CN110387565A - A kind of surface preparation method that can prepare a variety of nanowire structures - Google Patents
A kind of surface preparation method that can prepare a variety of nanowire structures Download PDFInfo
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- CN110387565A CN110387565A CN201910711900.XA CN201910711900A CN110387565A CN 110387565 A CN110387565 A CN 110387565A CN 201910711900 A CN201910711900 A CN 201910711900A CN 110387565 A CN110387565 A CN 110387565A
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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
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
-
- 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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
Abstract
A kind of surface preparation method that can prepare a variety of nanowire structures, belongs to technical field of surface.This method utilizes the electro-plating method of template auxiliary, by changing template pitch of holes, aperture and plating duration, can form the various structures patterns such as erect type, Conglobation type, round pool type, and can change the structure height and angle of erect type and Conglobation type.Nano wire is 4-50 μm high, and nano wire center is away from 60-500nm, nanowire diameter 5-400nm.Surface topography obtained by this kind of preparation method is controllable, structure type is diversified and can be across scale, erect type and the phase-change heat transfers fields such as Conglobation type can be used to condense, round pool type can be used to boil.
Description
Technical field
The present invention relates to a kind of copper nano-wire surface, refer in particular to a kind of to form erect type, Conglobation type, round pool type different morphologies
Copper nano-wire surface preparation method, be mainly characterized by using template auxiliary using electric plating method prepare different spacing and
The copper nano-wire surface of line footpath, this copper nano-wire surface can be used to effectively strengthen condensation and boiling due to its different structure pattern
Equal phase-change heat transfers field, belongs to functional structure.
Background technique
How to improve surface texture make its improve to greatest extent the effect of condensation heat transfer and boiling heat transfer be always heat management,
The research hotspot of water assembling sphere.In condensation heat transfer field, because its minimum condensing droplet can cause to close on nanostructured surface
And the limitation for inducing drop to bounce and getting rid of gravity is detached from surface, but most of nanostructures are for improving heat transfer efficiency aspect only
It is confined to the surface degree of supercooling (△ T < 5K) of very little, within the scope of bigger surface degree of supercooling, uncontrollable nonhomogen-ous nucleation meeting
Cause condensation to flood the appearance of mode, significantly limits the raising of heat transfer property on nanostructured surface.With traditional wetting
Property contrast surface compare, with high length-diameter ratio and erect type, Conglobation type nanowire surface, since it is with good space
Effect of restraint can sufficiently reduce a possibility that stream molecule enters on condensing surface inside super-hydrophobic nano cable architecture, very
The appearance for flooding mode is limited within the scope of big degree of supercooling, and transfer fluxes can be greatly improved.Document " Hydrophobic
copper nanowires for enhancing condensation heat transfer.(Nano Energy, 2017,
33: 177-183) " and " Three-Dimensional Superhydrophobic Nanowire Networks for
Enhancing Condensation Heat Transfer(Joule, 2018,2 (2) 269-279) " it is to utilize copper nanometer
Line realizes greatly improving for condensation heat transfer performance under big supercooling degree.In boiling heat transfer field, the table with micro-nano cavernous structure
Face also shows excellent advantage, document " Effects of nanowire height on improving boiling heat transfer performance
Pool boiling performance of water on silicon chips(International Journal of
Thermal Sciences, 2011,50:2084-2090) " cavernous structure formed using silicon nanowires is reported compared to perpendicular
Straight silicon nanowires and vertical copper nano-wire, boiling heat transfer effect significantly improve.Document " Enhancement of
Saturation Boiling of PF-5060 on Microporous Copper Dendrite Surfaces(Journal
Of Heat Transfer, 2010,132:071501-1) " in be utilized copper nano-wire formation bowl configurations, hole
Bigger heat-transfer effect is better.And in the preparation of copper nano-wire, it uses more for vapor phase method, liquid phase method, solvent-thermal method, template
Method, the research for preparing copper nano-wire with electrodeposition process are less.Document " Large-scale synthesis of high-
Quality ultralong copper nanowires.(Langmuir, 2005,21 (9): passes through in 3746-3748.) "
