CN108922791A - A kind of interdigital electrode and its preparation method and application with nanometer texture surface - Google Patents
A kind of interdigital electrode and its preparation method and application with nanometer texture surface Download PDFInfo
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- CN108922791A CN108922791A CN201810558621.XA CN201810558621A CN108922791A CN 108922791 A CN108922791 A CN 108922791A CN 201810558621 A CN201810558621 A CN 201810558621A CN 108922791 A CN108922791 A CN 108922791A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002110 nanocone Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims description 43
- 239000002184 metal Substances 0.000 claims description 43
- 239000011521 glass Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 11
- 239000002671 adjuvant Substances 0.000 claims description 10
- 239000006193 liquid solution Substances 0.000 claims description 10
- 238000007747 plating Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 239000003292 glue Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 229920002457 flexible plastic Polymers 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical group [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 238000007639 printing Methods 0.000 claims description 4
- 239000012691 Cu precursor Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 239000011686 zinc sulphate Substances 0.000 claims description 3
- 239000000049 pigment Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 239000000976 ink Substances 0.000 description 35
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 239000002985 plastic film Substances 0.000 description 10
- 229920006255 plastic film Polymers 0.000 description 10
- 239000004642 Polyimide Substances 0.000 description 8
- 238000004070 electrodeposition Methods 0.000 description 8
- 229920001721 polyimide Polymers 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000000089 atomic force micrograph Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 239000007832 Na2SO4 Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000011245 gel electrolyte Substances 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- 238000007641 inkjet printing Methods 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000010147 laser engraving Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- -1 timber Polymers 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The interdigital electrode and its preparation method and application with nanometer texture surface that the present invention relates to a kind of, the interdigital electrode is with pectination cycle pattern and at least one side has the metallic film of the micro-structure of nano-scale, and the micro-structure of the nano-scale is at least one of nanocone, nanometer sheet, nm wall；Preferably, the surface Root Mean Square roughness of the micro-structure one side with nano-scale of the metallic film is 8~200 nm, more preferably 10~100 nm.
Description
Technical field
The interdigital electrode and its preparation method and application with nanometer texture surface that the present invention relates to a kind of, belongs to engineering skill
Art field.
Background technique
Interdigital electrode is a kind of planar with the electrode of pectination cycle pattern, can be used as supercapacitor, lithium electricity
The collector of the devices such as pond, friction nanometer power generator, sensor.
On the one hand, the traditional preparation methods of interdigital electrode include that photoetching, inkjet printing, laser inscription, mask plate auxiliary are true
Sky sputtering etc., and these methods limit extensive, efficient, the inexpensive system of interdigital electrode because step is complicated, with high costs
It is standby.On the other hand, the interdigital electrode that conventional method is prepared, surface are that densification is smooth, limit interdigital electrode and electrode
Charge transmission between material, it is low so as to cause device performance.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of interdigital electrode and its system with nanometer texture surface
Preparation Method and application.
On the one hand, the present invention provides a kind of interdigital electrode with nanometer texture surface, the interdigital electrode be with
Pectination cycle pattern and at least one side have the metallic film of the micro-structure of nano-scale, and the micro-structure of the nano-scale is
At least one of nanocone, nanometer sheet, nm wall；Preferably, the micro-structure one with nano-scale of the metallic film
The surface Root Mean Square roughness in face is 8~200nm, more preferably 10~100nm.
In the present invention, the interdigital electrode with nanometer texture surface is attached on flexible parent metal, is made of metallic film,
It is in pectination cycle pattern in face, at least one side has the micro-structure of nano-scale (for example, nanocone, nanometer sheet, nm wall
Deng), the contact area of interdigital electrode and electrode material can be increased, to significantly improve charge transfer efficiency, improve super electricity
The performance of the devices such as container, lithium battery, friction nanometer power generator, sensor.Wherein, with the increasing of metal film surfaces roughness
Add, improve its charge transfer efficiency to a greater extent, so that the performance of supercapacitor is more preferable.
