CN106191967B - A kind of process of the doped graphene in polypyrrole coating - Google Patents
A kind of process of the doped graphene in polypyrrole coating Download PDFInfo
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- CN106191967B CN106191967B CN201610523826.5A CN201610523826A CN106191967B CN 106191967 B CN106191967 B CN 106191967B CN 201610523826 A CN201610523826 A CN 201610523826A CN 106191967 B CN106191967 B CN 106191967B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 49
- 238000000576 coating method Methods 0.000 title claims abstract description 40
- 239000011248 coating agent Substances 0.000 title claims abstract description 39
- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004070 electrodeposition Methods 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 15
- 229910001220 stainless steel Inorganic materials 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 238000003786 synthesis reaction Methods 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 4
- 238000000429 assembly Methods 0.000 claims description 4
- 230000000712 assembly Effects 0.000 claims description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229940075397 calomel Drugs 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 238000006392 deoxygenation reaction Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002848 electrochemical method Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Abstract
The invention belongs to composite coating corrosion-resistant field, in particular to a kind of process of the doped graphene in polypyrrole coating.This method specifically: graphene is prepared using liquid phase stripping method first, deionized water then is added in this graphene and is ultrasonically treated until being uniformly dispersed, obtain graphene suspension, then a certain amount of pyrrole monomer being added in this suspension together with surfactant under the conditions of being protected from light and being stirred makes it after completely dissolution, it is passed through a period of time nitrogen and removes dissolved oxygen acquisition synthetic solvent in solution, finally by metal surface electro-deposition polypyrrole/graphene composite coating of cyclic voltammetry under the conditions of being protected from light after the pre-treatment.The technical method technical process is simple, uniformly and fine and close by the polypyrrole coating after doped graphene, can significantly improve the corrosion resisting property of metallic matrix.
Description
Technical field
The invention belongs to composite coating corrosion-resistant field, in particular to a kind of technique of the doped graphene in polypyrrole coating
Method.
Background technique
The polyaniline coating electrochemically synthesized in acid medium from DeBerry discovery in 1985 can make stainless steel
Surface passivation and since improving its protective performance, the corrosion resistance and mechanism of electroconductive polymer coating are constantly subjected to people's
Concern.Since conducting polymer materials have electric conductivity and corrosion resistance concurrently, have in anticorrosive metal field boundless
Application prospect.However polymer coating is inevitably present some microdefects, affects coating in electrodeposition process
Compactness, during metal and alloy long service, corrosive medium can penetrate into matrix surface along these defects, right
Matrix causes corrosion failure, therefore how to reduce porosity under the premise of not influencing polymer coating conductivity and increase coating cause
Close property is the key technology for needing to solve at present.
Graphene is the two dimensional crystal of only monoatomic thickness, and each carbon atom is all made of sp in graphene2Hydridization, and tribute
It offers a remaining p orbital electron and forms a big pi bond, pi-electron can move freely, and assign graphene excellent electric conductivity.
Summary of the invention
The present invention is by graphene and polypyrrole coating material with high-specific surface area, excellent mechanical performances and conductive capability
Carry out compound, the conductive multifunctional composite with excellent corrosion-proof performance of acquisition, before not reducing polymer coating conductivity
The porosity for reducing coating as far as possible is put, the advantage at anti-corrosion and conductive aspect of two kinds of materials is given full play to, avoids simultaneously
Chemical method prepares the complex process of polypyrrole composite coating, directly through electrochemical method in graphene and pyrrole monomer solution
Synthesize PPy/ graphene composite coating.
