CN107445151A - Graphene, Graphene electrodes and preparation method thereof - Google Patents
Graphene, Graphene electrodes and preparation method thereof Download PDFInfo
- Publication number
- CN107445151A CN107445151A CN201710799200.1A CN201710799200A CN107445151A CN 107445151 A CN107445151 A CN 107445151A CN 201710799200 A CN201710799200 A CN 201710799200A CN 107445151 A CN107445151 A CN 107445151A
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- graphene
- preparation
- graphite oxide
- substrate
- reducing agent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of graphene, Graphene electrodes, wherein, the preparation method of graphene comprises the following steps：a）Prepare graphite oxide；B) graphite oxide is subjected to pre-reduction treatment；B) graphite oxide after pre-reduction treatment is arranged on substrate；And laser reduction c) is carried out to the substrate for being provided with graphite oxide, to form graphene.
Description
Technical field
The present invention relates to the preparation field of electronic component, more particularly to graphene, Graphene electrodes preparing technical field.
Background technology
Graphene is a kind of carbon molecules arranged by carbon atom and be connected with each other according to hexagon, and its structure is non-
It is often stable.Graphene has the characteristics that high conductivity, high tenacity, high intensity, extra specific surface area, the ratio surface of single-layer graphene
Product can reach 2630 m2/ g, it is highly desirable ultracapacitor energy storage material.Using ultracapacitor made of graphene,
Charging interval only needs 1 millisecond or so.
The traditional preparation methods of graphene have：Mechanical stripping method, chemical reduction method, microwave assisting method, chemical vapor deposition
Method etc..However, these methods all suffer from some such problems in actually producing in enormous quantities：High energy consumption, cost is greatly and not
It is easy to be prepared on a large scale.
The content of the invention
Purport of the present invention provides the preparation method of a kind of graphene and Graphene electrodes.
The present invention needs to propose a kind of graphene and preparation method thereof, and graphene preparation technology is simple and can carry significantly
High efficiency.
In addition, the present invention also needs to propose a kind of Graphene electrodes and preparation method thereof, the Graphene electrodes and its preparation
The technique of method is simple and production efficiency is high.
A kind of preparation method of graphene, comprises the following steps：
a）By graphite oxidation into graphite oxide solution；
B) it is 7-9 the graphite oxide solution that step a is obtained to be adjusted into PH；
C) reducing agent is added in the graphite oxide solution for obtaining step b, obtains the graphene solution of prereduction；
d）It is coated to prereduction graphene that step c is obtained is molten on substrate, laser irradiation is carried out to substrate, obtains graphene.
Wherein, step c）Including：Graphite oxide and Pre-reducing agent are configured to mixed liquor with water, with to the graphite oxide
Carry out pre-reduction treatment.
Wherein, the mass ratio of Pre-reducing agent described in mixed liquor and the graphite oxide is Pre-reducing agent：Graphite oxide=
0.1~0.5。
Wherein, Pre-reducing agent includes any of vitamin C, hydrazine hydrate, sodium borohydride or its combination.
Wherein, step d) includes：By mixed liquor coating over the substrate, the substrate is poly terephthalic acid second two
Appointing in ester, aluminium foil, silicon chip, dimethyl silicone polymer, modified dimethyl polysiloxane, Kynoar or polytetrafluoroethylene (PTFE)
It is a kind of.
Wherein, step d）Including：The substrate for being provided with prereduction graphene solution is pasted and is compacted in light carving CD
Shadow surface on after be put into light irradiation record machine, and be irradiated with the infrared laser of predetermined wavelength.
A kind of graphene is according to graphene made from the above method.
A kind of preparation method of Graphene electrodes, comprises the following steps：The graphene prepared by the above method is processed
Into any of interdigitated, parallel strip, helical form and combinations thereof shape, to obtain the Graphene electrodes.
According to the preparation method of the graphene of above-described embodiment, due to carrying out laser reduction（I.e. height reduces）Advance
A certain degree of prereduction is gone, the graphite oxide after prereduction is more prone to be reduced into graphene by laser reduction.
