CN102677115A - Multilayer nanowire and its preparation method by using anodic aluminum oxide template prepared by two-step anodic oxidation - Google Patents
Multilayer nanowire and its preparation method by using anodic aluminum oxide template prepared by two-step anodic oxidation Download PDFInfo
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Abstract
The invention relates to a multilayer nanowire and a preparation method of the multilayer nanowire by using anodic aluminum oxide template prepared by two-step anodic oxidation. The multilayer nanowire is [NiFe/Cu/Co/Cu]n, and has a diameter of 80-120nm. The NiFe layer and the Cu/Co/Cu layer are arranged alternately. The method includes performing potential-controlled electrodeposition by using double electrolytic cells and a three-electrode system; and placing an anodic aluminum oxide membrane electrode prepared by two-step anodic oxidation in a NiFe electrolytic cell, performing potential-controlled electrodeposition to obtain NiFe alloy, ultrasonically cleaning, rapidly transferring to a Cu/Co/Cu electrolytic cell, performing potential-controlled electrodeposition by double-pulsed technology to deposit Cu/Co/Cu, finishing a cycle, and repeating n cycles to obtain the final product. The prepared [NiFe/Cu/Co/Cu]n multilayer nanowire array has a controllable diameter and a controllable length. The method provided by the invention has characteristics of simple equipment and easy operation, and is carried out at a normal temperature and an atmospheric pressure, so that the production cost is low, and industrial production is easy to realize.
Description
Technical field
The invention belongs to the metal nano material field, particularly a kind of two-step anodization aluminum alloy pattern plate that utilizes prepares multi-layer nano line and method; With two-step anodization aluminium film (AAO) is template, through control sedimentation potential, galvanic deposit in two electrolyzers [NiFe/Cu/Co/Cu]
nMulti-layer nano line and preparation method.This method is cheap, and preparation is convenient, nanowire diameter homogeneous, controlled.
Background technology
At present; The technology that is used to prepare the nanometer multilayer line mainly contains molecular beam epitaxy, microlithography, nanometer planography, template etc.; The first three technology is complicated because of its required equipment, and factors such as working conditions harshness, preparation cost height are not that numerous researchists adopt, and consider from the angle of following commercial applications in addition; If new technology upgrading does not take place, these technology are difficult to be applied to commercially produce.And the equipment that the template electrochemical synthetic technology is adopted is simple, easy handling, and normal temperature and pressure can carry out, thereby production cost is low, is easy to realize suitability for industrialized production, is a kind of chemical process of preparation nanoscale material of exquisiteness.Anodised aluminium (Anodic Aluminum Oxide, AAO) pore size of template is controlled, and size is consistent, and cylinder hole is perpendicular to face, and is independent between the Kong Yukong, the staggered phenomenon of Kong Yukong do not occur, and hole is orderly columnar arrangement.Anodised aluminium porous-film (AAO) contains the cylindrical micropore of aperture basically identical, and needed nano wire is synthetic therein, is easy to collect, and adopts this method to synthesize polymkeric substance, metal, semi-conductor, carbon and other materials.
At present, both at home and abroad about [NiFe/Cu/Co/Cu]
nThe method of magnetron sputtering is adopted in the preparation of multi-layer nano line more, and this method needs protection of inert gas and under vacuum environment, operates, and has the instrument requirement height, shortcomings such as preparation cost height, and among the present invention [NiFe/Cu/Co/Cu]
nThe multi-layer nano line can be at room temperature environment, need not to prepare under the condition of gas shield, and preparation cost is low, and the multi-layer nano line of preparation has good giant magnetoresistance (GMR) effect, consults domestic literature at present, does not appear in the newspapers.Compare with multilayer film, the multi-layer nano line has much bigger resistance, and this just makes and utilizes general commercial measurement electric current to become possibility perpendicular to the giant magnetoresistance (CPP-GMR) of face.Multi-layer nano linear array great advantage is in room temperature with than just realizing the magnetic moment upset under the downfield; Thereby produce bigger magnetoelectricity resistance; Its GMR value will be much larger than the GMR value of multilayer film, thereby, at the high-density playback head; Magnetic resistance sensor, there is wide application prospect in fields such as magnetic RAM.
Summary of the invention
The object of the invention is exactly an AAO template of utilizing the preparation of secondary oxidation method, forms depositing time and sedimentation potential preparation [NiFe/Cu/Co/Cu] through the control plating bath
nThe multi-layer nano line.
