CN108018587A - A kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method - Google Patents
A kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method Download PDFInfo
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- CN108018587A CN108018587A CN201711285681.0A CN201711285681A CN108018587A CN 108018587 A CN108018587 A CN 108018587A CN 201711285681 A CN201711285681 A CN 201711285681A CN 108018587 A CN108018587 A CN 108018587A
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- polycarbonate template
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/022—Electroplating of selected surface areas using masking means
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/024—Electroplating of selected surface areas using locally applied electromagnetic radiation, e.g. lasers
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/028—Electroplating of selected surface areas one side electroplating, e.g. substrate conveyed in a bath with inhibited background plating
Abstract
The present invention relates to a kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method, step are as follows：Prepare polytetrafluoroethylene (PTFE) substrate, copper sheet and porous polycarbonate template；The preparation of working electrode；Prepare acidic electrolysis bath；The hole wetting of porous polycarbonate template；Cobalt nanowire and the preparation at cobalt-based bottom；Remove photoresist：Unexposed photoresist is removed using acetone, cleans patterned porous polycarbonate template surface with deionized water afterwards；Remove polycarbonate template：Polycarbonate template is removed using dichloromethane, you can obtains patterned nano-wire array.
Description
Technical field
The invention designs nano wire preparation field, more particularly to the preparation field of Magnetic Nanowire Arrays.
Background technology
Nano-wire array has extensive use in fields such as life science, medical treatment ＆ health, environmental protection, clean energy resourcies, especially
It is the micro-fluidic chip field in medical treatment ＆ health, and nano-wire array plays an important roll.
Micro-fluidic chip be it is a kind of technology of the manipulation for main feature is carried out to fluid in micro-meter scale space, having will be raw
Ability on the basic function micro in the laboratories such as thing, chemistry to a several square centimeter chips, therefore the chip reality that is otherwise known as
Test room.At this stage, the micro-fluidic chip of dominant form forms network by microchannel more, runs through whole system with controlled fluid,
To realize the various functions in the laboratories such as conventional chemical or biology.The essential characteristic and sharpest edges of micro-fluidic chip are a variety of
Monotechnics flexible combination and scale in small controllable platform integrate.
The sample detection or process flow of micro-fluidic chip can be divided into three sample introduction, mixing, detection or processing key steps,
Since the space scale of micro-fluidic chip is smaller, Reynolds number is smaller, thus the mixing of sample be during committed step.It is good
Good mixing can allow detection or handling result more accurate credible.But the spontaneous mixing for relying solely on sample is much unable to reach
It is required that.
Enlightened be subject to living nature eucaryote cilium, scientific research personnel, which proposes, is introduced into cilium in micro-fluidic chip, uses
Mixed in sample.Therefore, the ciliary structures feature of bionical nature, prepares the similar Magnetic Nanowire Arrays of shape just
It is particularly important.Up to the present, there are many methods for preparing nano-wire array, wherein electrochemical deposition is most commonly seen
One of mode.But most common two kinds of depositions template in electrochemical deposition, anodic oxidation aluminium formwork and polycarbonate template, all without
Method autonomous Design hole is distributed so that the distribution of nano-wire array can not be adjusted, and limit this technology to a certain extent
Development.
The content of the invention
The object of the present invention is to provide a kind of preparation method of the graphical nano-wire array based on polycarbonate template, system
Preparation Method is as follows：
A kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method, is comprised the following steps：
(1) copper sheet and porous polycarbonate template are prepared；
(2) preparation of working electrode：After the heating fusing of suitable martial virtue alloy, coated uniformly, then on copper sheet
Porous polycarbonate template is overlying on martial virtue alloy upper surface；The copper sheet back side and side are coated using epoxide-resin glue, is ensured
Cobalt ions can only deposit in porous polycarbonate form plate hole；A conducting wire, one end connection copper sheet back side are taken, the other end connects
Receiving electrode presss from both sides, and working electrode is made；
(3) photoresist is coated：Appropriate photoresist is coated in porous polycarbonate template upper surface, by the porous poly- carbonic acid
Ester template is placed in sol evenning machine, it is uniformly coated photoresist；
(4) exposure and development：The porous polycarbonate mould of coated photoresist is irradiated using UV light permeability mask plate
Photochemical reaction occurs for plate, irradiated photoresist, and property changed, during development can and developer solution chemical reaction occurs simultaneously
Remove；And the part that version is blocked is photo-etched, do not occur any change, discord developer solution reacts retained during development, so
The figure of reticle can just be stayed in figure in porous polycarbonate template by development；
(5) acidic electrolysis bath is prepared：Electrolyte includes：CoSO4 7H2O and H3BO3, molar concentration scope is respectively 0.60-
0.66M/L and 0.62-0.68M/L, and pH value is adjusted to 2.5-3.5；
(6) the hole wetting of porous polycarbonate template：Patterned porous polycarbonate template is placed in electrolyte,
The cobalt ions in the electrolyte is set to enter among porous polycarbonate form plate hole；
(7) preparation at cobalt nanowire and cobalt-based bottom：Platinized platinum is placed in electrolyte electrode and working electrode, two electrodes connect
Power supply is connected to, the situation of change by monitoring deposition current learns the deposition of cobalt nanowire, when cobalt nanowire has overflowed
Porous polycarbonate form plate hole starts to stop deposition during deposition；
(8) photoresist is removed：Unexposed photoresist is removed using acetone, is cleaned afterwards with deionized water patterned more
Hole polycarbonate template surface；
(9) polycarbonate template is removed：Polycarbonate template is removed using dichloromethane, you can obtains patterned nanometer
Linear array.
