation condition constant, with 3Vs
-1Velocity step ladder reduce anodic oxidation voltage, when voltage is reduced to 2.5V, stop step-down, the flushing.
3, the dc electrodeposition of nickel zinc alloy nano-wire preparation
The modification rear oxidation aluminum alloy pattern plate that obtains with step 2 is a negative electrode, and stereotype is an anode, realizes the prepared by electrodeposition of nickel zinc alloy nano-wire array in electroplate liquid with 40 ℃ of temperature ranges.
Consisting of of electroplate liquid wherein: zinc sulfate 90g/l, single nickel salt 180g/l, boric acid 50g/l, citric acid 20g/l, PH:2.5, galvanic deposit voltage: 6V.
Obtain nickel zinc solid solution alloy nano-wire array, nano-wire array has along the orientation of nickel [111], and its XRD photo as shown in Figure 5.
Claims (3)
1. the preparation method of a nickel zinc alloy nano-wire array is characterized in that, concrete steps are as follows:
1) the two-step anodization method of alumina formwork preparation
With the pure aluminum foil is anode, and identical pure aluminum foil is a negative electrode, places the oxalic acid of 0.3mol/l, heating in water bath, temperature is controlled at 25 ℃, voltage 40V, anodic oxidation 3h, after aluminium foil after the oxidation rinsed well with deionized water, immerse mass ratio and be 6% phosphoric acid and mass ratio and be 1.8% chromic acid mixing solutions, heating in water bath, temperature is controlled at 60 ℃, to remove irregular aluminum oxide rete, then carry out the anodic oxidation second time;
2) step-down of alumina formwork is modified
After the alumina formwork preparation was finished, adjusting the anodic oxidation temperature was 30 ℃, keeps other anodic oxidation condition constant, with 2～3Vs
-1Velocity step ladder reduce anodic oxidation voltage, when voltage is reduced to less than 2.5V, stop step-down, the flushing;
3) dc electrodeposition of nickel zinc alloy nano-wire preparation
With step 2) the modification rear oxidation aluminum alloy pattern plate that obtains is negative electrode, stereotype is an anode, realizes the prepared by electrodeposition of nickel zinc alloy nano-wire arrays in electroplate liquid with 35～45 ℃ of temperature ranges;
Consisting of of electroplate liquid wherein: zinc sulfate 70-150g/l, single nickel salt 140-210g/l, boric acid 40-55g/l, citric acid 15-25g/l, PH:1～3, galvanic deposit voltage: 4-6V.
2. the preparation method of nickel zinc alloy nano-wire array as claimed in claim 1 is characterized in that: during smaller or equal to 6V, the nickel zinc alloy nano-wire of generation is along nickel [111] preferred orientation more than or equal to 5V for galvanic deposit voltage.
3. the preparation method of nickel zinc alloy nano-wire array as claimed in claim 1 is characterized in that: during less than 5V, the nickel zinc alloy nano-wire of generation is along zinc [101] preferred orientation more than or equal to 4V for galvanic deposit voltage.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102050423B (en) * | 2009-11-06 | 2013-04-03 | 国家纳米科学中心 | Nickel-bismuth hybridized nanowire and preparation method thereof |
| CN101928972B (en) * | 2010-07-23 | 2011-11-09 | 北京航空航天大学 | Method for preparing nickel-polypyrrole double-layer nanowire array material |
| CN102181928B (en) * | 2011-04-02 | 2012-08-01 | 河北师范大学 | Method for preparing ZnNi/Ni-ZnO nano-tube through direct current deposition |
| CN102732963B (en) * | 2011-04-15 | 2015-03-04 | 中国科学技术大学 | Preparation method of monocrystalline metal nanowire array based on alumina template |
| CN102650066A (en) * | 2012-05-17 | 2012-08-29 | 西安交通大学 | Method for preparing aluminum oxide template by step decompression reaming |
| CN102677115A (en) * | 2012-05-23 | 2012-09-19 | 天津大学 | Multilayer nanowire and its preparation method by using anodic aluminum oxide template prepared by two-step anodic oxidation |
| CN104073857A (en) * | 2014-06-18 | 2014-10-01 | 华南理工大学 | Preparation method of nanoimprint nickel seal |
| CN104562097B (en) * | 2015-01-23 | 2017-10-20 | 华南理工大学 | A kind of preparation method of self-supporting nickel nano tube/linear array film |
| CN106048673B (en) * | 2016-05-27 | 2018-04-20 | 河北工业大学 | A kind of Cr3The preparation method of Al nano wires |
| CN108103467A (en) * | 2017-12-25 | 2018-06-01 | 浙江工业大学 | The preparation method of one-dimensional diameter gradient Zn ferrite nano wire |
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Non-Patent Citations (5)
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| Adolphe Foyet等.Template electrochemical deposition and characterization of zinc–nickel alloy nanomaterial.Journal of Electroanalytical Chemistry.2007,604137-143. * |
| Lifeng Liu等.Structural, Magnetic, and Magnetoresistive Properties of Electrodeposited Ni5Zn21 Alloy Nanowires.J.Phys.Chem.B.2006,11020158-20165. * |
| YU Mei等.Electrochemical modification process of anodic alumina membrane.Trans.Nonferrous Met.SOC.China.2006,16s681-s684. * |
| 于美等.基于氧化铝模板直接电沉积法镍纳米线的制备与表征.中国有色金属学报.2007,17(5),727-731. * |
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