Graphene reduction effect is substantially better than no pre-reduction treatment after imprinting of graphite oxide film after pre-reduction treatment
The graphene of preparation.Therefore, the present invention can be significantly shorter the time of laser reduction, improve production efficiency.
Meanwhile graphene possesses excellent mechanical property, basic reason is the individual layer of graphene or few Rotating fields, in stone
In black alkene preparation process, graphite oxide easily forms individual layer or few layer result in the solution, well dispersed, still, to aoxidizing stone
After ink is reduced, because the group of graphite oxide molecule interlayer removes, graphene is easy to occur to sink to gather, and loses graphene
Premium properties, therefore, by PH regulations to alkalescence in graphite oxide solution, then carry out reducing agent reduction, can effectively keep
Electrostatic interaction between graphene molecules layer, pre- anti-settling, individual layer or few layer graphene is made.
Brief description of the drawings：Fig. 1 is interdigitated Graphene electrodes.
Embodiment
Embodiment 1
First, 1g graphite and the 25ml concentrated sulfuric acids, 0.5g sodium nitrate are reacted 10 hours, reaction temperature is 4 DEG C, the 4g into reactant
Potassium permanganate, 80 DEG C are reacted 3 hours, add 40ml water, add 5ml hydrogen peroxide, graphite oxide is prepared；
Sodium hydroxide is added into obtained graphite oxide solution, regulation PH is 8, ultrasonic wave 30min, adds reducing agent vitamin
C, vitamin C are 1 with graphite oxide mass ratio：3, prereduction graphene solution is obtained,
Then, prereduction graphene solution is coated in thickness 180um PET film, is spontaneously dried 15 hours at room temperature.
Hereafter, in accordance with the following steps, the Graphene electrodes with interdigitated face shaping are formed by laser reduction.
The 1st, Nero softwares are installed on working machine.
2nd, the face shaping of Nero Cover Designer Software for Design Graphene electrodes is used as interdigitated（Such as Fig. 1 institutes
Show that A1, A2 represent positive and negative Graphene electrodes respectively）, and the radiation parameters such as gray scale, printing contrast are set.
3rd, the substrate for being provided with the graphite oxide by prereduction is pasted on dedicated optical carving CD label face, label surface
It is placed in down with light carving function（lightscribe）CD-ROM drive in, irradiation to be printed.
4th, the pattern of the face shaping of designed Graphene electrodes in above-mentioned 2 is selected, is placed in region to be printed, is started
Laser reduction.
5th, after the completion of irradiating, popping up drive removes light carving disk, takes out the Graphene electrodes obtained through light irradiation.
Thus, Graphene electrodes 1 are obtained.
Comparative example 1
In addition to not carrying out pre-reduction treatment, Graphene electrodes 2 are made in the same way.
It is not molten using the graphite oxide of pre-reduction treatment by more above-mentioned Graphene electrodes 1 and Graphene electrodes 2
Liquid, more difficult light irradiation is poor into complete interdigital or other shapes electrode, light irradiation erosion effect after the drying, it is virtually impossible to tests
Test its performance.
And in contrast, after adding Pre-reducing agent, light carving effect is fine, and irradiation a cycle just complete pattern can occur
（The shape of electrode）, as imprinting number increases, Graphene electrodes electric property is better, shows as the reduction of its resistance.But imprinting
After number is more than 10 times, just do not change significantly.Therefore, the number general control of imprinting is at 1 ~ 6 time.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art is not departing from the principle and objective of the present invention
In the case of above-described embodiment can be changed within the scope of the invention, change, replace and modification.
Claims (8)
1. a kind of preparation method of graphene, it is characterised in that comprise the following steps：
a）By graphite oxidation into graphite oxide solution；
B) it is 7-9 the graphite oxide solution that step a is obtained to be adjusted into PH；
C) reducing agent is added in the graphite oxide solution for obtaining step b, obtains the graphene solution of prereduction；
d）It is coated to prereduction graphene that step c is obtained is molten on substrate, laser irradiation is carried out to substrate, obtains graphene.