Preferably, the interdigital electrode with a thickness of 50nm~100 μm.
Preferably, the material of the interdigital electrode is at least one of Ni, Cu and Zn.
Preferably, the interdigital electrode is attached to flexible parent metal surface and make interdigital electrode is at least distally from flexible parent metal
One side have nano-scale micro-structure.The flexible parent metal is one of paper, cloth, flexible plastic.
On the other hand, the present invention also provides a kind of preparation sides of above-mentioned interdigital electrode with nanometer texture surface
Method, including：
After the seal for being carved with interdigital electrode pectination cycle pattern is dipped ink, go out pectination week in the surface imprint of conductive base
The ink logo of phase property pattern, the conductive base be FTO electro-conductive glass or sheet metal, surface Root Mean Square roughness be 8~
200nm, preferably 10~100nm；
The conductive base of the ink logo for printing off interdigital electrode shape is placed in metal front liquid solution after being electroplated,
Removal ink logo is simultaneously transferred to flexible parent metal surface, obtains the interdigital electrode with nanometer texture surface.
In the present invention, after the seal for being carved with interdigital electrode pectination cycle pattern is dipped ink, in conductive base (FTO
Electro-conductive glass or sheet metal, surface Root Mean Square roughness go out the ink of pectination cycle pattern for the surface imprint of 8~200nm)
Pattern.The conductive base of the ink logo for printing off interdigital electrode shape is placed in metal front liquid solution and is electroplated,
Form interdigital electrode.Since conductive base surface itself has the micro-structure of nano-scale, so that the close conduction that plating is formed
The one side of the interdigital electrode of substrate forms the micro-structure of nano-scale.Interdigital electrode is finally transferred to flexible parent metal surface, and
Make the one side of the micro-structure with nano-scale far from flexible parent metal.The method of the present invention includes embossed ink pattern, electronickelling,
Key steps, all operations such as removal ink, electrode transfer carry out in the solution, easy to operate, process stabilizing reliably, cost
It is cheap, it is conducive to promote.
Preferably, the ink is insulation, oleophylic, sticky liquid, ingredient includes alcohol, pigment and resin.
Preferably, the metal front liquid solution is in Ni precursor solution, Cu precursor solution and Zn precursor solution
One kind；Preferably, the metal front liquid solution is metal salt and the mixed aqueous solution that adjuvant is electroplated, and the metal salt is
NiSO4、Ni(NO3)2、CuSO4、Cu(NO3)2、ZnSO4With Zn (NO3)2At least one of, the plating adjuvant is NH4Cl
And H3BO3At least one of.
Also, the concentration of the plating adjuvant is 0.05 preferably, the concentration of the metal salt is 0.1~1.0mol/L
~5mol/L.
Preferably, applying -0.5~-2.0mA cm-2Constant current is electroplated, and the time of plating is 3~60 minutes.
Preferably, using organic reagent remove ink logo, the organic reagent be ethyl alcohol, methanol, isopropanol, acetone and
At least one of toluene.
Preferably, with transferable glue treatment of flexible substrates surface, then covering on one side by the flexible parent metal with transferable glue
The surface of conductive base after being placed on removal ink simultaneously fits closely it, then through separating so that interdigital electrode is transferred to flexible base
Material surface.
Fourth aspect, the present invention provides a kind of supercapacitors comprising above-mentioned interdigital electrode.
Compared with prior art, the present invention has the advantages that：
There are nanometer texture on interdigital electrode surface provided by the present invention, and smooth compared to the densification of conventional method preparation is interdigital
Electrode, can increase the contact area of interdigital electrode and electrode material, to significantly improve charge transfer efficiency, improve super capacitor
The performance of the devices such as device, lithium battery, friction nanometer power generator, sensor；
The preparation method of interdigital electrode provided by the present invention with nanometer texture surface, it is all operation in the solution into
Row.Compared to the methods of traditional photoetching, inkjet printing, laser inscription, mask plate auxiliary vacuum sputtering, process stabilizing is reliable,
It is easy to operate, it is low in cost, it is easy to accomplish, easy to promote and utilize.
