CN106653389A - Preparation method of graphene and carbon nanotube composite electrode material - Google Patents
Preparation method of graphene and carbon nanotube composite electrode material Download PDFInfo
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- CN106653389A CN106653389A CN201611050210.7A CN201611050210A CN106653389A CN 106653389 A CN106653389 A CN 106653389A CN 201611050210 A CN201611050210 A CN 201611050210A CN 106653389 A CN106653389 A CN 106653389A
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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
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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
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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
- H01G11/84—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
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- 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 preparation method of graphene and carbon nanotube composite electrode material. The preparation method comprises the following steps that S1: single metal is selected as a base which has a stereo sheet structure; and S2: the base of the step S1 is arranged in a plasma vacuum device, firstly the intensity of pressure in the plasma vacuum device is set as 100-300Pa and the temperature is set as 400-600 DEG C, then argon gas is piped into the plasma vacuum device, the mixed liquor of deionized water and an activator is continuously sprayed to the base when the argon gas is piped until the arranging time of the base of the step S1 in the plasma vacuum device is 35-45min, wherein the mixing ratio of the deionized water and the activator is 10:1-20:1, and the base of the step S1 is activated. The crystalline phenomenon between a graphene layer and the base can be avoided so that the quality of the graphene and carbon nanotube composite electrode material is enabled to be high, and the conductivity and the specific surface ratio of the graphene and carbon nanotube composite electrode material are enabled to be high.
Description
Technical field
The present invention relates to the preparation method technical field of electrode material, more particularly to a kind of Graphene and CNT it is compound
Electrode material preparation method.
Background technology
With the popularization and application of global regenerative resource, developing rapidly for ev industry and building for intelligent grid
If energy storage technology becomes the key link that restriction promotes energy development.Current renewable energy technologies mainly have wind energy, the sun
Energy, hydroelectric generation, but as they all have larger unpredictable and dramatic performance, very big is caused to the reliability of electrical network
Impact, therefore not yet applied on a large scale.And the development of energy storage technology can efficiently solve this problem, the essence of energy storage is
Realize the storage to electric energy.
The research to electrochemical energy storage technology is all being strengthened in countries in the world at present.The overall performance of electrochemical energy storing device
Main determining factor is the chemical property of electrode material, thus the research of electrode material that is combined of Graphene and CNT into
For the focus studied in this field, in existing technology, for example, Application No. 201310146410.2（It is a kind of to be based on foam
Preparation method of electrode of super capacitor of nickel and products thereof）A kind of electrode material of middle announcement, is by nickel foam substrate
One layer of graphene oxide of upper deposition, then obtains depositing the nickel foam of Graphene by electrochemical reduction, then in Graphene
Upper water coats one layer of CNT.But for producing the method for graphene oxide mainly by sulphuric acid, nitric acid, potassium permanganate etc.
Strong oxidizer
Graphite powder is aoxidized, so that strutted by oxygen-containing functional group between graphite flake layer that the detached purpose of lamella is reached, most
Graphene is obtained by the method for electronation afterwards, the Graphene obtained using said method, between Graphene and matrix easily
There is crystalline polamer so that the quality of Graphene is substantially reduced, and the carbon being transferred to using water painting method on graphene layer
Nanotube, winds each other and reunites and be extremely serious, greatly reduces its specific surface area and conductivity.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes the compound electrode of a kind of Graphene and CNT
The preparation method of material.
The preparation method of the compound electrode material of a kind of Graphene proposed by the present invention and CNT, including following step
Suddenly：
S1：Choose based on single metal, matrix is lamellar stereochemical structure；
S2：Matrix in S1 is placed in plasma vacuum device, first the pressure in plasma vacuum device is set to
100-300Pa and temperature setting are 400-600 DEG C, are then passed through argon in plasma vacuum device, are being passed through argon
The mixed proportion of the uninterrupted mixed liquor that deionized water and activator are sprayed to matrix, deionized water and activator is 10 simultaneously:
1-20:1, it is 35-45min until standing time of the matrix in S1 in plasma vacuum device, the matrix in S1 is carried out
Activation processing；
S3：Matrix after S2 is activated moves to vacuum drying oven intracavity, and the pressure of vacuum furnace chamber is set to 0-2Pa and temperature setting is
800-1200 DEG C, hybrid protection gas is passed first into, be then passed through after the 10-20min of hybrid protection gas is passed through
Carbon source so that vacuum drying oven intracavity portion occurs carbon source reaction, and the response time of carbon source is 10-20min, after carbon source reaction terminates, very
Matrix in empty furnace chamber naturally cools to room temperature, and the thickness for preparing graphene layer is 5-50nm；
S4：Precipitation transition metal layer is carried out using vacuum depositing process on the graphene layer described in S3；
S5：The matrix for being coated with transition metal layer described in S4 is placed in into vacuum furnace chamber, the pressure of vacuum furnace chamber be set to 0-2Pa with
And temperature setting is 1000-1500 DEG C, passes first into hybrid protection gas, when the internal temperature of vacuum furnace chamber reaches design temperature
When, start to be passed through carbon source, now the velocity ratio of carbon source and hybrid protection gas is 30:80-70:80, vacuum drying oven intracavity portion occurs
Carbon source is reacted, and the response time of carbon source is 30-90min, and after carbon source reaction terminates, the matrix of vacuum drying oven intracavity naturally cools to room
Temperature, the length for preparing CNT are 10-100um；
S6：The matrix for being coated with CNT described in S5 is soaked into 3-6h in deionized water, is then filtered, then in plating
Have on the matrix of CNT and be coated with activator, it is 300-700 to be put into the temperature setting in reacting furnace in 2-5h, and reacting furnace
DEG C, then deionized water carries out washing the matrix for being coated with CNT, Graphene is finally obtained and CNT is compound
Electrode material.
