CN105603469A - CuO/Ni core-shell nanowire and preparation method thereof - Google Patents

CuO/Ni core-shell nanowire and preparation method thereof Download PDF

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Publication number
CN105603469A
CN105603469A CN201510977753.2A CN201510977753A CN105603469A CN 105603469 A CN105603469 A CN 105603469A CN 201510977753 A CN201510977753 A CN 201510977753A CN 105603469 A CN105603469 A CN 105603469A
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cuo
nano
preparation
core
wire array
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CN105603469B (en
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杨峰
陈雷
崔立山
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • C25D1/006Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • C25D1/04Wires; Strips; Foils

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Abstract

The invention provides a CuO/Ni core-shell nanowire and a preparation method thereof. According to the preparation method, an AOO (anodic aluminum oxide) template is taken as a cathode, a carbon rod is taken as an anode, copper nanowire arrays are deposited in the AOO template with an electrochemical deposition method and then soaked in a phosphoric acid solution for pore expansion, thermal treatment is also performed, nickel nanowire arrays are deposited on the treated template, the AOO template containing the nickel nanowire arrays and the CuO nanowire arrays is obtained, finally, the AOO template is soaked in a sodium hydroxide solution, an aluminum oxide template is removed, and the CuO/Ni core-shell nanowire is obtained after ethanol cleaning and infrared drying. The preparation method adopts a simple process and can realize mass production, the cost is low, and the prepared CuO/Ni core-shell nanowire can be 25 mu m long.