Detailed description of the invention
Fig. 1 is the interdigital electrode preparation method flow chart provided by the invention with nanometer texture surface；
Fig. 2 is pectination cycle pattern provided by the invention；
Fig. 3 is seal photo provided by the invention；
Fig. 4 is FTO electro-conductive glass photo of the present invention；
Fig. 5 is the atomic force microscope images of FTO electro-conductive glass of the present invention；
Fig. 6 is the FTO electro-conductive glass photo provided by the invention with ink logo；
Fig. 7 is the FTO electro-conductive glass photo after electronickelling provided by the invention；
Fig. 8 is the FTO electro-conductive glass photo after removal ink provided by the invention；
Fig. 9 is the FTO electro-conductive glass photo provided by the invention for being covered with polyimide plastic film；
Figure 10 is the interdigital electrode provided by the invention for being attached to polyimide plastic film surface；
Figure 11 is the surface scan electron microscopic picture of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 12 is the profile scanning electron microscopic picture of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 13 is the high-resolution surface scanning electron microscopic picture of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 14 is the atomic force microscope images of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 15 is the X ray diffracting spectrum of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 16 is the x-ray photoelectron spectroscopy of the interdigital electrode provided by the invention with nanometer texture surface；
Figure 17 is electro-deposition MnO provided by the invention2Interdigital electrode photo afterwards；
Figure 18 is supercapacitor photo provided by the invention；
Figure 19 is the high-resolution surface scanning electron microscopic picture of the interdigital electrode provided by the invention without nano surface texture；
Figure 20 is the atomic force microscope images of the interdigital electrode provided by the invention without nano surface texture；
Figure 21 is supercapacitor cyclic voltammetry curve provided by the invention：1- is based on the interdigital electrode with nano surface texture
Supercapacitor；Supercapacitor of the 2- based on the interdigital electrode for not having nano surface texture.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
In the present invention, the interdigital electrode with nanometer texture surface is with pectination cycle pattern and at least one side has
Wherein, the micro-structure of nano-scale can be in nanocone, nanometer sheet, nm wall by the metallic film of the micro-structure of nano-scale
It is at least one.In alternative embodiments, the material of interdigital electrode can be at least one of Ni, Cu and Zn.Optional
In embodiment, interdigital electrode with a thickness of 50nm~100 μm.In alternative embodiments, interdigital electrode is attached to flexibility
Substrate surface and make interdigital electrode the one side for being at least distally from flexible parent metal have nano-scale micro-structure.Wherein, flexible
Substrate can be one of paper, cloth, flexible plastic.Wherein, the table of the micro-structure one side with nano-scale of metallic film
Face r.m.s. roughness is 8~200nm, more preferably 10~100nm.
The preparation method of interdigital electrode with nanometer texture surface of the invention includes printing ink pattern, electronickelling, goes
Except key steps such as ink, electrode transfers, have the characteristics that process stabilizing is reliable, easy to operate, low in cost, it is easy to spread to answer
With.Wherein the thickness of interdigital electrode is generally 50nm to 100 μm.As described in Figure 1, illustrate to following exemplary with nanometer texture
The preparation method of the interdigital electrode on surface.
Process seal.The present invention forms comb shape periodic patterns, the molding skill on seal surface using forming technique
Art includes but is not limited to laser engraving, machining, 3D printing etc..The material of seal can be rubber, timber, plastics, stone material etc.
Material can be carved, surface has the pectination cycle pattern of engraving.
