CN107768020B - The preparation method of formula of taking root fexible film electrode - Google Patents
The preparation method of formula of taking root fexible film electrode Download PDFInfo
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- CN107768020B CN107768020B CN201710761415.4A CN201710761415A CN107768020B CN 107768020 B CN107768020 B CN 107768020B CN 201710761415 A CN201710761415 A CN 201710761415A CN 107768020 B CN107768020 B CN 107768020B
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- fexible film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 45
- 239000011347 resin Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 238000002242 deionisation method Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 238000013461 design Methods 0.000 claims abstract description 3
- 238000005554 pickling Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000002929 anti-fatigue Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 229910017611 Ag(NH3)2 Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses the preparation methods for formula fexible film electrode of taking root, and are related to field of material engineering technology.The present invention includes: to carry out pit design in the surface of test piece for needing to make electrode first；Perfluorinated sulfonic resin coating is prepared on surface, and is full of pit；Coating pickling, deionization are washed, impurity and heteroion are removed；Test specimen is impregnated the regular hour in the solution of metal salt, carries out ion exchange；Test specimen is taken out, after deionization washing, impregnates in water, reducing agent is added, carry out chemical plating, obtains the internal fexible film electrode containing a large amount of metallics, electrode prepared by the present invention has antifatigue, and flexibility is strong, and has the advantages that well attached ability.
Description
Technical field
The present invention relates to field of material engineering technology, more particularly to the preparation method for formula fexible film electrode of taking root.
Background technique
With the growing of flexible electronic device and development, flexible energy storage device has become the heat of the research in energy storage field
Point.Wherein, core component of the electrode material as energy storage device, to become the research emphasis of researcher and receive
Extensive concern.Currently, the preparation method of fexible film electrode mainly has vacuum filtration process, cladding process, in situ synthesis;Mainly
Material includes metallic film, graphene etc., these materials cannot meet the performance requirements such as antifatigue, attachment, flexibility simultaneously.
To sum up, in the prior art, lack it is a kind of can meet simultaneously it is antifatigue, have flexibility, and have it is well attached
The electrode material of ability.
Summary of the invention
The present invention provides the preparation method of formula fexible film electrode of taking root, and can prepare a kind of antifatigue, has flexibility,
And the electrode material with well attached ability.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
The preparation method of formula of taking root fexible film electrode, comprising:
S1, pit is made on the surface of test specimen, obtains the surface of test piece that there is pit to design；
S2, perfluorinated sulfonic resin is covered in the surface of test piece, fills up the pit, obtain perfluorinated sulfonic resin painting
Layer, perfluorinated sulfonic resin can store metal ion；
S3, pickling, deionization washing are successively carried out to the test specimen, remove impurity and heteroion；
S4, the test specimen is impregnated in the solution of metal salt, carries out ion exchange, metal target cation is stored in
In resin, test specimen is then taken out, carries out deionization washing；
S5, the test specimen is impregnated in water, reducing agent is added, carries out chemical plating, obtains inside from electrode surface of test piece
The fexible film electrode containing a large amount of metallics of growth, formula of as taking root fexible film electrode.
Further, in the pit volume of perfluorinated sulfonic resin account for the 80% of the perfluorinated sulfonic resin total volume with
On.
Further, the surface of test piece is plane.
Further, metal is the metal that can be stabilized in air, including platinum, nickel, silver, gold in the metal salt.
The beneficial effects of the present invention are:
Pit is arranged in surface of test piece in the present invention, and perfluorinated sulfonic resin is stored in pit as root system, utilizes perfluor sulphur
Key reaction raw material displacement metallic of the acid resin as electrode material, because perfluorinated sulfonic resin not only covers test specimen table
Face also largely exists in the pit of surface of test piece, so that the amount of metal particles displaced significantly increases, therefore improves electrode
Adhesive ability and electrode electric conductivity；Perfluorinated sulfonic resin material is high-molecular organic material, tough and tensile softness, fatigue resistance
Can be good, because of the pit that perfluorinated sulfonic resin is covered and is filled with inside the surface and test specimen of test specimen, electrode has good
Flexibility.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the schematic diagram of the embodiment of the present invention.