Liquid phase method has synthesized the copper nano-wire of high quality.Document " Sythesis of ultralong copper nanowires for
high-performance transparent electrode.(Journal of the American Chemical
Society, 2012,134 (35): 14283-14286) " developed it is a kind of by organic amine system synthesized diameter for 78nm,
The method of copper nano-wire of the length from more than ten microns to several hundred microns.Patent CN201810220699.0 discloses a kind of using nitre
The sour copper copper nano-wire that in chlorination copper powders prepared by the solvent-thermal method of organic amine hexadecane and reduced sugar.Patent
CN201610837753.7 discloses a kind of method for preparing copper nano-wire by electronation after first roasting.Patent
CN201810454313.2 discloses a kind of method for preparing copper nano-wire with sol-gal process.To sum up, presently relevant field section
It grinds personnel and is prepared for copper nano-wire using a variety of methods, but prepare copper nano-wire using template combination electrochemical deposition method
The rare report of patent, patent CN105483795 disclose a kind of using underpotential deposition technology preparation complex copper nanometer.By owing
Current potential prepares composition metal nano wire in copper surface deposited metal monoatomic layer.Firstly, this patent is same as the patent to use mould
The method that plate auxiliary carries out electrochemical deposition, but what this patent used is bilateral AAO template, and prepared nano wire is directly firmly
It is grown on cathode surface；What the patent was used is single-pass AAO template, and prepared nano wire just intersperses among after having dissolved template
In solution, without accompanying place.Secondly, this patent only needs self assembly hydrophobic substance that can reach the effect for preventing copper nano-wire from aoxidizing
Fruit, it is simple and easy compared with the patent deposited metal monoatomic layer is anti-oxidant.Finally, this patent can only be made with a kind of method
The micro-Nano composite structure of the standby different morphologies formed by more nano wires, erect type and Conglobation type can be used for effectively improving condensation and pass
Heat, and round pool type can be used for effectively improving boiling heat transfer, in general, show huge potentiality in phase-change heat transfer field；It should
Patent is the single nano-wire of dispersion, is used for transparent electrode, and the purpose difference of the two is larger.
Summary of the invention
To solve problems of the prior art, the present invention provides a kind of containing there are many micro-Nano composite structure copper nano-wires
Surface preparation method, the micro-Nano composite structure of the different morphologies formed by more nano wires can be prepared with a kind of method, directly
Vertical type and Conglobation type can be used for effectively improving condensation heat transfer, and round pool type can be used for effectively improving boiling heat transfer, in phase-change heat transfer
Field shows huge potentiality.
The technical solution adopted by the present invention are as follows: a kind of surface preparation method that can prepare a variety of nanowire structures passes through control
Pallet pitch of holes, aperture, plating duration can form erect type, Conglobation type, round pool type structure, and height is about 4-50 μm, nanometer
The center spacing of line is between 60-500nm, and the diameter of nano wire is between 5-400nm.
Method includes the following steps:
Step 1 takes red copper block, polishes and ultrasonic oil removing is successively put into self-made clamp from bottom to up using two electrode systems
Plexiglass block, the cathode red copper block for connecting working electrode, porous anodic alumina template (AAO), the filter for being plated liquid wetting
Paper, connection sufficiently clamp anode red copper block, the plexiglass block of electrode, and electrochemical workstation sets voltage and time；
On the basis of two electrode systems of step 2 in step 1, reference electrode is added in an electroplanting device, forms three electrodes
System guarantees that anode red copper block and cathode red copper block spacing are 10-30mm, and reference electrode to two electrodes is equidistant, electricity
Chem workstation sets voltage and time；
Step 3 NaOH dissolves anodic oxidation aluminium formwork, and the surface washing of erect type and Conglobation type completely and after drying is put into ten
In eight alkyl hydrosulfides, 70 DEG C of water-bath 1h, this step is then ignored on the surface of round pool type.Electroplate liquid is according to cupric pyrophosphate: pyrophosphoric acid
Potassium: Triammonium citrate: mass ratio=5:30:3:100 ratio of deionized water is prepared, and pH value should be between 7-9.
- 1.5V is arrived in voltage setting -0.5 in the step 1, and 600-1200s is arranged in the time.
- 1.5V is arrived in voltage setting -0.5 in the step 2, and 1800-18000s is arranged in the time.
