CN104701034A - Preparation method of light-wave reduced grapheme membrane electrode - Google Patents

Preparation method of light-wave reduced grapheme membrane electrode Download PDF

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Publication number
CN104701034A
CN104701034A CN201510120775.7A CN201510120775A CN104701034A CN 104701034 A CN104701034 A CN 104701034A CN 201510120775 A CN201510120775 A CN 201510120775A CN 104701034 A CN104701034 A CN 104701034A
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China
Prior art keywords
preparation
membrane electrode
light wave
light
graphene oxide
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CN201510120775.7A
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Chinese (zh)
Inventor
杨震宇
胡金火
谢宇
向枫
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Nanchang University
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Nanchang University
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Priority to CN201510120775.7A priority Critical patent/CN104701034A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/26Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • H01M4/1393Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a preparation method of a light-wave reduced grapheme membrane electrode; the preparation method comprises the following steps: weighing graphene oxide and solvent according to a matching ratio, ultrasonically dispersing to form a graphene oxide colloidal solution; spraying a graphene oxide membrane on a current collector by means of a high-pressure electrostatic spraying device; reducing the graphene oxide membrane to a graphene membrane in a light-wave device, thereby obtaining the light-wave reduced grapheme membrane electrode. The advantages are as follows: the light-wave reduced grapheme membrane electrode has good conductivity and three-dimensional structure; the carbon-to-oxygen ratio is 6; any conductive agent and bonding agent are not needed to be added; the improvement of gram volumes of a super-capacitor and a lithium ion battery is facilitated, and good rate capability and cycle performance are not sacrificed.

Description

A kind of preparation method of light wave reduced graphene membrane electrode
Technical field
The present invention relates to electrochemistry new energy field, be specifically related to a kind of preparation method of light wave reduced graphene membrane electrode.
Background technology
Graphene is a kind of new material of the individual layer laminated structure be made up of carbon atom, is a kind ofly to form with sp2 hybridized orbit the flat film that hexangle type is honeycomb lattice by carbon atom.Graphene is thin, the hardest nano material in known world, and conductive coefficient is up to 5300 W/mK, and higher than carbon nano-tube and diamond, under normal temperature, its electron mobility is more than 15000 cm 2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height, and resistivity only about 10 -8Ω m, than copper or silver lower, be the material that world resistivity is minimum.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, and is therefore expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster.
At present, the main production process of Graphene mainly contains tear tape method, slight rubbing manipulation, silicon carbide epitaxial growth, metal surface growth, is oxidized thinning graphite flake method, hydrazine reducing process, cutting carbon nanotubes method etc.Constantly seek simple and effectively prepare Graphene and apply in super capacitor and battery, be the direction of research worker's ongoing effort of electrochemistry new energy field always.
Summary of the invention
The invention provides a kind of graphene film electrode with the reduction of employing light wave, the manufacturing process of this electrode need not add any conductive agent and binding agent, and in lithium ion battery and super capacitor, application has good gram volume, high rate performance and cycle performance.
The technical scheme that the present invention takes is: a kind of preparation method of light wave reduced graphene membrane electrode, is characterized in that preparation method is as follows:
(1) take graphene oxide and solvent by proportioning, ultrasonic disperse makes graphene oxide colloidal solution;
(2) high-voltage electrostatic spray device is utilized to spray graphene oxide on a current collector thin;
(3) in light wave device, graphene film is reduced to; Namely light wave reduced graphene membrane electrode of the present invention is obtained.
Further, making graphene oxide colloidal solution solvent used described in is water or the environmentally friendly solvent such as ethanol or the two mixed solution.
Further, the condition that described high-tension electricity is sprayed into film is: voltage 8-12KV, thermostat temperature 40-60 degree Celsius.
Further, the light wave generating apparatus of described light wave reduced graphene can be light-wave cooker or the halide torch heater of common kitchen tools; Power 300-600W, heating time 3-10 minute.
Further, the collector of described electrode is tinsel or thin slice.
Preferred: graphene oxide concentration 6-10mg/ml, spray voltage 8-10KV, constant temperature 60 degrees Celsius, light-wave cooker power 400W, heating time 6-9 minute.
More preferably: graphene oxide concentration 8 mg/ml, spray voltage 10KV, constant temperature 60 degrees Celsius, light-wave cooker power 400W, 7 minutes heating times.
Good effect of the present invention is as follows: light wave reduced graphene membrane electrode of the present invention has good conductivity and three-dimensional structure, C/O ratio is 6, and any conductive agent and binding agent need not be added, be conducive to the gram volume improving super capacitor and lithium ion battery, and do not sacrifice its good high rate performance and cycle performance.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
Preparation method is specific as follows: first by proportioning take graphene oxide and solvent supersonic dispersion make graphene oxide colloidal solution (aqueous solvent, 6 mg/ml), then high-voltage electrostatic spray device (spray voltage 8KV is utilized, constant temperature 40 degrees Celsius) spraying graphene oxide is thin on a current collector, finally (light-wave cooker in light wave device, power 300W, heats 6 minutes) be reduced to graphene film.Namely light wave reduced graphene membrane electrode of the present invention is obtained.
Embodiment 2
Preparation method is specific as follows: first by proportioning take graphene oxide and solvent supersonic dispersion make graphene oxide colloidal solution (aqueous solvent, 8 mg/ml), then high-voltage electrostatic spray device (spray voltage 10KV is utilized, constant temperature 60 degrees Celsius) spraying graphene oxide is thin on a current collector, finally (light-wave cooker in light wave device, power 600W, heats 4 minutes) be reduced to graphene film.Namely light wave reduced graphene membrane electrode of the present invention is obtained.
Embodiment 3
Preparation method is specific as follows: first by proportioning take graphene oxide and solvent supersonic dispersion make graphene oxide colloidal solution (aqueous solvent, 8 mg/ml), then high-voltage electrostatic spray device (spray voltage 10KV is utilized, constant temperature 60 degrees Celsius) spraying graphene oxide is thin on a current collector, finally (light-wave cooker in light wave device, power 400W, heats 10 minutes) be reduced to graphene film.Namely light wave reduced graphene membrane electrode of the present invention is obtained.
Embodiment 4
Preparation method is specific as follows: first by proportioning take graphene oxide and solvent supersonic dispersion make graphene oxide colloidal solution (ethanol, 6 mg/ml), then high-voltage electrostatic spray device (spray voltage 12KV is utilized, constant temperature 50 degrees Celsius) spraying graphene oxide is thin on a current collector, finally (light-wave cooker in light wave device, power 500W, heats 8 minutes) be reduced to graphene film.Namely light wave reduced graphene membrane electrode of the present invention is obtained.
Embodiment 5
Preparation method is specific as follows: first by proportioning take graphene oxide and solvent supersonic dispersion make graphene oxide colloidal solution (both second alcohol and waters mixed liquor, 8 mg/ml), then high-voltage electrostatic spray device (spray voltage 9KV is utilized, constant temperature 40 degrees Celsius) spraying graphene oxide is thin on a current collector, finally (halide torch heater in light wave device, power 300W, heats 3 minutes) be reduced to graphene film.Namely light wave reduced graphene membrane electrode of the present invention is obtained.
After tested, the light wave reduced graphene membrane electrode prepared by embodiment of the present invention 1-5, the ultracapacitor of development is with current density 0.2A/g discharge and recharge, and material specific capacity can reach 320F/g, and with 1A/g discharge and recharge 10000 times, capacity keeps more than 94%; The lithium ion battery developed with this electrode is with 0.2C discharge and recharge, and material specific capacity can reach 1460mAh/g, and with 1C rate charge-discharge 1000 times, capacity keeps more than 90%.And any conductive agent and adhesive need not be added in the process made, compared with the graphene film electrode reduced with chemical method, there is certain advantage.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.