1- perfluorinated sulfonic resin film, 2- test specimen.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, With reference to embodiment to this
Invention is described in further detail.
Embodiment 1: 8g perfluor sulfoacid resin solution (DuPont, NafionTM) is cast in into the good pit of cloth
Surface of test piece, as shown in Figure 1, test specimen is put into drying box, temperature is 80 DEG C, at perfluor after the volatilization of perfluorosulfonic acid resin solution solvent
Sulfonate resin film, depression volume are the 81% of perfluorinated sulfonic resin total volume.Test specimen is put into the hydrochloric acid solution of 2N/L and boils 30 points
Then clock is impregnated 1 hour, with going after the impurity in membrane removal and ion to immerse deionized water by test specimen after taking-up in deionized water
Immerse the chloroplatinous acid amine ([Pt (NH of 2mg Pt/ml3)4]Cl2), a small amount of ammonium hydroxide (5%) is added to eliminate acidity, PH is 10 left
The right side, soaking time 24 hours.It after test specimen is cleaned with deionized water, puts it into deionized water, is placed in 60 degrees Celsius
In water bath with thermostatic control, the sodium borohydride solution of the 5wt% of 4ml was added every 30 minutes, 3 hours take out cleaning, taken root
Formula fexible film electrode.
Embodiment 2: 8g perfluor sulfoacid resin solution (DuPont, NafionTM) is cast in into the good pit of cloth
Surface of test piece is put into drying box, and temperature is 80 DEG C, recessed at perfluorinated sulfonic resin film after the volatilization of perfluor sulfoacid resin solution solvent
Pit body product is the 82% of perfluorinated sulfonic resin total volume.Test specimen is put into the hydrochloric acid solution of 2N/L and boils 30 minutes to go in membrane removal
Impurity and ion after immerse deionized water, impregnate 1 hour in deionized water, electrode immersed into 0.01 mol/L after taking-up
[Ag(NH3)2] NO3Solution, soaking time are 24 hours, and after being cleaned with deionized water, test specimen is put into deionized water, and
It is placed in 60 degrees Celsius of water bath with thermostatic control, the sodium borohydride solution of the 5wt% of 4ml was added every 30 minutes, is taken out after 3 hours
Cleaning, obtains formula fexible film electrode of taking root.
Embodiment 3: 8g perfluor sulfoacid resin solution (DuPont, NafionTM) is cast in into the good pit of cloth
Surface of test piece is put into drying box, and temperature is 80 DEG C, and at perfluorinated sulfonic resin film after solvent volatilization, depression volume is perfluorinated sulfonic acid
The 80% of resin total volume.Test specimen is put into the impurity and ion for boiling that 30 minutes go in membrane removal in the hydrochloric acid solution of 2N/L, is then soaked
Enter in deionized water 1 hour, test specimen is immersed to the NiSO of 0.05 mol/L after taking-up4Solution, soaking time 24 are hour.Perfluor
After sulfonate resin is cleaned with deionized water, test specimen is put into deionized water, is placed in 87 degrees Celsius of water bath with thermostatic control, often
The NaH of the 2wt% of 4ml was added every 15 minutes2PO2Solution, 3 hours take out cleaning, obtain formula fexible film electrode of taking root.
Embodiment 4: 8g perfluor sulfoacid resin solution (DuPont, NafionTM) is cast in into the good pit of cloth
Surface of test piece is put into drying box, and temperature is 80 DEG C, recessed at perfluorinated sulfonic resin film after the volatilization of perfluor sulfoacid resin solution solvent
Pit body product is the 84% of perfluorinated sulfonic resin total volume.Test specimen is put into the hydrochloric acid solution of 2N/L and boils 30 minutes to go in membrane removal
Impurity and ion after immerse deionized water, impregnate 1 hour in deionized water, test specimen immersed into 0.01 mol/L after taking-up
[Au[phen]Cl2] Cl solution, soaking time is 24 hours.After test specimen is cleaned with deionized water, deionized water is put it into
In, it is placed in 60 degrees Celsius of water bath with thermostatic control, the Na of 2wt% is added2SO3Solution, 3 hours take out cleaning, obtain the formula of taking root
Fexible film electrode.
