CN109473293B - Preparation method of carbon material for super capacitor - Google Patents
Preparation method of carbon material for super capacitor Download PDFInfo
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- CN109473293B CN109473293B CN201810919175.0A CN201810919175A CN109473293B CN 109473293 B CN109473293 B CN 109473293B CN 201810919175 A CN201810919175 A CN 201810919175A CN 109473293 B CN109473293 B CN 109473293B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 34
- 239000003575 carbonaceous material Substances 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000005011 phenolic resin Substances 0.000 claims abstract description 40
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000006260 foam Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000007833 carbon precursor Substances 0.000 claims abstract description 4
- 238000005087 graphitization Methods 0.000 claims abstract 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 19
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 6
- 239000006230 acetylene black Substances 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011149 active material Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 8
- 238000013508 migration Methods 0.000 abstract 2
- 230000005012 migration Effects 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 229930006000 Sucrose Natural products 0.000 description 5
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 5
- 239000005720 sucrose Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention adopts phenolic resin as a main body, synthesizes phenolic resin carbon precursor by a hydrothermal method, assembles the super capacitor by using nickel foam as a narrow body, and tests the charging and discharging time of the capacitor under the constant current condition. The phenolic resin carbon base has higher graphitization degree and can provide a quick channel for electron migration, thereby having higher conductivity; and the structure is complex, the mechanical strength is good, the electron migration in the super capacitor can be improved, and a large number of micropores and mesopores are used for electron storage. The method is simple to operate and is used for improving the capacity, safety and other properties of the carbon-based super capacitor.
Description
Technical Field
The invention belongs to the technical field of green energy storage, and particularly relates to a preparation method of a carbon material for a super capacitor.
Background
At present, the shortage of energy is becoming an increasingly prominent problem with the development of mankind. Clean energy such as wind energy, solar energy, water energy and the like is generally converted into chemical energy for storage due to the intermittent energy production characteristic, but the chemical energy also has various problems such as (i) safety problem, (ii) long-term energy loss and (iii) inability of rapid charge and discharge. Compared with a chemical battery, the super capacitor has high power density and good cycle stability, and is excellent in charge and discharge performance under a large multiplying power, so that the super capacitor is hopefully substituted for the chemical battery to become a novel energy storage device. At present, the carbon material is the most applied electrode material in commercial supercapacitors, and has high conductivity, acid and alkali corrosion resistance and abundant and various structures.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon material for a super capacitor, the super capacitor prepared by the method can effectively solve the capacity problem of the capacitor, can effectively improve the capacity of the carbon-based super capacitor, and has wide application prospect in the field of energy storage.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for producing a carbon material usable for a supercapacitor, the method comprising:
synthesizing a phenolic resin carbon precursor by a hydrothermal method, and then graphitizing at high temperature; and preparing the super capacitor by using the foamed nickel as a carrier.
In the technical scheme, a series of novel carbon-based capacitor materials are prepared by a hydrothermal method, and porous carbon materials with different carbon sources, different shapes and structures and different pore size distributions are obtained through experimental design. The morphology and the structure of the carbon-based material are researched by adopting a scanning electron microscope and X-ray diffraction, and the influence of different factors on the performance of the carbon-based material supercapacitor is researched by adopting a cyclic voltammetry method and a charge-discharge test. The phenolic resin carbon source is simple in synthesis method and excellent in performance, and is an ideal material for manufacturing the super capacitor.
The invention adopts a hydrothermal method to synthesize graphitized phenolic resin carbon and prepare a super capacitor. The prepared super capacitor has the following advantages: 1. the preparation material is carbon, the price is low, and large-scale industrial production can be realized; 2. the capacitor has excellent performance:its capacitance exceeds 100F g-1. Can work in the range of-40 to +50 ℃; 3. the capacitor has long storage life: the storage life of the battery is more than 10 years under the normal temperature condition, and the annual capacity is reduced by about 1%; 4. the capacitor is safe and reliable: the capacitor has no gas precipitation in the storage and discharge processes, and the safety is good; can meet the requirements of various applications.
Preferably, the preparation method comprises the following steps:
(1) weighing hydroquinone, formaldehyde and nickel nitrate hexahydrate, stirring and dissolving in water for 10 minutes, transferring to a polytetrafluoroethylene reaction kettle, reacting in a vacuum drying oven at 160 ℃ for 12 hours, and taking out after cooling to room temperature to obtain a phenolic resin precursor;
(2) carbonizing the obtained phenolic resin precursor in a tubular furnace under the argon atmosphere at the heating rate of 5 ℃/min, preserving the heat for 1-4 hours at the temperature of 600-800 ℃, taking out the phenolic resin precursor after cooling to the room temperature, washing nickel by using a hydrochloric acid solution, and then centrifugally washing for three times to obtain graphitized phenolic resin carbon;
(3) preparing slurry according to the proportion of graphitized phenolic resin carbon, acetylene black and PVDF (80: 10); cutting the foamed nickel, weighing the cut foamed nickel to obtain the mass, and uniformly coating the slurry stirred for 12 hours on the foamed nickel; putting the mixture into a 60 ℃ oven and taking the mixture out for 12 hours;
(4) constant current charge and discharge tests are carried out on the foamed nickel coated with the active material at a current of 1mA to obtain a charge and discharge curve of voltage changing along with time, and CV tests are carried out at a scanning rate of 2mVs-1 to obtain a curve of current changing along with voltage.