Compared with prior art, which can adjust the hole of polycarbonate template point using photoetching process
Cloth, so as to adjust the distribution of nano wire, avoids influencing each other caused by nanowire density is excessive.Micro-nano robot has been expanded to exist
Biomedical and field of environment protection application range.
Brief description of the drawings
In order to make the content of the present invention more clearly understood, the specific embodiment below according to the present invention and combination
Attached drawing, the present invention is described in further detail, wherein：
Fig. 1 is the nano-wire array schematic diagram of general polycarbonate template deposition
Fig. 2 is the nano-wire array schematic diagram of the present invention
Reference numeral：101- cobalt nanowires；102- copper sheets；103- photoresists.
Embodiment
The object of the present invention is to provide a kind of preparation method of the graphical nano-wire array based on polycarbonate template, bag
Include step：
(1) cleaning of copper sheet substrate：Need before use successively using 200mL deionized waters, 100mL acetone, 100mL
Absolute ethyl alcohol and 200mL deionized waters clean copper sheet substrate (length of side 20mm), spare with 30 DEG C of low temperature dryings afterwards.
(2) preparation of working electrode：Suitable martial virtue alloy (70 DEG C of fusing point) is placed on copper sheet, is put into baking oven jointly
In be heated to its fusing point (70 DEG C), continue under this temperature environment, it is using quartz glass edge that martial virtue alloy-coated is uniform, so
Porous polycarbonate template (circular, aperture 200nm, diameter 19mm) is overlying on martial virtue alloy upper surface afterwards, while described in guarantee
Porous polycarbonate template has good contact with the martial virtue alloy, and the lower surface of porous polycarbonate template can be by the martial virtue
Alloy all covers.Take a fine copper wire (diameter 0.8mm), one end connection copper sheet back side, other end connection electrode folder.Utilize
Epoxide-resin glue coats the copper sheet back side and side, ensures that cobalt ions can only deposit in porous polycarbonate form plate hole.
(3) photoresist is coated：Appropriate photoetching is coated in above-mentioned working electrode upper surface (i.e. polycarbonate template upper surface)
Glue SU-8, the working electrode is placed in sol evenning machine, and rotating speed is 3000-4000 revs/min.
(4) exposure and development：The working electrode of coated photoresist is irradiated using UV light permeability mask plate, is irradiated
Photoresist photochemical reaction occurs, property changed, and when development will occur to chemically react and remove with developer solution；And
The part that version is blocked is photo-etched, does not occur any change, discord developer solution, which reacts, during development is retained on disk, so
The figure of reticle is transferred to disk surfaces, can just be stayed in figure on disk by development.
(5) the hole wetting of porous polycarbonate template：Working electrode is placed in the electrolyte of the quartzy electrolytic cell,
3min is stirred to electrolyte using magnetic agitation instrument, the cobalt ions in the electrolyte is entered porous polycarbonate template
Among hole.
(6) preparation of cobalt nanowire 101：The composition of electrolyte is：The CoSO of 0.63M/L4 7H2O's and 0.65M/L
H3BO3, while adjust pH value of solution=3 using H2SO4.Two electrode systems are that platinized platinum is placed in electrode and working electrode to quartzy electricity
In cell bath, two electrodes are connected to power supply, and power supply can provide " simple alternating current+constant voltage DC biasing ", " constant voltage DC "
Output modes such as " pulse direct currents ".Using digital multimeter to monitor the situation of change of deposition current, when cobalt nanowire is in hole
After the completion of depositing in hole, it may proceed to deposit in the porous polycarbonate template upper surface, deposition current, which occurs, at this time rises to.
Therefore the deposition of nano wire can be learnt from the situation of change of deposition current.When cobalt nanowire 101 overflowed it is described more
Hole polycarbonate template hole starts to stop deposition during deposition.
(7) photoresist is removed：Unexposed photoresist is removed using acetone, spends 200mL ionized water cleanings afterwards
Electrode.