Clean conductive base.The conductive base is first placed in acetone, ethyl alcohol and deionized water and is cleaned by ultrasonic 15
Minute, it is subsequently placed in 60~120 DEG C of baking ovens 0.5~6 hour dry.The conductive base include but is not limited to electro-conductive glass,
Sheet metal etc., surface Root Mean Square roughness are 8~200nm, preferably 10~100nm.
Embossed ink pattern.Ink is dipped with seal, imprints out ink logo in surfaces of conductive substrates.The ink is
A kind of insulation, oleophylic, sticky liquid, preferably Sipa SK-6 sign pen inks.
Configure metal front liquid solution.Wherein, metal front liquid solution is Ni precursor solution, Cu precursor solution and Zn
One of precursor solution.The metal front liquid solution is metal salt and the mixed aqueous solution that adjuvant is electroplated.It is wherein golden
Belonging to salt can be NiSO4、Ni(NO3)2、CuSO4、Cu(NO3)2、ZnSO4With Zn (NO3)2At least one of.Adjuvant, which is electroplated, to be
NH4Cl and H3BO3At least one of.In alternative embodiments, the concentration of metal salt can be 0.1~1.0mol/L, plating
The concentration of adjuvant can be 0.05~5mol/L.Using Ni precursor solution as example：Weigh a certain amount of nickel salt (including but not
It is limited to NiSO4、Ni(NO3)2Deng) and plating adjuvant (including but not limited to NH4Cl、H3BO3Deng) it is dissolved in deionized water, it forms dense
Degree is respectively 0.1~1.0mol/L and 0.05~0.5mol/L mixed aqueous solution.
Plating metal.Using electronickelling as example：The conductive base of ink logo will be printed on as working electrode, Ag/
As reference electrode, platinized platinum is used as to electrode for AgCl or saturated calomel electrode.Using galvanostatic method, apply -0.5~-2.0mA
cm-2Constant current is persistently electroplated 3~60 minutes in nickel presoma.Then, conductive base is taken out, deionized water cleaning, 60~
120 DEG C drying 0.5~6 hour.
Remove ink logo.Ink is rinsed using organic reagent, ink is cleaned, the organic reagent includes but unlimited
In ethyl alcohol, acetone, toluene.Then deionized water clean, 60~120 DEG C drying 0.5~6 hour.
Electrode transfer.With transferable glue treatment of flexible substrates, make its band toughness.Adhesive flexible parent metal is covered in
Surfaces of conductive substrates fits closely it, then tears, and the interdigital electrode for being attached to surfaces of conductive substrates is transferred to flexible parent metal
Surface.The transferable glue is preferably 3M Super-75.Wherein, flexible parent metal refers specifically to paper, cloth, flexible plastic
Substrate etc., it is characterized in that flexible folding.
Interdigital electrode is subjected to electro-deposition MnO2, it is then coated with gel electrolyte, obtains supercapacitor.Wherein electro-deposition
MnO2Including：Interdigital electrode is placed in MnO2In precursor solution, 0.5~30 point of electro-deposition under+0.2~+1.2V constant voltage
Clock obtains MnO2Film (with a thickness of 20-1000nm).Wherein, MnO2Precursor solution is Mn (CH3COO)2And Na2SO4Mixing
Aqueous solution.Mn(CH3COO)2Concentration can be 0.01~2.0mol/L.Na2SO4Concentration can be 0.005~0.5mol/L.