Technical scheme of the present invention is following:
A kind of two-step anodization aluminum alloy pattern plate that utilizes prepares the multi-layer nano line, and its multi-layer nano line is [NiFe/Cu/Co/Cu]
nNiFe layer and Cu/Co/Cu layer alternately rearrange, and diameter is 80 ~ 120nm.
Preferred multi-layer nano line total length is 80nm ~ 20 μ m.
The preparation method of multi-layer nano line of the present invention adopts two electrolyzers, utilizes three-electrode system to carry out double flute control current potential deposition; Earlier the two-step anodization aluminum film electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy through ultrasonic cleaning, is converted in the Cu/Co/Cu electrolyzer fast, through two pulse technology control current potential deposition Cu/Co/Cu, is 1 cycle, so repeats a n cycle; Obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.The described n cycle is preferably 1 ~ 250.The experimental installation synoptic diagram is seen accompanying drawing 1.
Described three-electrode system is: supporting electrode is a ruthenium titanium net, and reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying.
The electrolytic solution of NiFe electrolyzer of the present invention is: NiSO
46H
2O 50 ~ 90g/L, NiCl
26H
2O60 ~ 100g/L, H
3BO
320 ~ 40g/L, FeSO
47H
2O 10 ~ 30g/L, C
6H
5Na
3O
72H
2O 40 ~ 60g/L, the pH value is 2.5～3.0.
The electrolytic solution of Cu/Co/Cu electrolyzer of the present invention is: CoSO
47H
2O 140 ~ 160g/L, CuSO
45H
2O 2 ~ 6g/L, H
3BO
330 ~ 50g/L, bath pH value are 4.5～5.0.
Said NiFe alloy electrodeposition current potential is-0.95 ~-1.1V, NiFe coating is formed by mass percentage: Ni 74 ~ 85%, Fe 15 ~ 26%; The galvanic deposit current potential of Cu is-0.4 ~-0.6V; The galvanic deposit current potential of Co is-0.8 ~-1.0V.
Two-step anodization aluminium film method for preparing template of the present invention: high-purity aluminium flake mechanical polishing, oil removing are placed in the oxalic acid solution of 3wt% anodic oxidation under 40V voltage; Sull, aluminum substrate is immersed in 5wt%H after peeling off
3PO
4Remove the blocking layer in the solution, obtain to connect the AAO film; , be fixed on the Cu sheet as conductive layer in the AAO film one side sputter layer of Au film that connects, process the AAO template.
Advantage of the present invention is:
(1) equipment that is adopted is simple, and easy handling carries out under normal temperature, normal pressure usually, thereby production cost is low, easy realization of industrial production.
(2) galvanic deposit can obtain good epitaxially grown layer on the part of big area and complicated shape.
(3) galvanic deposit is carried out usually at normal temperatures, thereby can avoid Yin Gaowen and the thermal stresses and the interlayer thermodiffusion that cause, thereby obtains the different individual layers of one-component.
(4) electrodeposition rate of metal is fast, can shorten the sample preparation time largely.
(5) the main impellent of electrodeposition process is a cathode overpotential, thereby is free to control thickness (from several atomic shells to several ten thousand atomic shells), and whole electrodeposition process is easy to realize computer control.
(6) use [NiFe/Cu/Co/Cu] that present method prepares
nMulti-layer nano linear array controllable diameter, nanowire length is controlled.
Description of drawings
Fig. 1: double flute method deposition [NiFe/Cu/Co/Cu] n multi-layer nano line three-electrode system synoptic diagram.
Fig. 2: AAO template surface pattern.
Fig. 3: AAO template cross-section morphology.
Fig. 4: [NiFe/Cu/Co/Cu]
nThe stereoscan photograph of multi-layer nano linear array.
Fig. 5: [NiFe/Cu/Co/Cu]
nThe projection electromicroscopic photograph of multi-layer nano line.
Fig. 6: [NiFe/Cu/Co/Cu]
nThe projection electromicroscopic photograph of multi-layer nano line.
The practical implementation method
Following instance is to think to illustrate the present invention better and do not limit the present invention.
Instance 1
Preparation [NiFe/Cu/Co/Cu]
nTwo-step anodization aluminium film (AAO) template of multi-layer nano line, except that the AAO template of commercially available perforation, also can be by following prepared: high-purity aluminium flake mechanical polishing, oil removing are placed in the oxalic acid solution of 3wt% anodic oxidation under 40V voltage; Sull, aluminum substrate is immersed in 5wt%H after peeling off
3PO
4Remove the blocking layer in the solution, obtain to connect the AAO film; , be fixed on the Cu sheet as conductive layer in the AAO film one side sputter layer of Au film that connects, process the AAO template.AAO template electrode all adopts this prepared in the instance 2～5.AAO template surface and cross-section morphology are seen accompanying drawing 2 and accompanying drawing 3.