The invention has the benefit that a kind of copper nano-wire table that can form erect type, Conglobation type, round pool type different morphologies
The preparation method in face, orthostatic and Conglobation type surface are in super-hydrophobicity, can be used for effective enforcing condensation heat transfer；Round pool type surface
In Superhydrophilic, effective enhanced boiling heat transfer field can be used for, the copper nano-wire surface of this patent preparation is led in phase-change heat transfer
Domain can show huge potentiality.Compared with other patents, this patent can prepare different structure with a kind of preparation method
The micro-nano aggregate surface of pattern, and different purposes can be realized using different structure and morphologies.This method utilizes template auxiliary
Electro-plating method can form a variety of knots such as erect type, Conglobation type, round pool type by changing template pitch of holes, aperture and plating duration
Looks are configured, and the structure height and angle of erect type and Conglobation type can be changed.Nano wire is 4-50 μm high, and nano wire center is away from 60-
500nm, nanowire diameter 5-400nm.Surface topography obtained by this kind of preparation method is controllable, structure type is diversified and can be across
The phase-change heat transfers fields such as scale, erect type and Conglobation type can be used to condense, round pool type can be used to boil.The application only uses one
Kind method can prepare the micro-Nano composite structure of the different morphologies formed by more nano wires, and erect type and Conglobation type can be used for having
Effect improves condensation heat transfer, and round pool type can be used for effectively improving boiling heat transfer, in general, show in phase-change heat transfer field huge
Big potentiality.
Detailed description of the invention
Fig. 1 is laboratory holder structure drawing of device of the invention.
Fig. 2 is flow diagram of the invention.
Fig. 3 is 1 erect type of present example, Conglobation type, round pool type copper nano-wire body structure surface SEM figure.Wherein: amplifying
10000 times, scale bar is 20 μm.Erect type :(a) line spacing is 450nm, line footpath 360nm；(b) line spacing is 450nm, line
Diameter is 280nm；Conglobation type: (c) line spacing is 450nm, line footpath 200nm；(d) line spacing is 450nm, line footpath 110nm；Circle
Pit type: (e) line spacing is 125nm, line footpath 30nm；(f) line spacing is 65nm, line footpath 10nm.
Fig. 4 is the erect type and Conglobation type copper nano-wire surface SEM figure of 2 different height of present example.Wherein: picture is equal
10000 times of amplification, scale bar are 20 μm.(a) line spacing is 450nm, line footpath 200nm, and 3h is electroplated；(b) line spacing is
4h is electroplated in 450nm, line footpath 200nm；(c) line spacing is 450nm, line footpath 200nm, and 5h is electroplated；(d) line spacing is
1h is electroplated in 450nm, line footpath 280nm；(e) line spacing is 450nm, line footpath 280nm, and 2h is electroplated；(f) line spacing is
3h is electroplated in 450nm, line footpath 280nm.
Specific embodiment
The following examples are intended to illustrate the invention.
Embodiment 1
Erect type, Conglobation type, the preparation of round pool type copper nano-wire body structure surface
A, it takes red copper block to be polished with sand paper, and is sequentially placed into each ultrasound 10min of acetone, ethyl alcohol, deionized water, take out and use nitrogen
Drying.
B, in fixture, the red copper block, the porous anode that are successively put into plexiglass block from bottom to up, connect working electrode
Aluminum alloy pattern plate, drop have the filter paper of electroplate liquid, connect red copper block, the plexiglass block to electrode, and sufficiently clamp, template model 450-
360,450-280,450-200,450-110,125-30,65-10.Electrochemical workstation voltage setting -0.8V, time setting
900s。
D, the red copper block and another red copper block spacing 20mm of template, reference electrode the work selection of three-electrode system: are covered with
The distance of two electrodes of distance is 10mm.10800s is arranged in electrochemical workstation voltage setting -0.8V, time.
E, porous anodic alumina template will be dissolved with the NaOH of 2mol/L after the deionized water rinse of red copper block, spend from
With being dried with nitrogen after the sub- abundant rinse red copper block of water, it is put into the beaker of the Stearyl mercaptan equipped with 0.0025mol/L therewith,
And it tightly seals.Beaker is put into 70 DEG C of water-bath, takes out beaker after 1h, and by the red copper block taking-up nitrogen in beaker
Drying.