Claims (10)

1. a preparation method for light wave reduced graphene membrane electrode, the collector of described electrode is tinsel or thin slice, it is characterized in that preparation method is as follows:
(1) take graphene oxide and solvent by proportioning, ultrasonic disperse makes graphene oxide colloidal solution;
(2) high-voltage electrostatic spray device is utilized to spray graphene oxide on a current collector thin;
(3) in light wave device, graphene film is reduced to; Namely obtaining light wave is reduced graphene membrane electrode.
2. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 1, is characterized in that: described in make graphene oxide colloidal solution solvent used be water or ethanol or the two mixed solution.
3. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 1, is characterized in that: the condition that described high-tension electricity is sprayed into film is: spray voltage 8-12KV, thermostat temperature 40-60 degree Celsius.
4. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 1, is characterized in that: the light wave generating apparatus of described light wave reduced graphene is light-wave cooker or the halide torch heater of common kitchen tools; Its power is 300-600W, heating time 3-10 minute.
5. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 1, is characterized in that: described graphene oxide concentration 6-10mg/ml.
6. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 3, is characterized in that: described spray voltage 8-10KV, constant temperature 60 degrees Celsius.
7. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 4, is characterized in that: described light-wave cooker power 400W, heating time 6-9 minute.
8. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 5, is characterized in that: described graphene oxide concentration 8 mg/ml.
9. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 6, is characterized in that: described spray voltage 10KV.
10. the preparation method of a kind of light wave reduced graphene membrane electrode according to claim 7, is characterized in that: 7 minutes described heating times.
CN201510120775.7A 2015-03-19 2015-03-19 Preparation method of light-wave reduced grapheme membrane electrode Pending CN104701034A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106684315A (en) * 2017-01-05 2017-05-17 戴雪青 Preparation method of graphene battery negative electrode
CN108963186A (en) * 2018-04-11 2018-12-07 浙江湖州中科新伏能源科技有限公司 A kind of preparation method of graphene filter membrane and its application in the battery
CN110311110A (en) * 2019-06-30 2019-10-08 东莞理工学院 A kind of flexible lithium ion battery negative electrode material and its test method based on graphene
CN111725477A (en) * 2020-06-16 2020-09-29 深圳市信宇人科技股份有限公司 Preparation method of dry-process electrode material of lithium ion battery

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102881907A (en) * 2012-10-16 2013-01-16 湖南大学 Preparation method of graphene-based electrode material for lithium ion battery
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102881907A (en) * 2012-10-16 2013-01-16 湖南大学 Preparation method of graphene-based electrode material for lithium ion battery

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106684315A (en) * 2017-01-05 2017-05-17 戴雪青 Preparation method of graphene battery negative electrode
CN108963186A (en) * 2018-04-11 2018-12-07 浙江湖州中科新伏能源科技有限公司 A kind of preparation method of graphene filter membrane and its application in the battery
CN110311110A (en) * 2019-06-30 2019-10-08 东莞理工学院 A kind of flexible lithium ion battery negative electrode material and its test method based on graphene
CN111725477A (en) * 2020-06-16 2020-09-29 深圳市信宇人科技股份有限公司 Preparation method of dry-process electrode material of lithium ion battery

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