Preparation step of the invention are as follows:
(1) preparation of graphene
Graphene is prepared using liquid phase stripping method, technique are as follows: prepares graphite powder and dimethylformamide (DMF)
At 0.2mg/mL suspension, supernatant liquor is taken after 3~4h of ultrasonic disperse and is centrifuged, is dried, obtains graphene powder；
(2) preparation of Synthesis liquid
Graphene powder obtained in step (1) is added in deionized water and is ultrasonically treated 30~60min, is dispersed
Uniform graphene suspension；Pyrrole monomer and lauryl sodium sulfate (SDS) are then added to above-mentioned graphene in suspension,
The suspension, which is placed in progress magnetic agitation processing in light resistant container, again is sufficiently uniformly dissolved pyrrole monomer, finally in the suspension
It is passed through nitrogen in liquid and carries out deoxygenation processing to prevent pyrrole monomer oxidation, and continuing ultrasonic treatment makes graphene in the suspension
In it is fully dispersed, obtain Synthesis liquid,
In Synthesis liquid, graphene concentration is 5mg/mL~20mg/mL, and pyrrole monomer concentration is 20mg/mL~30mg/mL,
Lauryl sodium sulfate (SDS) concentration is 35mg/mL~55mg/mL,
In Synthesis liquid process for preparation, the stirring of pyrrole monomer and course of dissolution (are being kept away in the opaque container of black
Under the conditions of light) it carries out, after being uniformly dissolved, passes first into 10~20min of nitrogen and carry out deoxygenation processing, be further continued for being ultrasonically treated
10~20 minutes, it is ensured that graphene is sufficiently mixed with pyrrole monomer and is uniformly dispersed；
(3) electro-deposition composite coating
Electro-deposition is carried out by electrochemical cyclic voltammetry using three electrode assemblies under the conditions of being protected from light, wherein reference electrode
For saturated calomel electrode, auxiliary electrode is platinized platinum, and working electrode is metal stainless steel sample, and electrolyte is to obtain in step (2)
Synthesis liquid, electrodeposition temperature is 0~10 DEG C, and graphene/polypyrrole composite coating after electro-deposition clean with deionized water, does
It is dry,
Working electrode is metal stainless steel sample using preceding carrying out the following processing: being 10mm × 10mm stainless steel by surface area
Copper conductor is burn-on as contact conductor in sheet material one end, and the inactive face of sample is encapsulated with epoxy resin, and with No. 400-800
Sand paper polishing, acetone clean oil removing, drying,
In electrochemical cyclic voltammetry, scanning potential region is -0.2~1.0VSCE, sweep speed 30mV/s, circulation
10-20 times, the coating layer thickness of acquisition is 5-15um.
The beneficial effects of the present invention are: the present invention overcomes polypyrrole coating compactness obtained in the prior art
Difference, the disadvantages of porosity is big, by the intervention of graphene, are effectively filled with the defect of polypyrrole coating.Further, since with height
The graphene of electric conductivity it is compound, the electric conductivity of polypyrrole coating is also significantly improved.
Detailed description of the invention
Fig. 1 is embodiment 1 and the polymer coating sample surface morphology obtained of embodiment 3；Wherein (a) is pyrrole monomer
The pure PPy coating that aqueous solution is obtained by electrochemical method (b) is obtained for graphene/pyrroles's suspension by electrochemical method
PPy/ graphene composite coating；
It can be seen that the compactness of PPy/ graphene composite coating is significantly improved compared to pure PPy coating, this
It is since the intervention of graphene can be effective as the filling of polypyrrole coating defect, thus the more uniform cause of coating obtained
It is close.
Specific embodiment
Embodiment 1
2.5g pyrrole monomer and 4.3g lauryl sodium sulfate (SDS) are added in 100mL water, the stirring of pyrrole monomer and
Course of dissolution carries out (i.e. under the conditions of being protected from light) in the opaque container of black, and nitrogen 18min progress is passed through after being uniformly dissolved
Deoxygenation processing obtains Synthesis liquid to prevent pyrrole monomer oxidation；
It is that copper conductor is burn-on as contact conductor in 10mm × 10mm stainless steel sheet material one end, and is sealed with epoxy resin using area
The inactive face for filling sample cleans oil removing with the polishing of 400-800 sand paper, acetone, is dried,
Controlling electrodeposition temperature by water-bath under the conditions of being protected from light is 5 DEG C, and it is heavy to carry out electricity by electrochemical cyclic voltammetry
Product experiment, electrodeposition process use three electrode assemblies: saturated calomel electrode is made auxiliary electrode as reference electrode, platinized platinum, is passed through
For the metal stainless steel substrates of above-mentioned processing as working electrode, electrolyte is Synthesis liquid obtained above, scanning potential region is-
0.2~1.0VSCE, sweep speed 30mV/s, circulation 10 times, the polypyrrole coating after electro-deposition is cleaned with deionized water.