With two-step anodization aluminium film (AAO) is template; (supporting electrode is a ruthenium titanium net to utilize electrochemical workstation and software kit to combine three-electrode system; Reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying) adopt two electrolyzers to control current potential deposition [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Earlier the AAO electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Be converted to fast in the Cu/Co/Cu electrolyzer, control current potential two pulse deposition techniques Cu/Co/Cu, this is 1 cycle; So repeat n cycle, can obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Cycle n is 1 in this instance.
Contain NiSO in the NiFe electrolyzer plating bath
46H
2O 50g/L; NiCl
26H
2O 60g/L; H
3BO
320g/L; FeSO
47H
2O 30g/L; Na
3C
6H
5O
72H
2O 40g/L; Bath pH value is 2.5, and bath temperature is 15 ℃.Contain CoSO in the Cu/Co/Cu electrolyzer plating bath
47H
2O 160g/L, CuSO
45H
2O 2g/L, H
3BO
330g/L, the pH value of solution value is 5.0, bath temperature is 15 ℃.
The sedimentation potential of NiFe alloy is-1.1V that depositing time is 12.8S; The Cu sedimentation potential is-0.5V that depositing time is 62.5S; The Co sedimentation potential is-0.95V that depositing time is 10.7S.
[NiFe/Cu/Co/Cu]
nMulti-layer nano line total length is 80nm.Wherein the quality percentage composition of Ni, Fe is respectively in the NiFe alloy: Ni 74%, Fe 26%.
Instance 2
With two-step anodization aluminium film (AAO) is template; (supporting electrode is a ruthenium titanium net to utilize electrochemical workstation and software kit control three-electrode system; Reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying) adopt two electrolyzers to control current potential deposition [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Earlier the AAO electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Be converted to fast in the Cu/Co/Cu electrolyzer, control current potential two pulse deposition techniques Cu/Co/Cu, this is 1 cycle; So repeat n cycle, can obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Cycle n is 175 in this instance.
Contain NiSO in the NiFe electrolyzer plating bath
46H
2O 75g/L; NiCl
26H
2O 75g/L; H
3BO
330g/L; FeSO
47H
2O 20g/L; Na
3C
6H
5O
72H
2O 48g/L; Bath pH value is 3, and bath temperature is 25 ℃.Contain CoSO in the Cu/Co/Cu electrolyzer plating bath
47H
2O 140g/L, CuSO
45H
2O 2.5g/L, H
3BO
330g/L, the pH value of solution value is 5.0, bath temperature is 25 ℃.
The sedimentation potential of NiFe alloy is-0.95V that depositing time is 12.8S; The Cu sedimentation potential is-0.5V that depositing time is 62.5S; The Co sedimentation potential is-0.95V that depositing time is 10.7S.
[NiFe/Cu/Co/Cu]
nMulti-layer nano line total length is 1.4 μ m.Wherein the quality percentage composition of Ni, Fe is respectively in the NiFe alloy: Ni 80%, Fe 20%.
Instance 3
With two-step anodization aluminium film (AAO) is template; (supporting electrode is a ruthenium titanium net to utilize electrochemical workstation and software kit control three-electrode system; Reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying) adopt two electrolyzers to control current potential deposition [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Earlier the AAO electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Be converted to fast in the Cu/Co/Cu electrolyzer, control current potential two pulse deposition techniques Cu/Co/Cu, this is 1 cycle; So repeat n cycle, can obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Cycle n is 250 in this instance.
Contain NiSO in the NiFe electrolyzer plating bath
46H
2O 90g/L; NiCl
26H
2O 100g/L; H
3BO
340g/L; FeSO
47H
2O 10g/L; Na
3C
6H
5O
72H
2O 60g/L; Bath pH value is 3, and bath temperature is 35 ℃.Contain CoSO in the Cu/Co/Cu electrolyzer plating bath
47H
2O 160g/L, CuSO
45H
2O 3.5g/L, H
3BO
330g/L, the pH value of solution value is 4.5, bath temperature is 35 ℃.
The sedimentation potential of NiFe alloy is-1.0V that depositing time is 12.8S; The Cu sedimentation potential is-0.5V that depositing time is 62.5S; The Co sedimentation potential is-0.95V that depositing time is 10.7S.