2. the preparation method of graphene as claimed in claim 1, it is characterised in that the step c）Including：By the oxidation
Graphite is configured to mixed liquor with Pre-reducing agent with water, to carry out pre-reduction treatment to the graphite oxide.
3. the preparation method of graphene as claimed in claim 2, it is characterised in that the Pre-reducing agent described in the mixed liquor
Mass ratio with the graphite oxide is Pre-reducing agent：Graphite oxide=0.1 ~ 0.5.
4. the preparation method of graphene as claimed in claim 3, it is characterised in that the Pre-reducing agent includes vitamin C, water
Close any of hydrazine, sodium borohydride or its combination.
5. the preparation method of the graphene as any one of claim 2 ~ 4, it is characterised in that the step d) includes：
By mixed liquor coating over the substrate, the substrate is PET, aluminium foil, silicon chip, poly dimethyl
Any of siloxanes, modified dimethyl polysiloxane, Kynoar or polytetrafluoroethylene (PTFE).
6. the preparation method of graphene as claimed in claim 1, it is characterised in that the step d）Including：It will be provided with pre-
The substrate of reduced graphene solution is pasted and is compacted be put into light irradiation record machine after on shadow surface of the light carving with CD, and apparatus
The infrared laser for having predetermined wavelength is irradiated.
7. a kind of graphene, it is characterised in that the preparation method of the graphene according to any one of claim 1 ~ 8 is made.
8. a kind of preparation method of Graphene electrodes, it is characterised in that comprise the following steps：Will be according to claim 1 ~ 6
The obtained graphene of preparation method of graphene be processed into appointing in interdigitated, parallel strip, helical form and combinations thereof shape
One kind, to obtain the Graphene electrodes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710799200.1A CN107445151A (en) | 2017-09-07 | 2017-09-07 | Graphene, Graphene electrodes and preparation method thereof |
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| CN201710799200.1A CN107445151A (en) | 2017-09-07 | 2017-09-07 | Graphene, Graphene electrodes and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807932A (en) * | 2018-06-26 | 2018-11-13 | 山东科思姆特种材料技术开发有限公司 | Cathode material and preparation method thereof for graphene battery |
| CN110074758A (en) * | 2019-04-08 | 2019-08-02 | 清华大学 | Formula is tatooed without underlayer electrode preparation method and device based on multi-layer graphene |
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| CN101844761A (en) * | 2010-05-28 | 2010-09-29 | 上海师范大学 | Method of adopting laser radiation for preparing reduction-oxidation graphene |
| CN103508447A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| 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 |
| CN106800291A (en) * | 2015-11-25 | 2017-06-06 | 衡阳恒荣高纯半导体材料有限公司 | A kind of preparation method of Graphene |
| CN106976871A (en) * | 2017-06-06 | 2017-07-25 | 烟台市烯能新材料股份有限公司 | A kind of method that utilization crystalline flake graphite prepares graphene |
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2017
- 2017-09-07 CN CN201710799200.1A patent/CN107445151A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844761A (en) * | 2010-05-28 | 2010-09-29 | 上海师范大学 | Method of adopting laser radiation for preparing reduction-oxidation graphene |
| CN103508447A (en) * | 2012-06-26 | 2014-01-15 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| 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 |
| CN106800291A (en) * | 2015-11-25 | 2017-06-06 | 衡阳恒荣高纯半导体材料有限公司 | A kind of preparation method of Graphene |
| CN106976871A (en) * | 2017-06-06 | 2017-07-25 | 烟台市烯能新材料股份有限公司 | A kind of method that utilization crystalline flake graphite prepares graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108807932A (en) * | 2018-06-26 | 2018-11-13 | 山东科思姆特种材料技术开发有限公司 | Cathode material and preparation method thereof for graphene battery |
| CN108807932B (en) * | 2018-06-26 | 2021-04-02 | 山东科思姆特种材料技术开发有限公司 | Cathode material for graphene battery and preparation method thereof |
| CN110074758A (en) * | 2019-04-08 | 2019-08-02 | 清华大学 | Formula is tatooed without underlayer electrode preparation method and device based on multi-layer graphene |
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