(8) polycarbonate template is removed：Makrolon is removed successively using 200mL dichloromethane and 200mL deionized waters
Template, you can obtain patterned nano-wire array.
Claims (1)
1. a kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method, is comprised the following steps：
(1) copper sheet and porous polycarbonate template are prepared；
(2) preparation of working electrode：After the heating fusing of suitable martial virtue alloy, coated uniformly on copper sheet, then will be more
Hole polycarbonate template is overlying on martial virtue alloy upper surface；Coat the copper sheet back side and side using epoxide-resin glue, ensure cobalt from
Son can only deposit in porous polycarbonate form plate hole；Take a conducting wire, one end connection copper sheet back side, other end connection electricity
Pole presss from both sides, and working electrode is made；
(3) photoresist is coated：Appropriate photoresist is coated in porous polycarbonate template upper surface, by the porous polycarbonate mould
Plate is placed in sol evenning machine, it is uniformly coated photoresist；
(4) exposure and development：The porous polycarbonate template of coated photoresist is irradiated using UV light permeability mask plate, is shone
Photochemical reaction occurs for the photoresist penetrated, and property is changed, during development can and developer solution occur to chemically react and remove；
And the part that version is blocked is photo-etched, do not occur any change, discord developer solution reacts retained, such reticle during development
Figure by development figure can be just stayed in porous polycarbonate template；
(5) acidic electrolysis bath is prepared：Electrolyte includes：CoSO4 7H2O and H3BO3, molar concentration scope is respectively 0.60-
0.66M/L and 0.62-0.68M/L, and pH value is adjusted to 2.5-3.5；
(6) the hole wetting of porous polycarbonate template：Patterned porous polycarbonate template is placed in electrolyte, makes institute
The cobalt ions stated in electrolyte enters among porous polycarbonate form plate hole；
(7) preparation at cobalt nanowire and cobalt-based bottom：Platinized platinum is placed in electrolyte electrode and working electrode, two electrodes are connected to
Power supply, the situation of change by monitoring deposition current learn the deposition of cobalt nanowire, when cobalt nanowire overflowed it is porous
Polycarbonate template hole starts to stop deposition during deposition；
(8) photoresist is removed：Unexposed photoresist is removed using acetone, is cleaned afterwards with deionized water patterned porous poly-
Carbonic ester template surface.
(9) polycarbonate template is removed：Polycarbonate template is removed using dichloromethane, you can obtains patterned nanometer linear array
Row.
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| CN201711285681.0A CN108018587A (en) | 2017-12-07 | 2017-12-07 | A kind of method that graphical cobalt nanowire array is prepared based on polycarbonate template method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108598365A (en) * | 2018-05-25 | 2018-09-28 | 哈尔滨工业大学 | A kind of negative electrode for lithium secondary battery and preparation method thereof and its lithium secondary battery |
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| CN101319407A (en) * | 2008-06-25 | 2008-12-10 | 北京理工大学 | Preparation method of metallic oxide nanometer granular nano-array material |
| CN103482704A (en) * | 2013-09-04 | 2014-01-01 | 重庆大学 | MnO2 nanosheet self-assembled nanotube and preparation method thereof |
| US20150060266A1 (en) * | 2012-08-13 | 2015-03-05 | International Business Machines Corporation | Two mask process for electroplating metal employing a negative electrophoretic photoresist |
| CN106094445A (en) * | 2016-06-12 | 2016-11-09 | 中国科学院微电子研究所 | The manufacture method of large ratio of height to width nano level metal structure |
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2017
- 2017-12-07 CN CN201711285681.0A patent/CN108018587A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| CN101319407A (en) * | 2008-06-25 | 2008-12-10 | 北京理工大学 | Preparation method of metallic oxide nanometer granular nano-array material |
| US20150060266A1 (en) * | 2012-08-13 | 2015-03-05 | International Business Machines Corporation | Two mask process for electroplating metal employing a negative electrophoretic photoresist |
| CN103482704A (en) * | 2013-09-04 | 2014-01-01 | 重庆大学 | MnO2 nanosheet self-assembled nanotube and preparation method thereof |
| CN106094445A (en) * | 2016-06-12 | 2016-11-09 | 中国科学院微电子研究所 | The manufacture method of large ratio of height to width nano level metal structure |
Non-Patent Citations (2)
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| V.SUDHA RANI 等，: ""Structural and magnetic properties of electrodeposited cobalt nanowires in polycarbonate membrane"", 《PHYS.STATUS SOLIDI A,》 * |
| 李晓茹 等，: ""图案化金属铜纳米线阵列的制备与表征"", 《功能材料》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108598365A (en) * | 2018-05-25 | 2018-09-28 | 哈尔滨工业大学 | A kind of negative electrode for lithium secondary battery and preparation method thereof and its lithium secondary battery |
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Application publication date: 20180511 |
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