Preferably, in the S1, matrix is nickel, copper or cobalt.
Preferably, in the S4, transition metal layer is nickel, cobalt or ferrum.
Preferably, in the S3 and S5, hybrid protection gas is the mixed gas of argon and helium.
Beneficial effects of the present invention：
1st, activation processing is carried out to matrix by step S2, is easy to graphene layer to be precipitated on matrix, is conducive to Graphene
The growth of layer, and is passed through carbon source to obtain graphene layer in S5, it is to avoid occur crystallization, pole between graphene layer and matrix
The big quality that improve Graphene；
2nd, by the setting of graphene layer and CNT so that the specific surface of the compound electrode material of Graphene and CNT
Product and conductivity are high；
3rd, activation processing is carried out to CNT by S6 so that the activity of CNT is greatly enhanced, greatly enhances stone
The conductivity of the compound electrode material of black alkene and CNT is high；
The present invention can avoid occurring crystalline polamer between graphene layer and matrix so that the compound electricity of Graphene and CNT
The quality of pole material is high, and the conductivity and specific surface rate of the compound electrode material of Graphene and CNT are high.
Specific embodiment
The present invention is further explained with reference to specific embodiment.
Embodiment one
A kind of preparation method of the compound electrode material of Graphene and CNT, including following step are proposed in the present embodiment
Suddenly：
S1：Choose based on single metal, matrix is lamellar stereochemical structure；
S2：Matrix in S1 is placed in plasma vacuum device, first the pressure in plasma vacuum device is set to
100Pa and temperature setting are 400 DEG C, are then passed through argon in plasma vacuum device, while argon is passed through not between
The mixed proportion of the mixed liquor broken to matrix sprinkling deionized water and activator, deionized water and activator is 10:1, until S1
In standing time of the matrix in plasma vacuum device be 35min, activation processing is carried out to the matrix in S1；
S3：Matrix after S2 is activated moves to vacuum drying oven intracavity, and the pressure of vacuum furnace chamber is set to 0Pa and temperature setting is
800 DEG C, hybrid protection gas is passed first into, then carries out being passed through carbon source after the 10min of hybrid protection gas is passed through so that
There is carbon source reaction in vacuum drying oven intracavity portion, the response time of carbon source is 10min, after carbon source reaction terminates, the base of vacuum drying oven intracavity
Body naturally cools to room temperature, and the thickness for preparing graphene layer is 10nm；
S4：Precipitation transition metal layer is carried out using vacuum depositing process on the graphene layer described in S3；
S5：The matrix for being coated with transition metal layer described in S4 is placed in into vacuum furnace chamber, the pressure of vacuum furnace chamber be set to 0Pa and
Temperature setting is 1000 DEG C, passes first into hybrid protection gas, when the internal temperature of vacuum furnace chamber reaches design temperature, is started
Carbon source is passed through, now the velocity ratio of carbon source and hybrid protection gas is 30:80, there is carbon source reaction, carbon source in vacuum drying oven intracavity portion
Response time be 30min, carbon source reaction terminate after, the matrix of vacuum drying oven intracavity naturally cools to room temperature, prepares carbon and receives
The length of mitron is 10um；
S6：The matrix for being coated with CNT described in S5 is soaked into 3h in deionized water, is then filtered, be then coated with
Activator is coated with the matrix of CNT, it is 300 DEG C to be put into the temperature setting in reacting furnace in 2h, and reacting furnace, then is spent
Ionized water carries out washing the matrix for being coated with CNT, and the compound electrode material of Graphene and CNT is finally obtained.