Description

A kind of CuO/Ni core-shell nano line and preparation method thereof
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of CuO/Ni core-shell nano line and preparation method thereof.
Background technology
Core-shell nano line is due to unique physical and chemical performance, solar cell, photocatalysis, nano electron device,The aspects such as magnetic storage apparatus have wide practical use, and how preparing core-shell nano line becomes people's study hotspot.
The method of preparing at present core-shell nano line has hydrothermal synthesis method, electron beam epitaxial growth method, physical sputtering method, gasPhase sedimentation etc. These methods are used to extensively prepare the core-shell nano such as metal/metal, semiconductor/metal line, and oxygenThe rarely found report of compound/metal nucleocapsid nano wire.
Summary of the invention
In order to solve the problems of the technologies described above, the object of the present invention is to provide a kind of CuO/Ni core-shell nano line and system thereofPreparation Method, this preparation method has that technique is simple, cost is low, can produce in a large number the CuO/Ni nucleocapsid preparingThe length of nano wire can reach 25 μ m.
Object of the present invention is achieved by the following technical programs:
A preparation method for CuO/Ni core-shell nano line, comprises the following steps:
(1), taking anodised aluminium (AOO) template as negative electrode, carbon-point are as anode, adopt electrochemical deposition method at sunDeposited copper nano-wire array in utmost point alumina formwork;
(2) anodic oxidation aluminium formwork that contains Arrays of Copper Nanowires step (1) being obtained immerses in phosphoric acid solutionRow reaming 10-40min, the template after reaming is positioned in the heat-treatment furnace of 60-150 DEG C and processes 1-2h, is containedThe anodic oxidation aluminium formwork of CuO nano-wire array;
(3) utilize electrochemical deposition method, nickel deposited in the anodic oxidation aluminium formwork that contains CuO nano-wire arrayNano-wire array, obtains the anodic oxidation aluminium formwork that contains nickel nano-wire array and contain CuO nano-wire array;
(4) anodic oxidation that contains nickel nano-wire array and contain CuO nano-wire array step (3) being obtainedAluminum alloy pattern plate immerses in sodium hydroxide solution, removes alumina formwork, in ethanol, cleans, and utilizes infrared lamp to dry,Thereby obtain CuO/Ni core-shell nano line.
In above-mentioned preparation method, preferably, in described step (1), before depositing, first antianode oxidationAluminum alloy pattern plate carries out pretreatment, and described pretreatment is to utilize the method for magnetron sputtering thick at its back spatter one deck 200nmThe Ag layer of degree is as conductive electrode.
In above-mentioned preparation method, preferably, in step (1), the pore size of described anodic oxidation aluminium formwork is20-80nm。
In above-mentioned preparation method, preferably, in described step (1), every liter of electrolysis of deposited copper nano-wire arrayIn liquid, contain the CuSO of 90g4·5H2The H of O, 45g2SO4; Preferably, deposition voltage is 2V.
In above-mentioned preparation method, preferably, in described step (2), every liter of electrolysis of nickel deposited nano-wire arrayIn liquid, contain the NiSO of 100g4·6H2The NiCl of O, 30g2, 40g H3BO3; Preferably, deposition voltage is3V。
In above-mentioned preparation method, preferably, in step (2), the mass fraction of described phosphoric acid solution is 5%.
In above-mentioned preparation method, preferably, in step (4), the amount of substance concentration of described sodium hydroxide solutionFor 6mol/L.
The CuO/Ni core-shell nano line that the present invention also provides above-mentioned preparation method to prepare, this CuO/Ni nucleocapsidThe diameter of nano wire is 50-120nm, and length is 5-25 μ m.
Beneficial effect of the present invention:
Preparation method of the present invention has that technique is simple, cost is low, can produce in a large number the CuO/Ni core preparingThe length of shell nano wire can reach 25 μ m.
Brief description of the drawings
Fig. 1 is the SEM scanning electron microscope (SEM) photograph of the CuO/Ni core-shell nano line of embodiment 1;
Fig. 2 is the TEM transmission electron microscope picture of the CuO/Ni core-shell nano line of embodiment 1;
Fig. 3 is the sem energy spectrum analysis figure of the CuO/Ni core-shell nano line of embodiment 1;
Fig. 4 is the SEM scanning electron microscope (SEM) photograph of the CuO/Ni core-shell nano line of embodiment 2;
Fig. 5 is the TEM transmission electron microscope picture of the CuO/Ni core-shell nano line of embodiment 2.
Detailed description of the invention
Understand for technical characterictic of the present invention, object and beneficial effect being had more clearly, existing to skill of the present inventionArt scheme is carried out following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment 1
The present embodiment provides a kind of preparation method of CuO/Ni core-shell nano line, comprises the following steps:
(1) taking aperture as 80nm anodic oxidation aluminium formwork as negative electrode, carbon-point is anode, adopts electrochemical deposition sideMethod is deposited copper nano-wire array in anodic oxidation aluminium formwork; Wherein, before depositing, first antianode is oxidized aluminum dipping formPlate carries out pretreatment, the method for utilizing magnetron sputtering at the Ag layer of its back spatter one deck 200nm thickness as conductionElectrode; The CuSO that contains 90g in every liter of electrolyte of deposited copper nano-wire array4·5H2The H of O, 45g2SO4;Deposition voltage is 2V.
(2) anodic oxidation aluminium formwork that contains Arrays of Copper Nanowires step (1) being obtained immerses mass fractionIn 5% phosphoric acid solution, carry out reaming, the template after reaming 10min is positioned in the heat-treatment furnace of 80 DEG C and processes 1.5h,Obtain the anodic oxidation aluminium formwork that contains CuO nano-wire array.
(3) utilize electrochemical deposition method, nickel deposited in the anodic oxidation aluminium formwork that contains CuO nano-wire arrayNano-wire array, obtains the anodic oxidation aluminium formwork that contains nickel nano-wire array and contain CuO nano-wire array; ItsIn every liter of electrolyte of middle nickel deposited nano-wire array, contain NiSO4·6H2O is 100g, NiCl2For 30g, H3BO3For 40g; Deposition voltage is 3V.
(4) anodic oxidation that contains nickel nano-wire array and contain CuO nano-wire array step (3) being obtainedAluminum alloy pattern plate immerses in the sodium hydroxide solution that amount of substance concentration is 6mol/L and corrodes 30min, removes alumina formwork,In ethanol, clean, utilize infrared lamp to dry, thereby obtain the CuO/Ni core-shell nano that diameter is about 100nmLine.
As depicted in figs. 1 and 2, the SEM scanning electron microscope (SEM) photograph of the CuO/Ni core-shell nano line that Fig. 1 is the present embodiment,Fig. 2 is the TEM transmission electron microscope picture of the CuO/Ni core-shell nano line of the present embodiment. Can be found out by Fig. 1 and Fig. 2:The present embodiment has successfully prepared CuO/Ni core-shell nano linear array, and this nanowire diameter is 100nm.
Fig. 3 is the CuO/Ni core-shell nano line sweep electro microscope energy spectrum analysis chart of the present embodiment. As seen from Figure 3:The composition of nano wire is Cu, O, Ni, and what further prove preparation is CuO/Ni core-shell nano line.
Embodiment 2
The present embodiment provides a kind of preparation method of CuO/Ni core-shell nano line, comprises the following steps:
(1) taking aperture as 30nm anodic oxidation aluminium formwork as negative electrode, carbon-point is anode, adopts electrochemical deposition sideMethod is deposited copper nano-wire array in anodic oxidation aluminium formwork; Wherein, before depositing, first antianode is oxidized aluminum dipping formPlate carries out pretreatment, the method for utilizing magnetron sputtering at the Ag layer of its back spatter one deck 200nm thickness as conductionElectrode; The CuSO that contains 90g in every liter of electrolyte of deposited copper nano-wire array4·5H2The H of O, 45g2SO4;Deposition voltage is 2V.
(2) anodic oxidation aluminium formwork that contains Arrays of Copper Nanowires step (1) being obtained immerses mass fractionIn 5% phosphoric acid solution, carry out reaming, the template after reaming 15min is positioned in the heat-treatment furnace of 80 DEG C and processes 1.5h,Obtain the anodic oxidation aluminium formwork that contains CuO nano-wire array.
(3) utilize electrochemical deposition method, nickel deposited in the anodic oxidation aluminium formwork that contains CuO nano-wire arrayNano-wire array, obtains the anodic oxidation aluminium formwork that contains nickel nano-wire array and contain CuO nano-wire array; ItsThe NiSO that contains 100g in every liter of electrolyte of middle nickel deposited nano-wire array4·6H2The NiCl of O, 30g2、40gH3BO3; Deposition voltage is 3V.
(4) anodic oxidation that contains nickel nano-wire array and contain CuO nano-wire array step (3) being obtainedAluminum alloy pattern plate immerses in the sodium hydroxide solution that amount of substance concentration is 6mol/L and corrodes 50min, removes alumina formwork,In ethanol, clean, utilize infrared lamp to dry, thereby obtain the CuO/Ni core-shell nano that diameter is about 50nmLine.
As shown in Figure 4 and Figure 5, the SEM scanning electron microscope (SEM) photograph of the CuO/Ni core-shell nano line that Fig. 4 is the present embodiment,Fig. 5 is the TEM transmission electron microscope picture of the CuO/Ni core-shell nano line of the present embodiment. By Fig. 4 and known reality of Fig. 5Execute example and successfully prepared CuO/Ni core-shell nano linear array, this nanowire diameter is 50nm.
In sum, the preparation method of a kind of CuO/Ni core-shell nano line provided by the invention, have technique simple,Cost is low, can produce in a large number CuO/Ni core-shell nano line, and the length of the CuO/Ni core-shell nano line preparing canReach 25 μ m.