In the present invention, also interdigital electrode can be applied to supercapacitor, lithium battery, friction nanometer power generator, sensor
Deng greatly improving the performance of each device.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Basic step is as shown in Figure 1：
(1) seal is processed：The present invention forms comb shape periodic patterns on seal surface using laser ablation method.The comb shape week
Phase property pattern is as shown in Fig. 2, seal is as shown in Figure 3；
(2) conductive base is cleaned：The conductive base is electro-conductive glass (surface Root Mean Square roughness is 13.303nm), specifically
It says as FTO electro-conductive glass on ground.FTO electro-conductive glass is first placed in acetone, ethyl alcohol and deionized water and is cleaned by ultrasonic 15 minutes, so
It is placed in 60 DEG C of baking ovens 2 hours dry.FTO electro-conductive glass after cleaning is as shown in figure 4, its atomic force microscope images such as figure
Shown in 5；
(3) embossed ink pattern：The seal described in step (1) dips ink (Sipa SK-6 signature pen inks), leads in FTO
Electric glass surface imprints out ink logo.FTO electro-conductive glass with ink logo, as shown in Figure 6；
(4) nickel presoma is configured：Weigh a certain amount of NiSO4And NH4Cl is dissolved in deionized water, and composition concentration is respectively 0.1mol/L
With the mixed aqueous solution of 0.05mol/L；
(5) electronickelling：Using the FTO electro-conductive glass for having ink logo in step (3) as working electrode, Ag/AgCl electrode is made
For reference electrode, platinized platinum is used as to electrode.Using galvanostatic method, application -1.5mA cm-2Constant current, the nickel forerunner described in step 4
It is persistently electroplated in body 10 minutes.Then, conductive base is taken out, deionized water cleaning, 60 DEG C drying 1 hour.After electronickelling
FTO electro-conductive glass is as shown in Figure 7；
(6) ink logo is removed：Ink is rinsed using ethyl alcohol, ink is cleaned.Then deionized water is cleaned, and 60 DEG C of dryings 1 are small
When.FTO electro-conductive glass after removing ink logo is as shown in Figure 8；
(7) electrode shifts：Polyimide plastic film is handled with the transferable glue of 3M Super-75 type, makes its band toughness.By band
The polyimide plastic film of viscosity is covered in gained FTO conductive glass surface in step 6, fits closely it (such as Fig. 9 institute
Show), it then tears, the interdigital electrode for being attached to FTO conductive glass surface is transferred to polyimide plastic film.It is attached to polyamides
The interdigital electrode of imines Plastic film surface is as shown in Figure 10.Figure 11 and Figure 12 is respectively the interdigital electricity observed under scanning electron microscope
Pole, electrode width 1.4mm, spacing is 300 μm, with a thickness of 200nm.Figure 13 is the surface shape observed under surface sweeping Electronic Speculum
Looks, the micro-structure of nano-scale are present in interdigital electrode surface.Figure 14 is the surface topography observed under atomic force microscope, table
Face r.m.s. roughness is 10.876nm.Figure 15 is the X ray diffracting spectrum of interdigital electrode, it can be verified that interdigital electrode ingredient is gold
Belong to nickel.Figure 16 is the x-ray photoelectron spectroscopy of interdigital electrode, can illustrate have nickel oxide to be present in interdigital electrode surface；
(8) MnO is configured2Presoma：Weigh a certain amount of Mn (CH3COO)2And Na2SO4It is dissolved in deionized water, concentration is
0.1mol/L；
(9) electro-deposition MnO2：The interdigital electrode for being attached to polyimide plastic film surface is working electrode, Ag/AgCl electrode
As reference electrode, platinized platinum is used as to electrode.Application+0.6V constant voltage, the MnO described in step 82Continue electro-deposition in presoma
4 minutes.Then, interdigital electrode is taken out, deionized water cleaning, 60 DEG C drying 1 hour.Electro-deposition MnO2Interdigital electrode afterwards is such as
Shown in Figure 17, MnO2Uniform fold is on interdigital electrode surface, wherein MnO2Film with a thickness of 200nm；
(10) gel electrolyte is configured：Weigh 1.5g sodium carboxymethylcellulose, 3.0g Na2SO4It is dissolved in 25mL deionized water, is added
To 90 DEG C, continuing magnetic force stirs 3 hours heat, forms classifying gel shape substance, cooled to room temperature；
(11) it is coated with gel electrolyte：Gel electrolyte described in step 10 is coated on electro-deposition MnO described in step 92Afterwards
Interdigital electrode surface and step 7 in interdigital electrode surface, formed supercapacitor.Supercapacitor is as shown in figure 18.