Embodiment two
A kind of preparation method of the compound electrode material of Graphene and CNT, including following step are proposed in the present embodiment
Suddenly：
S1：Choose based on single metal, matrix is lamellar stereochemical structure；
S2：Matrix in S1 is placed in plasma vacuum device, first the pressure in plasma vacuum device is set to
200Pa and temperature setting are 500 DEG C, are then passed through argon in plasma vacuum device, while argon is passed through not between
The mixed proportion of the mixed liquor broken to matrix sprinkling deionized water and activator, deionized water and activator is 15:1, until S1
In standing time of the matrix in plasma vacuum device be 40min, activation processing is carried out to the matrix in S1；
S3：Matrix after S2 is activated moves to vacuum drying oven intracavity, and the pressure of vacuum furnace chamber is set to 1Pa and temperature setting is
1000 DEG C, hybrid protection gas is passed first into, then carry out being passed through carbon source after the 15min of hybrid protection gas is passed through, make
Obtain vacuum drying oven intracavity portion and carbon source reaction occurs, the response time of carbon source is 15min, after carbon source reaction terminates, vacuum drying oven intracavity
Matrix naturally cools to room temperature, and the thickness for preparing graphene layer is 25nm；
S4：Precipitation transition metal layer is carried out using vacuum depositing process on the graphene layer described in S3；
S5：The matrix for being coated with transition metal layer described in S4 is placed in into vacuum furnace chamber, the pressure of vacuum furnace chamber be set to 1Pa and
Temperature setting is 1250 DEG C, passes first into hybrid protection gas, when the internal temperature of vacuum furnace chamber reaches design temperature, is started
Carbon source is passed through, now the velocity ratio of carbon source and hybrid protection gas is 60:80, there is carbon source reaction, carbon source in vacuum drying oven intracavity portion
Response time be 60min, carbon source reaction terminate after, the matrix of vacuum drying oven intracavity naturally cools to room temperature, prepares carbon and receives
The length of mitron is 50um；
S6：The matrix for being coated with CNT described in S5 is soaked into 4h in deionized water, is then filtered, be then coated with
Activator is coated with the matrix of CNT, it is 550 DEG C to be put into the temperature setting in reacting furnace in 4h, and reacting furnace, then is spent
Ionized water carries out washing the matrix for being coated with CNT, and the compound electrode material of Graphene and CNT is finally obtained.
Embodiment three
A kind of preparation method of the compound electrode material of Graphene and CNT, including following step are proposed in the present embodiment
Suddenly：
S1：Choose based on single metal, matrix is lamellar stereochemical structure；
S2：Matrix in S1 is placed in plasma vacuum device, first the pressure in plasma vacuum device is set to
300Pa and temperature setting are 600 DEG C, are then passed through argon in plasma vacuum device, while argon is passed through not between
The mixed proportion of the mixed liquor broken to matrix sprinkling deionized water and activator, deionized water and activator is 20:1, until S1
In standing time of the matrix in plasma vacuum device be 45min, activation processing is carried out to the matrix in S1；
S3：Matrix after S2 is activated moves to vacuum drying oven intracavity, and the pressure of vacuum furnace chamber is set to 2Pa and temperature setting is
1200 DEG C, hybrid protection gas is passed first into, then carry out being passed through carbon source after the 20min of hybrid protection gas is passed through, make
Obtain vacuum drying oven intracavity portion and carbon source reaction occurs, the response time of carbon source is 20min, after carbon source reaction terminates, vacuum drying oven intracavity
Matrix naturally cools to room temperature, and the thickness for preparing graphene layer is 50nm；
S4：Precipitation transition metal layer is carried out using vacuum depositing process on the graphene layer described in S3；
S5：The matrix for being coated with transition metal layer described in S4 is placed in into vacuum furnace chamber, the pressure of vacuum furnace chamber be set to 2Pa and
Temperature setting is 1500 DEG C, passes first into hybrid protection gas, when the internal temperature of vacuum furnace chamber reaches design temperature, is started
Carbon source is passed through, now the velocity ratio of carbon source and hybrid protection gas is 70:80, there is carbon source reaction, carbon source in vacuum drying oven intracavity portion
Response time be 90min, carbon source reaction terminate after, the matrix of vacuum drying oven intracavity naturally cools to room temperature, prepares carbon and receives
The length of mitron is 100um；
S6：The matrix for being coated with CNT described in S5 is soaked into 6h in deionized water, is then filtered, be then coated with
Activator is coated with the matrix of CNT, it is 700 DEG C to be put into the temperature setting in reacting furnace in 5h, and reacting furnace, then is spent
Ionized water carries out washing the matrix for being coated with CNT, and the compound electrode material of Graphene and CNT is finally obtained.
