CN101928972B - Method for preparing nickel-polypyrrole double-layer nanowire array material - Google Patents
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- CN101928972B CN101928972B CN2010102349729A CN201010234972A CN101928972B CN 101928972 B CN101928972 B CN 101928972B CN 2010102349729 A CN2010102349729 A CN 2010102349729A CN 201010234972 A CN201010234972 A CN 201010234972A CN 101928972 B CN101928972 B CN 101928972B
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Abstract
The invention discloses a method for preparing a nickel-polypyrrole double-layer nanowire array material. The method comprises the following specific preparation processes of: 1) preparing an aluminum oxide template; 2) modifying the aluminum oxide template through voltage reduction; and 3) preparing a nickel-polypyrrole double-layer nanowire array through constant-voltage and direct-current electrodeposition by a double-tank method. In the method, on the basis of preparing the aluminum oxide template, the aluminum oxide template is subjected to voltage reduction modification by a continuous voltage reduction method, so that the template can be directly used for the electrodeposition of a two-electrode system, and the nickel-polypyrrole double-layer nanowire array is prepared by the double-tank method. The invention provides a method for preparing the nickel-polypyrrole double-layer nanowire array in the aluminum oxide template which is subjected to the continuous voltage reduction modification through the electrodeposition by two-electrode and double-tank methods, which simplifies the preparation process.
Description
Technical field
The present invention relates to a kind of preparation method of double-deck one-dimensional nano line array material, more particularly say, be meant a kind of preparation method of nickel-polypyrrole double-layer nanowire array material of high order.
Background technology
One dimension Nano structure has unique character such as electronics, optics and catalysis, makes them become the ideal material of nano surface engineering and constructing function nanostructure.At present, the monodimension nanometer material preparation method is a lot, and wherein template is occupied very consequence in the preparation of monodimension nanometer material, is the most directly method of preparation monodimension nanometer material, has advantages such as simple and generally suitable.Chang Yong template mainly contains alumina formwork and track etching polycarbonate template the most.
Because the existence of heterojunction structure has excellent physical properties in the multilayer monodimension nanometer material, the preparation of multilayer monodimension nanometer material has recently caused scientist's extensive concern, becomes the popular domain of investigation of materials.Zamborini[Aneta JMieszawska, Romaneh Jalilian, Gamini U.Sumanasekera, Francis P.Zamborini.Small 2007,3 (5) 722-756] etc. the people preparation of nano heterogeneous joint is summarized, mentioned the alumina formwork electro-deposition preparation method therein especially, and to adopting this method to prepare Ag, Pt, Pd, Fe, the preparation of the relevant multi-layer nano line with Ni of Co is illustrated.
Differing materials can be realized function diversification in conjunction with preparation multi-layer nano line structure, because coupling effect, the light of multi-layer nano line, electricity, magnetic property also can be further enhanced, and its excellent performance makes it be widely used in preparation of devices such as nano-sensor, nanometer transmission system, novel solar battery, nano electron device.In order to realize the application need development effectively economic assembling means of nano wire in nano-device, wherein the magnetic assembling is the assemble method of very attractive on the other hand.It is the necessary condition that realizes the magnetic assembling that preparation has magnetospheric multi-layer nano line structure.Consider the functionality advantage and the wide application prospect in relevant nano-device thereof of polypyrrole nano structure, about multi-layer nano line preparation causing investigator's the concern of polypyrrole and magneticmetal.People such as Vincent [Vincent Callegari.Sophie Demoustier-Champagne.Interfacing ConjugatedPolymers with Magnetic Nanowires[J] .Applied materials and interface, 2010,2 (5): 1369-1376] in the polycarbonate template of a metal spraying, utilized CHI660B type electrochemical workstation adopted three-electrode system prepared by electrodeposition Ni-PPy-Pt, Ni-PPy-Co multi-layer nano line.People [Mangesh A.Bangar such as Mangesh A.Bangar, Carlos M.Hangarter, Bongyoung Yoo, Youngwoo Rheem, Wilfred Chen, Ashok Mulchandani, Nosang V.Myunga.Magnetically assembled multisegmented nanowires and their applicaions[J] .Electroanalysis, 2008,1:1-7.] utilize alumina formwork to adopt direct current multiple-grooved method to prepare the Au-Ni-Ppy-Au nano thread structure.Polypyrrole section is strong for ammonia, hydrogen sulfide and carbon dioxide susceptibility, and the nickel section makes nano wire have ferromagnetic property.
