CN107394107A - The preparation method of Graphene electrodes - Google Patents
The preparation method of Graphene electrodes Download PDFInfo
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- CN107394107A CN107394107A CN201610322655.XA CN201610322655A CN107394107A CN 107394107 A CN107394107 A CN 107394107A CN 201610322655 A CN201610322655 A CN 201610322655A CN 107394107 A CN107394107 A CN 107394107A
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- graphene
- graphene electrodes
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- mixed solution
- graphite oxide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 22
- 239000010439 graphite Substances 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 239000012046 mixed solvent Substances 0.000 claims abstract description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 14
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 235000019253 formic acid Nutrition 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000005030 aluminium foil Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 description 15
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- RFXSFVVPCLGHAU-UHFFFAOYSA-N benzene;phenol Chemical compound C1=CC=CC=C1.OC1=CC=CC=C1.OC1=CC=CC=C1 RFXSFVVPCLGHAU-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
Classifications
-
- 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
- H01M4/04—Processes of manufacture in general
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention discloses a kind of preparation method of Graphene electrodes.The preparation method of the graphene comprises the following steps：Formic acid and phenol are well mixed according to 1: 11: 5 ratio, obtain mixed solvent；Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the adding proportion of the graphite oxide and the mixed solvent is 10 15mg/ml；The mixed solution is subjected to the 40min of ultrasonic disperse 30；Mixed solution after will be scattered carries out high-temperature high-voltage reaction, and reaction pressure is 2 4MPa, and reaction temperature is 220 280 DEG C；Washing, drying, obtain graphene；The graphene is processed into Graphene electrodes, colelctor electrode is connected in the Graphene electrodes.The preparation method of Graphene electrodes provided by the invention, the reducing degree of graphite oxide is high, and graphene product quality is good, and the electric conductivity of Graphene electrodes is good.
Description
Technical field
The present invention relates to graphite technology field, and in particular to a kind of preparation method of Graphene electrodes.
Background technology
For graphene as a kind of carbon material of new bi-dimensional cellular shape structure, it has good electric conductivity (7200S/
M), larger theoretical specific surface area (2600m2/ g), the superior performance such as high mechanical stability, therefore cause extensive concern.
Application of the graphene in terms of electrode has been suggested, and it has good electric conductivity.The preparation of Graphene electrodes relies primarily on
In the preparation of grapheme material.
The method for preparing graphene at present mainly has：(1) the graceful Chester university An Deli of micromechanics stripping method, such as Britain
People prepares graphene using adhesive tape method, though this method can obtain the higher few layer graphene of quality, yield is relatively low, process is numerous
It is trivial to limit its use；(2) chemical vapour deposition technique, this method are in the reactor with catalyst substrate, and carbon atom exists
Deposition growing is into graphene on substrate, and this method can produce substantial amounts of graphene, but the growth conditions of graphene it is harsh, into
This is also higher.(3) oxidation-reduction method, this method include two steps：Graphite aoxidizes to form graphite oxide through strong oxidizer, oxidation
Graphite is through chemistry or heat-treats to obtain graphene.Because this method cost is relatively low, simple to operate and be widely used.
Chemical reduction method is considered as the effective ways for largely preparing graphene, and conventional reducing agent has hydrazine hydrate, to benzene
Diphenol etc., but the high toxicity of these reducing agents, have great harm to environment and human body.Therefore new hypotoxicity reduction
Agent gradually attracts attention.However, the reaction condition of prior art makes hypotoxicity reducing agent, graphene can produce in preparation technology
A large amount of to reunite, agglomeration reduces the reducing degree of graphite oxide, influences the product quality of graphene.
Therefore, it is necessary to provide a kind of preparation method of new Graphene electrodes.
The content of the invention
The purpose of the present invention is to overcome above-mentioned technical problem, there is provided a kind of preparation of the good Graphene electrodes of electric conductivity
Method.
In order to solve the above technical problems, the preparation method of Graphene electrodes provided by the invention, comprises the following steps：
S1：Formic acid and phenol are well mixed according to 1: 1-1: 5 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide mixes with described
The adding proportion of solvent is 10-15mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 30-40min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 2-4MPa, reaction temperature 220-
280℃；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into Graphene electrodes, colelctor electrode is connected in the Graphene electrodes.
Preferably, the shape of the Graphene electrodes is in one kind in interdigitated, parallel strip and helical form.
Preferably, the current collection extremely aluminium foil.
Compared with prior art, the preparation method of Graphene electrodes provided by the invention, by selecting rational graphene
Preparation technology, wherein mainly selecting suitable reducing agent and related process parameters, graphite oxide is reduced sufficiently, is not only improved
Its reducing degree, and the product quality of graphene is improved, so as to improving the electric conductivity of Graphene electrodes.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of Graphene electrodes, comprises the following steps：
S1：Formic acid and phenol are well mixed according to 1: 5 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide mixes with described
The adding proportion of solvent is 10mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 30min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 2MPa, and reaction temperature is 220 DEG C,
Reaction time is 24h；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into the Graphene electrodes of interdigitated, colelctor electrode, institute are connected in the Graphene electrodes
State current collection extremely aluminium foil.