The conventional electrode material of the contrast electrode material compound with the Graphene and CNT of embodiment one to three, implements
Raising percentage ratio such as following table of the compound electrode material of the Graphene and CNT of example one to three than conventional electrode material：
| Embodiment | One | Two | Three |
| Graphene Quality advance percentage ratio | 15% | 30% | 26% |
| Conductivity improves percentage ratio | 20% | 35% | 18% |
| Specific surface area improves percentage ratio | 12% | 25% | 16% |
From the electrode material of above table, the compound electrode material of Graphene proposed by the present invention and CNT and routine
Compare, the performance tool of the compound electrode material of Graphene and CNT is significantly improved.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.
Claims (4)
1. the preparation method of the compound electrode material of a kind of Graphene and CNT, it is characterised in that comprise the following steps：
S1：Choose based on single metal, matrix is lamellar stereochemical structure；S2：Matrix in S1 is placed in plasma vacuum device,
It is 400-600 DEG C that the pressure in plasma vacuum device is set to 100-300Pa and temperature setting first, then to wait from
Argon is passed through in sub- vacuum equipment, the mixing of deionized water and activator is uninterruptedly sprayed while argon is passed through to matrix
The mixed proportion of liquid, deionized water and activator is 10:1-20:1, until the putting in plasma vacuum device of the matrix in S1
The time is put for 35-45min, activation processing is carried out to the matrix in S1；S3：Matrix after S2 is activated moves to vacuum drying oven intracavity,
It is 800-1200 DEG C that the pressure of vacuum furnace chamber is set to 0-2Pa and temperature setting, passes first into hybrid protection gas, Ran Hou
Carry out being passed through carbon source after being passed through the 10-20min of hybrid protection gas so that vacuum drying oven intracavity portion occurs carbon source reaction, carbon source
Response time be 10-20min, carbon source reaction terminate after, the matrix of vacuum drying oven intracavity naturally cools to room temperature, prepares stone
The thickness of black alkene layer is 5-50nm；S4：Precipitation transition metal layer is carried out using vacuum depositing process on the graphene layer described in S3；
S5：The matrix for being coated with transition metal layer described in S4 is placed in into vacuum furnace chamber, the pressure of vacuum furnace chamber be set to 0-2Pa with
And temperature setting is 1000-1500 DEG C, passes first into hybrid protection gas, when the internal temperature of vacuum furnace chamber reaches design temperature
When, start to be passed through carbon source, now the velocity ratio of carbon source and hybrid protection gas is 30:80-70:80, vacuum drying oven intracavity portion occurs
Carbon source is reacted, and the response time of carbon source is 30-90min, and after carbon source reaction terminates, the matrix of vacuum drying oven intracavity naturally cools to room
Temperature, the length for preparing CNT are 10-100um；S6：By the matrix for being coated with CNT described in S5 in deionized water
Middle immersion 3-6h, is then filtered, and is then coated with activator on the matrix for be coated with CNT, is put into 2- in reacting furnace
Temperature setting in 5h, and reacting furnace is 300-700 DEG C, then deionized water carries out washing the matrix for being coated with CNT, most
Graphene and CNT compound electrode material is obtained eventually.
2. the preparation method of the compound electrode material of a kind of Graphene according to claim 1 and CNT, its feature
It is that, in the S1, matrix is nickel, copper or cobalt.
3. the preparation method of the compound electrode material of a kind of Graphene according to claim 1 and CNT, its feature
It is that, in the S4, transition metal layer is nickel, cobalt or ferrum.
4. the preparation method of the compound electrode material of a kind of Graphene according to claim 1 and CNT, its feature
It is that, in the S3 and S5, hybrid protection gas is the mixed gas of argon and helium.
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| CN201611050210.7A CN106653389A (en) | 2016-11-25 | 2016-11-25 | Preparation method of graphene and carbon nanotube composite electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488654A (en) * | 2021-07-27 | 2021-10-08 | 深圳齐锂纳米科技有限公司 | Graphene composite layered conductive agent supported by carbon nano tube |
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| US20150318120A1 (en) * | 2013-01-30 | 2015-11-05 | Empire Technology Development Llc. | Carbon nanotube-graphene composite |
| CN105256312A (en) * | 2015-10-28 | 2016-01-20 | 梧州三和新材料科技有限公司 | Preparing method for graphene and carbon nano tube composite porous electrode material |
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| CN102923686A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Graphene/carbon nanotube composite material preparation method |
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