Because alumina formwork and nuclear track etching polycarbonate template are all non-conductive, so need simultaneously take physical method such as magnetron sputtering at it when being used for prepared by electrodeposition, coating one deck precious metal such as thermal evaporation such as platinum, gold etc. make preparation process comparatively loaded down with trivial details and expensive as the electrodes conduct layer.What above listed document adopted all is these class methods.So need the new method of exploitation to make the more easy economy of preparation process.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nickel-polypyrrole double-layer nanowire array material, be characterized on the basis of two-step approach, taking the method for continuous step-down that alumina formwork is carried out the step-down modification, thereby make template can be directly used in two electrode system galvanic deposit, adopt double flute method dc electrodeposition to prepare nickel-polypyrrole double-layer nanowire array.Simplified preparation process, the method for a kind of employing two electrodes, double flute method prepared by electrodeposition nickel-polypyrrole double-layer nanowire array in the alumina formwork of step-down modification continuously is provided.
Technical scheme of the present invention is as follows:
1, the preparation of alumina formwork
The two-step approach preparation of alumina formwork can roughly be divided into two processes: the pre-treatment process and the anode oxidation process of sample.
The pre-treatment of aluminium foil: mainly comprise specimen surface degrease and high temperature annealing.The surface grease removal is that sample is immersed in the acetone, and the excusing from death ripple cleans 15～20min, uses washed with de-ionized water then; High temperature annealing is that sample is placed retort furnace, 500 ℃ of insulation 1.5h, and stove is chilled to room temperature, to eliminate the aluminum substrate internal stress, makes crystal grain be tending towards even; Take out afterwards, simultaneously coat chloroprene rubber, dry (24 hours) at aluminium foil.
Anodised process was divided into for three steps: anodic oxidation for the first time, nitration mixture is peeled off and anodic oxidation for the second time.
Anodic oxidation for the first time: as anode, as negative electrode, place the oxalic acid of 0.3mol/L with aluminium flake with aluminium foil, useful area is 30mm * 30mm, and at 25 ℃, anodic oxidation 3h under the situation of voltage 40V keeps magnetic agitation in the anode oxidation process.
Nitration mixture is peeled off: after will rinsing well with deionized water through the aluminium foil after the anodic oxidation, immerse massfraction and be 6% phosphoric acid and 1.8% chromic acid mixing solutions, and heating in water bath, temperature is controlled at 60 ℃, and reaction 3h is with complete molten deoxidation aluminium lamination.
Anodic oxidation for the second time: carry out the anodic oxidation second time on the aluminium foil of peeling off through nitration mixture, condition is with oxidizing condition is identical for the first time, and oxidization time is 3h.
2, the alumina formwork step-down is modified
After anodic oxidation is for the second time finished, keep other condition constant, reduce voltage significantly, be reduced to 2mA/cm until electric current
2, stop step-down, wait for after electric current is replied and repeat rapid depressurization again, reduce to 17V until voltage, reduce the step-down amplitude, change 1mA/cm with electric current
2Be unit, step-down is until dropping to required voltage (promptly can be used for prepared by electrodeposition below the 6v) one by one, but electric current is not less than 1mA/cm should guarantee that step-down is finished the time
2In the step-down modification along with the continuous reduction of oxidation voltage, the continuous attenuation of the thickness on blocking layer.Barrier layer thickness was enough little after modification was finished, and electronics can tunnel barriers under electric field action when carrying out galvanic deposit, thereby dc electrodeposition can directly be carried out.This step-down modification is to the almost not influence of alumina formwork of two-step anodization process of preparing.Alumina formwork can directly carry out dc electrodeposition after modifying, need not to carry out surperficial metal spraying and handle, and has reduced the loaded down with trivial details property of conventional dc electrodeposition experimentation greatly.
3, double flute method constant voltage dc electrodeposition prepares nickel-polypyrrole double-layer nanowire array
Nickel plating solution and plating polypyrrole solution are placed in two coating baths, and the template after earlier step-down being modified deposits 2min as negative electrode in nickel plating solution.Template after then step-down being modified deposits 2min as negative electrode in the polypyrrole electroplate liquid.For fear of the plating bath crossed contamination, template moved on to another coating bath from a coating bath before, rinse well with deionized water, and ultrasonic 5min.