Comparative example 1
Polyimide plastic film is handled using the transferable glue of 3M Super-75 type, makes its band toughness.By adhesive polyamides
Imines plastic film is covered in the polyimide plastic film table that interdigital electrode is stained with obtained in the step of embodiment 1 (7)
Then face is torn, so that the one side of the micro-structure with nano-scale of interdigital electrode, close to flexible parent metal, surface does not have table
The one side of face nanometer texture is far from flexible parent metal.The high-resolution surface scanning electron microscope of interdigital electrode without nano surface texture
Picture and atomic force microscope images difference are as illustrated in figures 19 and 20.With the fork with nano surface texture in step (7)
Refer to that electrode is compared, the electrode surface is more smooth, and surface Root Mean Square roughness is only 5.005nm.It prepares on this basis super
Capacitor obtains the supercapacitor of the interdigital electrode without nano surface texture referring to embodiment 1.
Figure 21 is the cyclic voltammetry curve of supercapacitor.Based on provided by the invention interdigital with nano surface texture
The supercapacitor capacitance of electrode is 4.15mF cm-2, the super capacitor based on the interdigital electrode for not having nano surface texture
Device capacitance is 2.96mF cm-2.It can be seen that the interdigital electrode with nano surface texture can increase interdigital electrode and electrode
The contact area of material improves the performance of supercapacitor to significantly improve charge transfer efficiency.
Claims (10)
1. a kind of interdigital electrode with nanometer texture surface, which is characterized in that the interdigital electrode is with pectination cycle
Pattern and at least one side have the metallic film of the micro-structure of nano-scale, and the micro-structure of the nano-scale is nanocone, receives
At least one of rice piece, nm wall；Preferably, the surface of the micro-structure one side with nano-scale of the metallic film is equal
Root mean square roughness is 8~200 nm, more preferably 10~100 nm.
2. interdigital electrode according to claim 1, which is characterized in that the interdigital electrode with a thickness of the μ of 50 nm~100
m。
3. interdigital electrode according to claim 1 or 2, which is characterized in that the material of the interdigital electrode is Ni, Cu and Zn
At least one of.
4. interdigital electrode according to any one of claim 1-3, which is characterized in that the interdigital electrode is attached to flexibility
Substrate surface and make interdigital electrode the one side for being at least distally from flexible parent metal have nano-scale micro-structure；Preferably, institute
Stating flexible parent metal is one of paper, cloth, flexible plastic.
5. a kind of preparation method of such as interdigital electrode of any of claims 1-4 with nanometer texture surface,
It is characterized in that, including：
After the seal for being carved with interdigital electrode pectination cycle pattern is dipped ink, go out pectination week in the surface imprint of conductive base
The ink logo of phase property pattern, the conductive base are FTO electro-conductive glass or sheet metal, and surface Root Mean Square roughness is 8~200
Nm, preferably 10~100 nm；
The conductive base of the ink logo for printing off interdigital electrode shape is placed in metal front liquid solution after being electroplated,
Removal ink logo is simultaneously transferred to flexible parent metal surface, obtains the interdigital electrode with nanometer texture surface.
6. preparation method according to claim 5, which is characterized in that the ink is insulation, oleophylic, sticky liquid,
Ingredient includes alcohol, pigment and resin.
7. preparation method according to claim 5 or 6, which is characterized in that the metal front liquid solution is Ni presoma
One of solution, Cu precursor solution and Zn precursor solution；Preferably, the metal front liquid solution is metal salt and electricity
The mixed aqueous solution of adjuvant is plated, the metal salt is NiSO4、Ni(NO3)2、CuSO4、Cu(NO3)2、ZnSO4With Zn (NO3)2In
At least one, the plating adjuvant be NH4Cl and H3BO3At least one of；It is highly preferred that the concentration of the metal salt
Concentration for 0.1~1.0mol/L, the plating adjuvant is 0.05~5mol/L.