[NiFe/Cu/Co/Cu]
nMulti-layer nano line total length is 20 μ m.Wherein the quality percentage composition of Ni, Fe is respectively in the NiFe layer alloy: Ni 85%, Fe 15%.Gained [NiFe/Cu/Co/Cu]
nThe stereoscan photograph of multi-layer nano linear array is seen accompanying drawing 4, and the TEM photo of single multi-layer nano line is seen accompanying drawing 5 and Fig. 6.
Instance 4
With two-step anodization aluminium film (AAO) is template; (supporting electrode is a ruthenium titanium net to utilize electrochemical workstation and software kit control three-electrode system; Reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying) adopt two electrolyzers to control current potential deposition [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Earlier the AAO electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Be converted to fast in the Cu/Co/Cu electrolyzer, control current potential two pulse deposition techniques Cu/Co/Cu, this is 1 cycle; So repeat n cycle, can obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Cycle n is 12 in this instance.
Contain NiSO in the NiFe electrolyzer plating bath
46H
2O 75g/L; NiCl
26H
2O 75g/L; H
3BO
330g/L; FeSO
47H
2O 10g/L; Na
3C
6H
5O
72H
2O 42g/L; Bath pH value is 3, and bath temperature is 20 ℃.Contain CoSO in the Cu/Co/Cu electrolyzer plating bath
47H
2O 140g/L, CuSO
45H
2O 6g/L, H
3BO
340g/L, the pH value of solution value is 5.0, bath temperature is 20 ℃.
The sedimentation potential of NiFe alloy is-1.0V that depositing time is 12.8S; The Cu sedimentation potential is-0.5V that depositing time is 62.5S; The Co sedimentation potential is-0.95V that depositing time is 10.7S.
[NiFe/Cu/Co/Cu]
nMulti-layer nano line total length is 960nm.Wherein the quality percentage composition of Ni, Fe is respectively in the NiFe alloy: Ni 80%, Fe 20%.
Instance 5
With two-step anodization aluminium film (AAO) is template; (supporting electrode is a ruthenium titanium net to utilize electrochemical workstation and software kit control three-electrode system; Reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying) adopt two electrolyzers to control current potential deposition [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Earlier the AAO electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Be converted to fast in the Cu/Co/Cu electrolyzer, control current potential two pulse deposition techniques Cu/Co/Cu, this is 1 cycle; So repeat n cycle, can obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.Cycle n is 24 in this instance.
Contain NiSO in the NiFe electrolyzer plating bath
46H
2O 75g/L; NiCl
26H
2O 75g/L; H
3BO
330g/L; FeSO
47H
2O 10g/L; Na
3C
6H
5O
72H
2O 42g/L; Bath pH value is 3, and bath temperature is 30 ℃.Contain CoSO in the Cu/Co/Cu electrolyzer plating bath
47H
2O 160g/L, CuSO
45H
2O 2g/L, H
3BO
350g/L, the pH value of solution value is 5.0, bath temperature is 30 ℃.
The sedimentation potential of NiFe alloy is-1.1V that depositing time is 12.8S; The Cu sedimentation potential is-0.5V that depositing time is 62.5S; The Co sedimentation potential is-0.95V that depositing time is 10.7S.
[NiFe/Cu/Co/Cu]
nMulti-layer nano line total length is 1.92 μ m.Wherein the quality percentage composition of Ni, Fe is respectively in the NiFe alloy: Ni 80%, Fe 20%.
Claims (9)
1. one kind is utilized the two-step anodization aluminum alloy pattern plate to prepare the multi-layer nano line, it is characterized in that the multi-layer nano line is [NiFe/Cu/Co/Cu]
nNiFe layer and Cu/Co/Cu layer alternately rearrange; Diameter is 80 ~ 120nm.
2. multi-layer nano line as claimed in claim 1 is characterized in that multi-layer nano line total length is 80nm ~ 20 μ m.
3. the preparation method of the multi-layer nano line of claim 1 is characterized in that adopting two electrolyzers, utilizes three-electrode system to carry out double flute control current potential deposition; Earlier the two-step anodization aluminum film electrode is placed the NiFe electrolyzer, control current potential deposition NiFe alloy is through ultrasonic cleaning; Being converted to fast in the Cu/Co/Cu electrolyzer, through two pulse technology control current potential deposition Cu/Co/Cu, is 1 cycle; So repeat n cycle, obtain [NiFe/Cu/Co/Cu]
nThe multi-layer nano line.
4. method as claimed in claim 2 is characterized in that described cycle n is 1 ~ 250.
5. method as claimed in claim 2 is characterized in that described three-electrode system is: supporting electrode is a ruthenium titanium net, and reference electrode is SCE SCE, and working electrode is the two-step anodization aluminium film of bottom metal spraying.