Claims (10)

1. a preparation method for CuO/Ni core-shell nano line, is characterized in that, comprises the following steps:
(1) taking anodic oxidation aluminium formwork as negative electrode, carbon-point is anode, adopts electrochemical deposition method in anodic oxidationDeposited copper nano-wire array in aluminum alloy pattern plate;
(2) anodic oxidation aluminium formwork that contains Arrays of Copper Nanowires step (1) being obtained immerses in phosphoric acid solutionRow reaming 10-40min, the template after reaming is positioned in the heat-treatment furnace of 60-150 DEG C and processes 1-2h, is containedThe anodic oxidation aluminium formwork of CuO nano-wire array;
(3) utilize electrochemical deposition method, nickel deposited in the anodic oxidation aluminium formwork that contains CuO nano-wire arrayNano-wire array, obtains the anodic oxidation aluminium formwork that contains nickel nano-wire array and contain CuO nano-wire array;
(4) anodic oxidation that contains nickel nano-wire array and contain CuO nano-wire array step (3) being obtainedAluminum alloy pattern plate immerses in sodium hydroxide solution, removes alumina formwork, in ethanol, cleans, and utilizes infrared lamp to dry,Thereby obtain CuO/Ni core-shell nano line.
2. preparation method according to claim 1, is characterized in that: in described step (1), sinkingBefore long-pending, first antianode alumina formwork carries out pretreatment, and described pretreatment is to utilize the method for magnetron sputtering to carry on the back at itThe Ag layer of face sputter one deck 200nm thickness is as conductive electrode.
3. preparation method according to claim 1, is characterized in that: in step (1), and described anodic oxygenThe pore size of changing aluminum alloy pattern plate is 20-80nm.
4. preparation method according to claim 1, is characterized in that: in described step (1), and deposited copperThe CuSO that contains 90g in every liter of electrolyte of nano-wire array4·5H2The H of O, 45g2SO4
5. preparation method according to claim 1, is characterized in that: in described step (1), carrying outWhen deposition, deposition voltage is 2V.
6. preparation method according to claim 1, is characterized in that: in described step (2), and nickel depositedThe NiSO that contains 100g in every liter of electrolyte of nano-wire array4·6H2The NiCl of O, 30g2, 40g H3BO3;Deposition voltage is 3V.
7. preparation method according to claim 1, is characterized in that: in step (2), described phosphoric acid is moltenThe mass fraction of liquid is 5%.
8. preparation method according to claim 1, is characterized in that: in step (4), and described hydroxideThe amount of substance concentration of sodium solution is 6mol/L.
9. the CuO/Ni core-shell nano line that the preparation method described in a claim 1-8 any one prepares.
10. CuO/Ni core-shell nano line according to claim 9, is characterized in that: this CuO/Ni nucleocapsidThe diameter of nano wire is 50-120nm, and length is 5-25 μ m.
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Cited By (8)