The obtained polypyrrole coating surface uniformity of this example is poor (such as attached drawing 1 (a)), relative to matrix stainless steel,
In acidity (0.3mol/L H2SO4) corrosion potential improves 140mV in environment, corrosion rate falls to 0.4mm/a from 1.1mm/a.
Embodiment 2
1.0g graphene is added in 100mL deionized water and is ultrasonically treated 60min, it is outstanding to obtain finely dispersed graphene
2.5g pyrrole monomer and 4.3g lauryl sodium sulfate (SDS) are then added to above-mentioned graphene in suspension by supernatant liquid, then should
Suspension, which is placed in progress magnetic agitation processing in light resistant container, is sufficiently uniformly dissolved pyrrole monomer, finally leads in the suspension
Enter nitrogen 18min and carry out deoxygenation processing to prevent pyrrole monomer oxidation, and continuing ultrasonic treatment 20min keeps graphene outstanding at this
It is fully dispersed in supernatant liquid, obtain Synthesis liquid；
The pretreatment and electro-deposition of working electrode metal stainless steel substrates prepare the technique of composite coating with embodiment 1.
Compared with Example 1, surface uniformity obtains the present embodiment polypyrrole/graphene composite coating obtained
(such as attached drawing 1 (b)) is significantly improved, relative to matrix stainless steel, in acidity (0.3mol/L H2SO4) corrosion potential mentions in environment
High 210mV, corrosion rate fall to 0.2mm/a from 1.1mm/a.
Embodiment 3
2.0g graphene is added in 100mL deionized water and is ultrasonically treated 60min, it is outstanding to obtain finely dispersed graphene
2.5g pyrrole monomer and 4.3g lauryl sodium sulfate (SDS) are then added to above-mentioned graphene in suspension by supernatant liquid, then should
Suspension, which is placed in progress magnetic agitation processing in light resistant container, is sufficiently uniformly dissolved pyrrole monomer, finally leads in the suspension
Enter nitrogen 18min and carry out deoxygenation processing to prevent pyrrole monomer oxidation, and continuing ultrasonic treatment 20min keeps graphene outstanding at this
It is fully dispersed in supernatant liquid, obtain Synthesis liquid；
The pretreating process of working electrode metal stainless steel substrates is the same as embodiment 1.
Controlling electrodeposition temperature by water-bath under the conditions of being protected from light is 5 DEG C, and it is heavy to carry out electricity by electrochemical cyclic voltammetry
Product experiment, electrodeposition process use three electrode assemblies: saturated calomel electrode is made auxiliary electrode as reference electrode, platinized platinum, is passed through
For the metal stainless steel substrates of above-mentioned processing as working electrode, electrolyte is Synthesis liquid obtained above, scanning potential region is-
0.2~1.0VSCE, sweep speed 30mV/s, circulation 15 times, the polypyrrole coating after electro-deposition is cleaned with deionized water.