8. the preparation method according to any one of claim 5-7, which is characterized in that apply -0.5~-2.0 mA cm-2
Constant current is electroplated, and the time of plating is 3~60 minutes.
9. the preparation method according to any one of claim 5-8, which is characterized in that with transferable glue treatment of flexible substrates
Then surface by the surface for the conductive base of the flexible parent metal with transferable glue being covered in after removal ink on one side and keeps it tight
Closely connected conjunction, then through separating so that interdigital electrode is transferred to flexible parent metal surface.
10. a kind of super capacitor comprising the interdigital electrode of any of claims 1-4 with nanometer texture surface
Device.
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| CN110010371A (en) * | 2019-02-28 | 2019-07-12 | 北京大学 | A kind of micro super capacitor and its manufacturing method towards Universal flexible substrate |
| CN110085444A (en) * | 2019-04-23 | 2019-08-02 | 西北工业大学深圳研究院 | Flexible miniature supercapacitor and preparation method thereof based on electrochemistry increasing material manufacturing |
| CN110085445A (en) * | 2019-05-23 | 2019-08-02 | 南京邮电大学 | A kind of flexible super capacitor and preparation method thereof |
| CN111505065A (en) * | 2020-04-20 | 2020-08-07 | 河北工业大学 | Interdigital counter electrode type flexible touch sensor based on super-capacitor sensing principle and preparation method thereof |
| CN111596135A (en) * | 2020-05-29 | 2020-08-28 | 中国科学院微电子研究所 | Method for analyzing resistance characteristics of electrodeposited gold structure |
| CN113162477A (en) * | 2021-02-05 | 2021-07-23 | 西安交通大学 | Liquid drop energy collecting device and method based on thin film interdigital electrode |
| CN116261388A (en) * | 2023-05-16 | 2023-06-13 | 北京中科飞鸿科技股份有限公司 | Method for preparing interdigital electrode for semiconductor package and semiconductor package |
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| CN110010371A (en) * | 2019-02-28 | 2019-07-12 | 北京大学 | A kind of micro super capacitor and its manufacturing method towards Universal flexible substrate |
| CN110085444A (en) * | 2019-04-23 | 2019-08-02 | 西北工业大学深圳研究院 | Flexible miniature supercapacitor and preparation method thereof based on electrochemistry increasing material manufacturing |
| CN110085445A (en) * | 2019-05-23 | 2019-08-02 | 南京邮电大学 | A kind of flexible super capacitor and preparation method thereof |
| CN110085445B (en) * | 2019-05-23 | 2021-04-06 | 南京邮电大学 | Flexible super capacitor and preparation method thereof |
| CN111505065A (en) * | 2020-04-20 | 2020-08-07 | 河北工业大学 | Interdigital counter electrode type flexible touch sensor based on super-capacitor sensing principle and preparation method thereof |
| CN111596135A (en) * | 2020-05-29 | 2020-08-28 | 中国科学院微电子研究所 | Method for analyzing resistance characteristics of electrodeposited gold structure |
| CN113162477A (en) * | 2021-02-05 | 2021-07-23 | 西安交通大学 | Liquid drop energy collecting device and method based on thin film interdigital electrode |
| CN116261388A (en) * | 2023-05-16 | 2023-06-13 | 北京中科飞鸿科技股份有限公司 | Method for preparing interdigital electrode for semiconductor package and semiconductor package |
| CN116347971A (en) * | 2023-05-24 | 2023-06-27 | 北京中科飞鸿科技股份有限公司 | Semiconductor package for radio frequency front end |
| CN116347971B (en) * | 2023-05-24 | 2023-08-08 | 北京中科飞鸿科技股份有限公司 | Semiconductor package for radio frequency front end |
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