When between two coating baths, shifting, need keep switch-on regime as the template after the step-down modification of negative electrode;
The correlation parameter of electric deposition nickel is: single nickel salts 160-240g/L, nickelous chloride 35g/L, boric acid 45g/L, sodium lauryl sulphate 0.05g/L, pH:3, temperature: 25～45 ℃, deposition voltage: step 2) adds 2～3V, anode on the voltage basis after step-down is finished: the nickel plate;
After the nickel plating, when carrying out the polypyrrole galvanic deposit, carry out the plating of big voltge surge earlier, promptly in step 2) add the strike plating that 5-7V voltage carries out extremely lack (5-6 second) on the voltage basis after step-down is finished, then voltage is dropped to required size and carry out normal electrical and deposit;
The correlation parameter of galvanic deposit polypyrrole is: pyrroles (py) 0.1mol/L, lithium perchlorate (LiClO
4) 0.2mol/L, ethanol volume fraction 75% aqueous solution, pH:5, temperature: 5 ℃, deposition voltage is a step 2) add 3～5V, anode on the voltage basis after step-down is finished: aluminium foil.
The invention has the advantages that: the easy manufacture that has realized nickel-polypyrrole double-layer nanowire array material.Provide after the alumina formwork process step-down modification, directly carried out the double flute of nickel-polypyrrole double-layer nanowire array, the technology of preparing of two electrode constant voltage dc electrodepositions without any processing.Two electrodes, the double flute method dc electrodeposition technology of preparing of directly carrying out nickel-polypyrrole double-layer nanowire array after this step-down is modified can realize simple, the preparation fast of such monodimension nanometer material (double-layer nanometer linear array).Saved alumina formwork is peeled off, drying is preserved pre-treatment, the processing of complicated and time consumption costlinesses such as metal spraying.
Description of drawings
Fig. 1 is the stereoscan photograph of the nickel-polypyrrole double-layer nanowire of embodiment 1 preparation;
Fig. 2 is the infrared spectrogram of the nickel-polypyrrole double-layer nanowire of embodiment 1 preparation;
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
1, the preparation of alumina formwork
The pre-treatment of aluminium foil: sample is immersed in the acetone, and the excusing from death ripple cleans 15～20min, uses washed with de-ionized water then; High temperature annealing is that sample is placed retort furnace, 500 ℃ of insulation 1.5h, and stove is chilled to room temperature, to eliminate the aluminum substrate internal stress, makes crystal grain be tending towards even; Take out afterwards, simultaneously coat chloroprene rubber, dry (24 hours) at aluminium foil.
Anodic oxidation for the first time: as anode, as negative electrode, place the oxalic acid of 0.3mol/L with aluminium flake with aluminium foil, useful area is 30mm * 30mm, and at 25 ℃, anodic oxidation 3h under the situation of voltage 40V keeps magnetic agitation in the anode oxidation process.
Nitration mixture is peeled off: after will rinsing well with deionized water through the aluminium foil after the anodic oxidation, immerse massfraction and be 6% phosphoric acid and 1.8% chromic acid mixing solutions, and heating in water bath, temperature is controlled at 60 ℃, and reaction 3h is with complete molten deoxidation aluminium lamination.
Anodic oxidation for the second time: carry out the anodic oxidation second time on the aluminium foil of peeling off through nitration mixture, condition is with oxidizing condition is identical for the first time, and oxidization time is 3h.
2, the alumina formwork step-down is modified
After anodic oxidation is for the second time finished, keep other condition constant, reduce voltage significantly, be reduced to 2mA/cm until electric current
2, stop step-down, wait for after electric current is replied and repeat rapid depressurization again, reduce to 17V until voltage, reduce the step-down amplitude, change 1mA/cm with electric current
2Be unit, step-down is until dropping to 3V one by one.
3, double flute method constant voltage dc electrodeposition nickel-polypyrrole double-layer nanowire array
Nickel plating solution and plating polypyrrole solution are placed in two coating baths, and the template after earlier step-down being modified deposits 2min as negative electrode in nickel plating solution.Template after then step-down being modified deposits 2min as negative electrode in the polypyrrole electroplate liquid.Before template moved on to another coating bath from a coating bath, rinse well with deionized water, and ultrasonic 5min.
The electrolytic solution of electric deposition nickel is: single nickel salts 160g/L, nickelous chloride 35g/L, boric acid 45g/L, sodium lauryl sulphate 0.05g/L; PH:3; Temperature: 25 ℃; Deposition voltage: 5V; Anode: nickel plate.
After the nickel plating, when carrying out the polypyrrole galvanic deposit, carry out big voltge surge earlier, adopt 10V voltage to carry out extremely lacking the strike plating of (5-6 second).The assurance polypyrrole is grown with promotion at nickel nano wire top forming core.Then voltage is dropped to required size and carry out the normal electrical deposition.
The galvanic deposit correlation parameter of polypyrrole section is as follows: pyrroles (py): 0.1mol/L, lithium perchlorate (LiClO
4): 0.2mol/L, ethanol volume fraction 75% aqueous solution; PH:2, temperature: 5 ℃, deposition voltage: 7V, anode: aluminium foil.