The uniformity and compactness of the present embodiment polypyrrole/graphene composite coating obtained are preferable, relative to matrix
Stainless steel, in acidity (0.3mol/L H2SO4) corrosion potential improves 273mV in environment, corrosion rate is fallen to from 1.1mm/a
0.11mm/a。
Claims (1)
1. a kind of process of the doped graphene in polypyrrole coating, it is characterised in that: the step of the method is,
(1) preparation of graphene；
Graphene is prepared using liquid phase stripping method, and technique is to be configured to graphite powder and dimethylformamide (DMF)
0.2mg/mL suspension takes supernatant liquor after 3~4h of ultrasonic disperse and is centrifuged, is dried, obtains graphene powder；
(2) preparation of Synthesis liquid；
Graphene obtained in step (1) is added in deionized water and is ultrasonically treated 30~60min, obtains finely dispersed stone
Black alkene suspension；Then pyrrole monomer and lauryl sodium sulfate are added in above-mentioned graphene suspension, then by the suspension
Liquid, which is placed in light resistant container, carries out magnetic agitation, nitrogen is finally passed through into the suspension, and continue to be ultrasonically treated, obtained
Synthesis liquid, graphene concentration are 5mg/mL~20mg/mL, and pyrrole monomer concentration is 20mg/mL~30mg/mL, dodecyl sulphur
Sour na concn is 35mg/mL~55mg/mL, and being passed through the nitrogen time is 10~20min, continues to be ultrasonically treated after being passed through nitrogen
Time be 10~20min；
(3) electro-deposition composite coating；
Electro-deposition is carried out by electrochemical cyclic voltammetry using three electrode assemblies under the conditions of being protected from light, wherein reference electrode is full
And calomel electrode, auxiliary electrode are platinized platinum, working electrode is metal stainless steel sample, and electrolyte is to close obtained in step (2)
At liquid, electrodeposition temperature is 0~10 DEG C, and graphene/polypyrrole composite coating after electro-deposition is cleaned with deionized water, is dry；
In the electrochemical cyclic voltammetry, scanning potential region is -0.2~1.0VSCE, sweep speed 30mV/s, circulation 10-20
It is secondary；The working electrode is metal stainless steel sample using preceding carrying out the following processing: being 10mm × 10mm stainless steel by surface area
Copper conductor is burn-on as contact conductor in sheet material one end, and the inactive face of sample is encapsulated with epoxy resin, and with No. 400-800
Sand paper polishing, acetone clean oil removing, drying.
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| CN107254705B (en) * | 2017-06-09 | 2020-12-11 | 常州大学 | Preparation process of nano TiN-PANI composite conductive polymer coating |
| CN109786124B (en) * | 2018-12-05 | 2024-04-05 | 南通南京大学材料工程技术研究院 | Flexible asymmetric supercapacitor and preparation method thereof |
| CN111128472B (en) * | 2019-12-17 | 2021-04-06 | 浙江大学 | Method for preparing conductive polymer film on graphene surface through electrodeposition |
| CN111593347A (en) * | 2020-06-02 | 2020-08-28 | 太原理工大学 | Flexible composite film material and preparation method thereof |
| CN113789554B (en) * | 2021-08-16 | 2022-12-02 | 华中科技大学 | Magnesium alloy with protective coating and preparation method and application thereof |
| CN114307674B (en) * | 2021-12-28 | 2022-12-09 | 北京林业大学 | Preparation method of special hydrophilic and hydrophobic membrane based on electric gradient morphology regulation |
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| CN104593847A (en) * | 2015-01-15 | 2015-05-06 | 青岛华高能源科技有限公司 | Preparation method of metal surface graphene/polypyrrole protective composite film |
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| CN103454333B (en) * | 2013-09-06 | 2015-05-13 | 南京理工大学 | Electrochemical detection method for pesticide imidacloprid based on polypyrrole/reduced graphene oxide (PPy/RGO) modified glassy carbon electrode |
| CN104711655B (en) * | 2015-03-26 | 2017-06-09 | 兰州明仁智能科技有限公司 | A kind of method that graphene-based antiseptic wearable coat is prepared in Mg alloy surface by liquid phase electrophoretic deposition |
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| "高质量石墨烯分散液的制备";唐晶晶;《中国优秀硕士学位论文全文数据库（电子期刊） 工程科技I辑》;20130615;第B020-200页 |
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Application publication date: 20161207 Assignee: Senbiao Technology Services (Shandong) Co.,Ltd. Assignor: CHANGZHOU University Contract record no.: X2023980051006 Denomination of invention: A Process Method for Doping Graphene into Polypyrrole Coatings Granted publication date: 20190125 License type: Common License Record date: 20231209 |
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