Embodiment 2
A kind of preparation method of Graphene electrodes, comprises the following steps：
S1：Formic acid and phenol are well mixed according to 1: 1 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide mixes with described
The adding proportion of solvent is 15mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 40min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 4MPa, and reaction temperature is 260 DEG C,
Reaction time is 15h；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into the Graphene electrodes of parallel strip, colelctor electrode is connected in the Graphene electrodes,
The current collection extremely aluminium foil.
Embodiment 3
A kind of preparation method of Graphene electrodes, comprises the following steps：
S1：Formic acid and phenol are well mixed according to 1: 3 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide mixes with described
The adding proportion of solvent is 12mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 35min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 3MPa, and reaction temperature is 280 DEG C,
Reaction time is 18h；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into spiral helicine Graphene electrodes, colelctor electrode, institute are connected in the Graphene electrodes
State current collection extremely aluminium foil.
Embodiment 4
A kind of preparation method of Graphene electrodes, comprises the following steps：
S1：Formic acid and phenol are well mixed according to 1: 4 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide mixes with described
The adding proportion of solvent is 13mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 40min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 3.5MPa, reaction temperature 240
DEG C, reaction time 20h；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into the Graphene electrodes of parallel strip, colelctor electrode is connected in the Graphene electrodes,
The current collection extremely aluminium foil.
The preparation method of Graphene electrodes provided by the invention, by selecting rational graphene preparation technology, wherein main
Rational reducing agent and related process parameters are selected, is reduced sufficiently graphite oxide, not only increases its reducing degree, and
The product quality of graphene is improved, so as to improve the electric conductivity of Graphene electrodes.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (3)
1. a kind of preparation method of Graphene electrodes, it is characterised in that comprise the following steps：
S1：Formic acid and phenol are well mixed according to 1: 1-1: 5 ratio, obtain mixed solvent；
S2：Graphite oxide is scattered in the in the mixed solvent, obtains mixed solution, the graphite oxide and the mixed solvent
Adding proportion be 10-15mg/ml；
S3：The mixed solution is subjected to ultrasonic disperse 30-40min；
S4：Mixed solution after will be scattered carries out high-temperature high-voltage reaction, reaction pressure 2-4MPa, reaction temperature 220-280
℃；
S5：Washing, drying, obtain graphene；
S6：The graphene is processed into Graphene electrodes, colelctor electrode is connected in the Graphene electrodes.
2. the preparation method of Graphene electrodes according to claim 1, it is characterised in that the shape of the Graphene electrodes
In one kind in interdigitated, parallel strip and helical form.
3. the preparation method of Graphene electrodes according to claim 1, it is characterised in that the current collection extremely aluminium foil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610322655.XA CN107394107A (en) | 2016-05-17 | 2016-05-17 | The preparation method of Graphene electrodes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610322655.XA CN107394107A (en) | 2016-05-17 | 2016-05-17 | The preparation method of Graphene electrodes |
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| Publication Number | Publication Date |
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| CN107394107A true CN107394107A (en) | 2017-11-24 |
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| CN201610322655.XA Pending CN107394107A (en) | 2016-05-17 | 2016-05-17 | The preparation method of Graphene electrodes |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101864098A (en) * | 2010-06-03 | 2010-10-20 | 四川大学 | Preparation method of polymer/graphene composite material through in situ reduction |
| US20110165321A1 (en) * | 2010-01-07 | 2011-07-07 | Aruna Zhamu | Continuous process for producing spacer-modified nano Graphene electrodes for supercapacitors |
| CN102530927A (en) * | 2010-12-24 | 2012-07-04 | 中国科学院兰州化学物理研究所 | Graphene preparation method |
| CN104211047A (en) * | 2013-05-30 | 2014-12-17 | 纳米新能源（唐山）有限责任公司 | Graphene, graphene electrode, graphene supercapacitor and preparation method thereof |
-
2016
- 2016-05-17 CN CN201610322655.XA patent/CN107394107A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110165321A1 (en) * | 2010-01-07 | 2011-07-07 | Aruna Zhamu | Continuous process for producing spacer-modified nano Graphene electrodes for supercapacitors |
| CN101864098A (en) * | 2010-06-03 | 2010-10-20 | 四川大学 | Preparation method of polymer/graphene composite material through in situ reduction |
| CN102530927A (en) * | 2010-12-24 | 2012-07-04 | 中国科学院兰州化学物理研究所 | Graphene preparation method |
| CN104211047A (en) * | 2013-05-30 | 2014-12-17 | 纳米新能源（唐山）有限责任公司 | Graphene, graphene electrode, graphene supercapacitor and preparation method thereof |
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Application publication date: 20171124 |
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