See Table 1 for details for formula of taking root made from above-described embodiment fexible film electrode parameter.
The tensile strength ratio of 1 embodiment test specimens of table and conductive ratio
| Embodiment | Sheet resistance (Ω) | Film thickness direction resistance (Ω) |
| 1 | < 1 | < 0.1 |
| 2 | < 1 | < 0.1 |
| 3 | < 1 | < 0.1 |
| 4 | < 1 | < 0.1 |
The obtained of 1-4 takes root formula fexible film electrode parameter it is found that using prepared by the present invention through the foregoing embodiment
Formula of taking root fexible film electrode has preferable electric conductivity.
To sum up, the beneficial effects of the present invention are:
Pit is set in test specimen, perfluorinated sulfonic resin is stored in pit as root system, by increasing perfluorinated sulfonic resin
Volume increases the quantity of displacement and storage metal ion, so that electrode has good adhesive ability；
After reducing agent is added, metallic, ingrowing, a large amount of intensive metallics are restored near coating surface
Provide the electric conductivity of electrode；
Perfluorinated sulfonic resin is covered and filled in surface of test piece and pit, and it is good that perfluorinated sulfonic resin has electrode
Flexibility.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (4)
1. the preparation method of formula of taking root fexible film electrode, which comprises the following steps:
S1, pit is made on the surface of test specimen, obtains the surface of test piece that there is pit to design；
S2, perfluorinated sulfonic resin is covered in the surface of test piece, fills up the pit, obtain perfluorinated sulfonic resin coating；
S3, pickling, deionization washing are successively carried out to the test specimen；
S4, the test specimen is impregnated in the solution of metal salt, is then taken out, carry out deionization washing；
S5, the test specimen is impregnated in water, reducing agent is added, carries out chemical plating, obtains from the surface of test piece ingrowing
The fexible film electrode containing a large amount of metallics, obtain formula fexible film electrode of taking root.
2. the preparation method of formula fexible film electrode according to claim 1 of taking root, which is characterized in that complete in the pit
The volume of perfluorosulfonic acid resin accounts for 80% or more of the perfluorinated sulfonic resin total volume.
3. the preparation method of formula fexible film electrode according to claim 1 of taking root, which is characterized in that in the S2,
The surface of test piece is plane.
4. the preparation method of formula fexible film electrode according to claim 1 of taking root, which is characterized in that in the metal salt
Metal is the metal that can be stabilized in air, including platinum, nickel, silver, gold.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710761415.4A CN107768020B (en) | 2017-08-30 | 2017-08-30 | The preparation method of formula of taking root fexible film electrode |
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|---|---|---|---|
| CN201710761415.4A CN107768020B (en) | 2017-08-30 | 2017-08-30 | The preparation method of formula of taking root fexible film electrode |
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| CN107768020A CN107768020A (en) | 2018-03-06 |
| CN107768020B true CN107768020B (en) | 2019-10-22 |
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| US20030036483A1 (en) * | 2000-12-06 | 2003-02-20 | Arendt Paul N. | High temperature superconducting thick films |
| CN101626083B (en) * | 2009-07-31 | 2011-01-05 | 重庆大学 | Method for preparing proton exchange membrane fuel cell electrode with high catalyst utilization ratio |
| CN102522570A (en) * | 2011-12-29 | 2012-06-27 | 新源动力股份有限公司 | Method for preparing enhanced membrane electrode (MEA) of proton exchange membrane fuel cell (PEMFC) |
| KR20160091512A (en) * | 2015-01-23 | 2016-08-03 | 전북대학교산학협력단 | Manufacturing method of carbon black sheet for PEMFC using electrophoretical deposition, carbon black sheet and MEA for fuel cell prepared by using this sheet |
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