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CN106856228A (en) * 2016-12-27 2017-06-16 Tcl集团股份有限公司 A kind of QLED devices and preparation method thereof
CN108311150A (en) * 2017-01-17 2018-07-24 中国科学院上海高等研究院 It is a kind of to grow the catalyst and its preparation method and application that Cu nano wires obtain on Ni
CN110361424A (en) * 2019-07-17 2019-10-22 徐靖才 A kind of n-p heterogeneous type nucleocapsid array gas sensitive and preparation method thereof
CN112886023A (en) * 2019-11-29 2021-06-01 大连大学 CuO-NiNPs/PET-ITO electrode and application thereof
CN112993266A (en) * 2019-12-16 2021-06-18 大连大学 Constructed starch fuel cell constructed by applying CuO-NiNPs/carbon cloth plastic electrode
CN113092552A (en) * 2019-12-23 2021-07-09 大连大学 Method for constructing lactose fuel cell by CuO-NiNPs/MFC electrode
CN113189176A (en) * 2020-05-20 2021-07-30 郑州轻工业大学 Ni/Au composite nanowire array and application thereof in enzyme-free glucose sensor electrode
CN113533297A (en) * 2021-07-07 2021-10-22 陕西师范大学 Super-hydrophobic CuO @ Ag nanowire array and application thereof in circulating SERS detection of malachite green

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106856228A (en) * 2016-12-27 2017-06-16 Tcl集团股份有限公司 A kind of QLED devices and preparation method thereof
CN108311150A (en) * 2017-01-17 2018-07-24 中国科学院上海高等研究院 It is a kind of to grow the catalyst and its preparation method and application that Cu nano wires obtain on Ni
CN110361424B (en) * 2019-07-17 2021-11-19 中国计量大学 N-p heterogeneous core-shell array gas-sensitive material and preparation method thereof
CN110361424A (en) * 2019-07-17 2019-10-22 徐靖才 A kind of n-p heterogeneous type nucleocapsid array gas sensitive and preparation method thereof
CN112886023B (en) * 2019-11-29 2022-07-12 大连大学 CuO-NiNPs/PET-ITO electrode and application thereof
CN112886023A (en) * 2019-11-29 2021-06-01 大连大学 CuO-NiNPs/PET-ITO electrode and application thereof
CN112993266A (en) * 2019-12-16 2021-06-18 大连大学 Constructed starch fuel cell constructed by applying CuO-NiNPs/carbon cloth plastic electrode
CN113092552A (en) * 2019-12-23 2021-07-09 大连大学 Method for constructing lactose fuel cell by CuO-NiNPs/MFC electrode
CN113092552B (en) * 2019-12-23 2022-12-13 大连大学 Method for constructing lactose fuel cell by CuO-NiNPs/MFC electrode
CN113189176A (en) * 2020-05-20 2021-07-30 郑州轻工业大学 Ni/Au composite nanowire array and application thereof in enzyme-free glucose sensor electrode
CN113189176B (en) * 2020-05-20 2023-12-29 郑州轻工业大学 Ni/Au composite nanowire array and application thereof in enzyme-free glucose sensor electrode
CN113533297A (en) * 2021-07-07 2021-10-22 陕西师范大学 Super-hydrophobic CuO @ Ag nanowire array and application thereof in circulating SERS detection of malachite green
CN113533297B (en) * 2021-07-07 2023-02-24 陕西师范大学 Super-hydrophobic CuO @ Ag nanowire array and application of array in circulating SERS (surface enhanced Raman scattering) detection of malachite green

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