F, using the porous anodic alumina template of 450-360 and 450-280 model, copper nano-wire surface is in upright
Type, as shown in (a) and (b) in Fig. 3；Using the porous anodic alumina template of 450-200 and 450-110 model, copper nano-wire
Surface is in Conglobation type, and (c), (d) are shown in Fig. 3；Using the porous anodic alumina template of 125-30 and 65-10 model,
Copper nano-wire surface is in round pool type, and (e), (f) are shown in Fig. 3.Therefore, it by control line spacing and line footpath, can present straight
The various structures patterns such as vertical type, Conglobation type, round pool type, wherein erect type and Conglobation type body structure surface are conducive to condensation heat transfer, circle
Pit type is conducive to boiling heat transfer.
Embodiment 2
The erect type of different height and the preparation of Conglobation type copper nano-wire surface
A, it takes red copper block to be polished with sand paper, and is sequentially placed into each ultrasound 10min of acetone, ethyl alcohol, deionized water, take out and use nitrogen
Drying.
B, in two electrode systems that fixture provides, the purple that is successively put into plexiglass block from bottom to up, connects working electrode
Copper billet, porous anodic alumina template, drop have the filter paper of electroplate liquid, connect red copper block, the plexiglass block to electrode, and sufficiently press from both sides
Tightly, template model 450-360,450-200.900s is arranged in electrochemical workstation voltage setting -0.8V, time.
C, in the three-electrode system that electroplating pool provides, cathode pole red copper block and anode red copper block spacing 20mm, reference electricity
Pole span is 10mm with a distance from two electrodes.Voltage setting -0.8V, when selecting the template of 450-360 model, time difference
It is set as 3600s, 7200s, 10800s.When select 450-200 template when, the time be respectively set to 10800s, 14400s,
18000s。
D, porous anodic alumina template will be dissolved with the NaOH of 2mol/L after the deionized water rinse of red copper block, spend from
With being dried with nitrogen after the sub- abundant rinse red copper block of water, it is put into the beaker of the Stearyl mercaptan equipped with 0.0025mol/L therewith simultaneously
It is put into 70 DEG C of water-bath, takes out beaker after 1h, and the red copper block in beaker is taken out with being dried with nitrogen.
F, using the porous anodic alumina template of 450-200 model, second step electroplating time is respectively 3h, 4h and 5h,
3h height is about 10.9 μm, and the height of 4h is about 42 μm, and the height that 5h is electroplated is greater than 50 μm；Using the porous of 450-360 model
Anodic oxidation aluminium formwork, second step electroplating time are respectively 1h, 2h and 3h, and the height of 1h is about 4.5 μm, and the height of 2h is about
9.4 μm, the height of 3h is about 11.2 μm.For the nanowire surface of Conglobation type (450-200), height is higher, is more conducive to
It limits hydrone under the conditions of low-pressure experiment to enter inside configuration and form the phenomenon that flooding, to be conducive to compared with big supercooling degree
Dropwise condensation, augmentation of heat transfer are realized in range；For the nano wire of erect type (450-360) pattern, height is higher, reunites existing
As being more obvious, the angle of the structure formed after reunion is bigger, under suitable angle, is conducive to promote under normal pressure experiment condition
The merging of drop induces spring, to be conducive to augmentation of heat transfer.
Claims (4)
1. a kind of surface preparation method that can prepare a variety of nanowire structures, it is characterised in that: by controlling template pitch of holes, hole
Diameter, plating duration can form erect type, Conglobation type, round pool type structure, and about 4-50 μm of height, the center spacing of nano wire exists
Between 60-500nm, the diameter of nano wire is between 5-400nm；
Method includes the following steps:
Step 1 takes red copper block, polishes and ultrasonic oil removing is successively put into self-made clamp from bottom to up using two electrode systems
Plexiglass block, porous anodic alumina template, the filter paper for being plated liquid wetting, connects the cathode red copper block for connecting working electrode
Anode red copper block, the plexiglass block to electrode are connect, and is sufficiently clamped, electrochemical workstation sets voltage and the time carries out electricity
Plating；
On the basis of two electrode systems of step 2 in step 1, reference electrode is added in an electroplanting device, forms three electrodes
System guarantees that anode red copper block and cathode red copper block spacing are 10-30mm, and reference electrode to two electrodes is equidistant, electricity
Chem workstation sets voltage and the time is electroplated；
Step 3 NaOH dissolves anodic oxidation aluminium formwork, and the surface washing of erect type and Conglobation type completely and after drying is put into dress
Have in Stearyl mercaptan, 70 DEG C of water-bath 1h.