6. method as claimed in claim 2 is characterized in that the electrolytic solution of NiFe electrolyzer is: NiSO
46H
2O 50 ~ 90g/L, NiCl
26H
2O 60 ~ 100g/L, H
3BO
320 ~ 40g/L, FeSO
47H
2O 10 ~ 30g/L, C
6H
5Na
3O
72H
2O40 ~ 60g/L, the pH value is 2.5～3.0.
7. method as claimed in claim 2 is characterized in that the electrolytic solution of Cu/Co/Cu electrolyzer is: CoSO
47H
2O140 ~ 160g/L, CuSO
45H
2O 2 ~ 6g/L, H
3BO
330 ~ 50g/L, bath pH value are 4.5～5.0.
8. method as claimed in claim 2, it is characterized in that said NiFe alloy electrodeposition current potential be-0.95 ~-1.1V, NiFe coating is formed by mass percentage: Ni 74 ~ 85%, Fe 15 ~ 26%; The galvanic deposit current potential of Cu is-0.4 ~-0.6V; The galvanic deposit current potential of Co is-0.8 ~-1.0V.
9. the method for claim 2: it is characterized in that two-step anodization aluminium film method for preparing template is: high-purity aluminium flake mechanical polishing, oil removing are placed in the oxalic acid solution of 3wt% anodic oxidation under 40V voltage; Sull, aluminum substrate is immersed in 5wt%H after peeling off
3PO
4Remove the blocking layer in the solution, obtain to connect the AAO film; , be fixed on the Cu sheet as conductive layer in the AAO film one side sputter layer of Au film that connects, process the AAO template.
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| CN103603004A (en) * | 2013-11-27 | 2014-02-26 | 天津大学 | Method for preparing CdS nanowires by using two-step anodized aluminum template |
| CN103614745A (en) * | 2013-12-05 | 2014-03-05 | 天津大学 | Method for preparing FeMn nanowires by utilizing secondary anodic alumina template |
| CN104089994A (en) * | 2014-01-07 | 2014-10-08 | 浙江工商大学 | Preparation method of ammonia sensor based on anodic alumina nanowire |
| CN104152958A (en) * | 2014-08-14 | 2014-11-19 | 天津大学 | Method for manufacturing multilayer nanowires by template electrochemical synthesis technology |
| CN104846411A (en) * | 2015-04-27 | 2015-08-19 | 北京航空航天大学 | Method for preparing flowerlike nanometer cobalt by using anodised aluminum template, and product of same |
| CN105483795A (en) * | 2016-01-21 | 2016-04-13 | 广州中国科学院先进技术研究所 | Method for preparing composite copper nanowire with underpotential deposition technology |
| CN105655143A (en) * | 2016-04-11 | 2016-06-08 | 中国工程物理研究院材料研究所 | Metal/amorphous nickel-cobalt hydroxide composite electrode for super capacitor and preparation method thereof |
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| CN103614745A (en) * | 2013-12-05 | 2014-03-05 | 天津大学 | Method for preparing FeMn nanowires by utilizing secondary anodic alumina template |
| CN104089994A (en) * | 2014-01-07 | 2014-10-08 | 浙江工商大学 | Preparation method of ammonia sensor based on anodic alumina nanowire |
| CN104152958A (en) * | 2014-08-14 | 2014-11-19 | 天津大学 | Method for manufacturing multilayer nanowires by template electrochemical synthesis technology |
| CN104846411A (en) * | 2015-04-27 | 2015-08-19 | 北京航空航天大学 | Method for preparing flowerlike nanometer cobalt by using anodised aluminum template, and product of same |
| CN104846411B (en) * | 2015-04-27 | 2017-08-25 | 北京航空航天大学 | The method and its product of flower-like nanometer metal cobalt are prepared using anodic oxidation aluminium formwork |
| CN105483795A (en) * | 2016-01-21 | 2016-04-13 | 广州中国科学院先进技术研究所 | Method for preparing composite copper nanowire with underpotential deposition technology |
| CN105655143A (en) * | 2016-04-11 | 2016-06-08 | 中国工程物理研究院材料研究所 | Metal/amorphous nickel-cobalt hydroxide composite electrode for super capacitor and preparation method thereof |
| CN105655143B (en) * | 2016-04-11 | 2018-08-14 | 中国工程物理研究院材料研究所 | A kind of preparation method of ultracapacitor metal/amorphous nickel cobalt hydroxide combination electrode |
| CN105967142A (en) * | 2016-04-27 | 2016-09-28 | 中国计量大学 | Multi-layer periodic nanowire array used for SERS substrate and manufacturing method thereof |
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