Embodiment 2
1, the preparation of alumina formwork
With embodiment 1.
2, the alumina formwork step-down is modified
After anodic oxidation is for the second time finished, keep other condition constant, reduce voltage significantly, be reduced to 2mA/cm until electric current
2, stop step-down, wait for after electric current is replied and repeat rapid depressurization again, reduce to 17V until voltage, reduce the step-down amplitude, change 1mA/cm with electric current
2Be unit, step-down is until dropping to 4V one by one.
3, double flute method constant voltage dc electrodeposition nickel-polypyrrole double-layer nanowire array
Nickel plating solution and plating polypyrrole solution are placed in two coating baths, and the template after earlier step-down being modified deposits 2min as negative electrode in nickel plating solution.Template after then step-down being modified deposits 2min as negative electrode in the polypyrrole electroplate liquid.Before template moved on to another coating bath from a coating bath, rinse well with deionized water, and ultrasonic 5min.
The electrolytic solution of electric deposition nickel is: single nickel salts 200g/L, nickelous chloride 35g/L, boric acid 45g/L, sodium lauryl sulphate 0.05g/L; PH:3; Temperature: 35 ℃; Deposition voltage: 6V; Anode: nickel plate.
When carrying out the polypyrrole galvanic deposit, carry out big voltge surge after the nickel plating earlier, adopt 10V voltage to carry out extremely lacking the strike plating of (5-6 second).The assurance polypyrrole is grown with promotion at nickel nano wire top forming core.Then voltage is dropped to required size and carry out the normal electrical deposition.
The galvanic deposit correlation parameter of polypyrrole section is as follows: pyrroles (py): 0.1mol/L, lithium perchlorate (LiClO
4): 0.2mol/L, ethanol volume fraction 75% aqueous solution, pH:2, temperature: 5 ℃, deposition voltage: 8V, anode: aluminium foil.
Embodiment 3
1, the preparation of alumina formwork
With embodiment 1.
2, the alumina formwork step-down is modified
After anodic oxidation is for the second time finished, keep other condition constant, reduce voltage significantly, be reduced to 2mA/cm until electric current
2, stop step-down, wait for after electric current is replied and repeat rapid depressurization again, reduce to 17V until voltage, reduce the step-down amplitude, change 1mA/cm with electric current
2Be unit, step-down is until dropping to 5V one by one.
3, double flute method constant voltage dc electrodeposition nickel-polypyrrole double-layer nanowire array
Nickel plating solution and plating polypyrrole solution are placed in two coating baths, and the template after earlier step-down being modified deposits 2min as negative electrode in nickel plating solution.Template after then step-down being modified deposits 2min as negative electrode in the polypyrrole electroplate liquid.For fear of the plating bath crossed contamination, template moved on to another coating bath from a coating bath before, rinse well with deionized water, and ultrasonic 5min.
The electrolytic solution of electric deposition nickel is: single nickel salts 240g/L, and nickelous chloride 35g/L, boric acid 45g/L, sodium lauryl sulphate 0.05g/L, pH:3, temperature: 45 ℃, deposition voltage: 6V, anode: nickel plate.
After the nickel plating, when carrying out the polypyrrole galvanic deposit, carry out big voltge surge earlier, adopt 11V voltage to carry out extremely lacking the strike plating of (5-6 second).The assurance polypyrrole is grown with promotion at nickel nano wire top forming core.Then voltage is dropped to required size and carry out the normal electrical deposition.
The galvanic deposit correlation parameter of polypyrrole section is as follows: pyrroles (py) 0.1mol/L, lithium perchlorate (LiClO
4) 0.2mol/L, ethanol volume fraction 75% aqueous solution, pH:2, temperature: 5 ℃, deposition voltage: 10V, anode: aluminium foil.