2. a kind of surface preparation method that can prepare a variety of nanowire structures according to claim 1, which is characterized in that electricity
Plating solution is according to cupric pyrophosphate: potassium pyrophosphate: Triammonium citrate: mass ratio=5:30:3:100 ratio of deionized water is prepared, pH
Value is between 7-9.
3. a kind of surface preparation method that can prepare a variety of nanowire structures according to claim 1, it is characterised in that: step
- 1.5V is arrived in voltage setting -0.5 in rapid 1, and 600-1200s is arranged in the time.
4. a kind of surface preparation method that can prepare a variety of nanowire structures according to claim 1, it is characterised in that: step
- 1.5V is arrived in voltage setting -0.5 in rapid 2, and 1800-18000s is arranged in the time.
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| CN201910711900.XA CN110387565A (en) | 2019-08-02 | 2019-08-02 | A kind of surface preparation method that can prepare a variety of nanowire structures |
| PCT/CN2020/073161 WO2021022800A1 (en) | 2019-08-02 | 2020-01-20 | Surface preparation method capable of preparing various nanowire structures |
| CN202010204923.4A CN111218702B (en) | 2019-08-02 | 2020-03-22 | Surface preparation method capable of preparing various nanowire structures |
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| CN202010204923.4A Active CN111218702B (en) | 2019-08-02 | 2020-03-22 | Surface preparation method capable of preparing various nanowire structures |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176388A (en) * | 2020-09-21 | 2021-01-05 | 深圳拓扑精膜科技有限公司 | Electroplating clamping device and method for preparing patterned nanowire by using same |
| WO2021022800A1 (en) * | 2019-08-02 | 2021-02-11 | 大连理工大学 | Surface preparation method capable of preparing various nanowire structures |
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| CN111996560A (en) * | 2020-07-10 | 2020-11-27 | 深圳先进技术研究院 | Metal wire preparation method, metal wire and clamp |
| CN112657805B (en) * | 2020-12-01 | 2022-07-19 | 大连理工大学 | Nanowire-fluorocarbon composite coating and preparation method thereof |
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| CN1995468A (en) * | 2006-12-18 | 2007-07-11 | 天津理工大学 | Diameter-controllable metal nm-line array preparation method |
| DE102008015333B4 (en) * | 2008-03-20 | 2021-05-12 | Gsi Helmholtzzentrum Für Schwerionenforschung Gmbh | Nanowire structural element, process for its production, microreactor system and catalyst system |
| TWI454422B (en) * | 2012-04-12 | 2014-10-01 | Nat Univ Tsing Hua | A method for manufacturing a copper nano-wire with high density of twins |
| CN103448316B (en) * | 2013-08-07 | 2015-07-29 | 许昌学院 | A kind of copper substrate superhydrophobic laminated film with low-friction coefficient and preparation method thereof |
| WO2017095925A1 (en) * | 2015-11-30 | 2017-06-08 | The Regents Of The University Of California | Low-density interconnected metal foams and methods of manufacture |
| CN105483795B (en) * | 2016-01-21 | 2017-12-05 | 广州中国科学院先进技术研究所 | A kind of method that compound copper nano-wire is prepared using underpotential deposition technology |
| CN109778249B (en) * | 2019-02-22 | 2020-05-22 | 浙江交通科技股份有限公司 | Preparation method for preparing metal core-shell nanowire |
| US11229090B2 (en) * | 2019-05-10 | 2022-01-18 | Northrop Grumman Systems Corporation | Multilayered nanowire arrays with lateral interposers |
| CN110387565A (en) * | 2019-08-02 | 2019-10-29 | 大连理工大学 | A kind of surface preparation method that can prepare a variety of nanowire structures |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021022800A1 (en) * | 2019-08-02 | 2021-02-11 | 大连理工大学 | Surface preparation method capable of preparing various nanowire structures |
| CN112176388A (en) * | 2020-09-21 | 2021-01-05 | 深圳拓扑精膜科技有限公司 | Electroplating clamping device and method for preparing patterned nanowire by using same |
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Application publication date: 20191029 |