Claims (1)
1. the preparation method of a nickel-polypyrrole double-layer nanowire array material is characterized in that, concrete steps are as follows:
1) the two-step anodization method of alumina formwork preparation
The pre-treatment of aluminium foil: sample is immersed in the acetone, and ultrasonic cleaning 15～20min uses washed with de-ionized water then; High temperature annealing is that sample is placed retort furnace, 500 ℃ of insulation 1.5h, and stove is chilled to room temperature, to eliminate the aluminum substrate internal stress, makes crystal grain be tending towards even; Take out afterwards, simultaneously coat chloroprene rubber, dry at aluminium foil;
Anodic oxidation for the first time: as anode, as negative electrode, place the oxalic acid of 0.3mol/L with aluminium flake with aluminium foil, useful area is 30mm * 30mm, and at 25 ℃, anodic oxidation 3h under the situation of voltage 40V keeps magnetic agitation in the anode oxidation process;
Nitration mixture is peeled off: after will rinsing well with deionized water through the aluminium foil after the anodic oxidation, immerse massfraction and be 6% phosphoric acid and 1.8% chromic acid mixing solutions, and heating in water bath, temperature is controlled at 60 ℃, and reaction 3h is with complete molten deoxidation aluminium lamination;
Anodic oxidation for the second time: carry out the anodic oxidation second time on the aluminium foil of peeling off through nitration mixture, condition is with oxidizing condition is identical for the first time, and oxidization time is 3h;
2) the alumina formwork step-down is modified
After step 1) is finished, keep other condition constant, reduce voltage significantly, be reduced to 2mA/cm until electric current
2, stop step-down, wait for after electric current is replied and repeat rapid depressurization again, reduce to 17V until voltage, reduce the step-down amplitude, change 1mA/cm with electric current
2Be unit, be depressurized to one by one and be used for prepared by electrodeposition below the 6v, but electric current is not less than 1mA/cm should guarantee that step-down is finished the time
2
3) double flute method constant voltage dc electrodeposition prepares nickel-polypyrrole double-layer nanowire array
Nickel plating solution and plating polypyrrole solution are placed in two coating baths, template after earlier step-down being modified is as negative electrode, in nickel plating solution, deposit 2min, then in the polypyrrole electroplate liquid, deposit 2min, for fear of the plating bath crossed contamination, before template moved on to another coating bath from a coating bath, rinse well with deionized water, and ultrasonic 5min;
When between two coating baths, shifting, need keep switch-on regime as the template after the step-down modification of negative electrode;
The correlation parameter of electric deposition nickel is: single nickel salts 160-240g/L, nickelous chloride 35g/L, boric acid 45g/L, sodium lauryl sulphate 0.05g/L, pH:3, temperature: 25～45 ℃, deposition voltage: step 2) adds 2～3V, anode on the voltage basis after step-down is finished: the nickel plate;
After the nickel plating, when carrying out the polypyrrole galvanic deposit, carry out the plating of big voltge surge earlier, promptly in step 2) add 5-7V voltage on the voltage basis after step-down is finished and carry out the 5-6 strike plating of second, then voltage is dropped to required size and carry out the normal electrical deposition;
The correlation parameter of galvanic deposit polypyrrole is: pyrroles (py) 0.1mol/L, lithium perchlorate (LiClO
4) 0.2mol/L, ethanol volume fraction 75% aqueous solution, pH:5, temperature: 5 ℃, deposition voltage is a step 2) add 3～5V, anode on the voltage basis after step-down is finished: aluminium foil.
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| CN102675877B (en) * | 2011-03-18 | 2013-09-04 | 中国科学院合肥物质科学研究院 | Polypyrrole nanowire, and preparation method and usage thereof |
| CN104073857A (en) * | 2014-06-18 | 2014-10-01 | 华南理工大学 | Preparation method of nanoimprint nickel seal |
| 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 |
| CN116041778A (en) * | 2022-12-22 | 2023-05-02 | 之江实验室 | Ultrathin flexible conductive polymer hollow nano-column array, preparation method thereof and application thereof in mercury ion adsorption |
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| CN101016641A (en) * | 2006-12-31 | 2007-08-15 | 武汉大学 | Method of preparing three-dimensional aluminum oxide nano template by constant-current decompression |
| CN101139730A (en) * | 2007-06-12 | 2008-03-12 | 太原理工大学 | Strong anodic oxidation method for preparing porous pellumina |
| CN101498050A (en) * | 2009-01-16 | 2009-08-05 | 北京航空航天大学 | Preparation of nickel zinc alloy nano-wire array material |
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| CN101962792A (en) * | 2009-07-24 | 2011-02-02 | 中国科学院金属研究所 | Method for preparing pore diameter controllable through hole anodized aluminum oxide film |
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| CN101016641A (en) * | 2006-12-31 | 2007-08-15 | 武汉大学 | Method of preparing three-dimensional aluminum oxide nano template by constant-current decompression |
| CN101139730A (en) * | 2007-06-12 | 2008-03-12 | 太原理工大学 | Strong anodic oxidation method for preparing porous pellumina |
| CN101660188A (en) * | 2008-10-11 | 2010-03-03 | 大连海事大学 | Method for embedding nano metal at inside and surface of anodic oxide film hole of aluminum and alloy of aluminum |
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