Preferably, the temperature for the incubation in step (3) is 800 ℃.
Preferably, in the step (1), 1-8% of hydroquinone, 0.5-5% of formaldehyde, 5-28% of nickel nitrate hexahydrate and the balance of water are calculated according to mass percentage.
Preferably, the size of the nickel foam in step (3) is 10 x 10 cm.
The invention has the beneficial effects that:
1. the graphitized phenolic resin carbon prepared by a hydrothermal method is a cheap one of carbon-based supercapacitors, and can be popularized and applied in a large scale;
2. the capacitor has excellent performance and the capacitance of the capacitor exceeds 100F g-1. Can work in the range of-40 to +50 ℃;
3. the capacitor has long storage life: the storage life of the battery is more than 10 years under the normal temperature condition, and the annual capacity is reduced by about 1%;
4. the capacitor is safe and reliable: the capacitor has no gas precipitation in the storage and discharge processes, and the safety is good; can meet the requirements of various applications.
Drawings
FIG. 1 is a SEM image of phenolic carbon of the present invention.
FIG. 2 is a carbon infrared spectrum of phenolic resin at different carbonization temperatures according to the present invention.
FIG. 3 is an XRD pattern of the phenolic resin of the present invention after nickel catalyzed 800 ℃ carbonization.
FIG. 4 is a charge-discharge diagram of a supercapacitor made of phenolic carbon in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example 1: taking graphitized phenolic resin carbon as an example:
the embodiment of the invention provides a preparation method of a material for a super capacitor, which comprises the following steps:
(1) preparation of graphitized phenolic resin carbon: weighing 1% of hydroquinone, 5% of formaldehyde and 28% of nickel nitrate hexahydrate according to the mass percentage, stirring and dissolving the hydroquinone, the formaldehyde and the nickel nitrate hexahydrate in water for 10 minutes, transferring the mixture into a polytetrafluoroethylene reaction kettle, reacting the mixture in a vacuum drying oven at 160 ℃ for 12 hours, and taking out the mixture after cooling to room temperature. Carbonizing the obtained phenolic resin precursor in a tube furnace under the argon atmosphere, wherein the heating rate is 5 ℃ for min-1And keeping the temperature at 800 ℃ for 1 hour, taking out after cooling to room temperature, washing nickel by using a hydrochloric acid solution, and then centrifugally washing for three times to obtain the graphitized phenolic resin carbon, wherein the synthesized phenolic resin carbon is a ribbon network as shown in a Scanning Electron Microscope (SEM) diagram of figure 1.
(2) The slurry was prepared according to the ratio of phenolic resin carbon to acetylene black to PVDF 80: 10. 10 x 10cm of nickel foam was cut and weighed, and the slurry stirred for 12 hours was uniformly coated on the nickel foam. After being put into an oven at 60 ℃ and taken out for 12 hours, the carbonized phenolic resin carbon at different temperatures and different times is synthesized as shown in figure 2 and figure 3, and the graphitizing degree of the synthesized phenolic resin carbon is the highest at 800 ℃ for 2 hours.
(3) And (3) testing the battery performance: constant current charge and discharge test was performed on the nickel foam coated with the active material at a current of 1mA to obtain a charge and discharge curve of voltage with time, see FIG. 4, at 2mV s-1The CV test was performed to obtain a current versus voltage curve.
Example 2: graphitized sucrose carbon synthesis example
The embodiment of the invention provides a preparation method of a negative electrode material for a lithium ion battery, which comprises the following steps:
(1) preparation of graphitized sucrose carbon: weighing 1-8% of sucrose and 5-28% of nickel nitrate hexahydrate by mass percent, stirring and dissolving in water for 10 minutes, transferring the mixture into a polytetrafluoroethylene reaction kettle, reacting in a vacuum drying oven at 160 ℃ for 12 hours, and taking out after cooling to room temperature. Carbonizing the obtained sucrose carbon precursor in a tube furnace under argon atmosphere at a heating rate of 5 ℃ for min-1And keeping the temperature at 800 ℃ for 1-4 hours at 600-.
(2) The slurry is prepared according to the mixture ratio of sucrose carbon, acetylene black and PVDF which is 80: 10. 10 x 10cm of nickel foam was cut and weighed, and the slurry stirred for 12 hours was uniformly coated on the nickel foam. Putting the mixture into an oven at 60 ℃ and taking the mixture out for 12 hours.
(3) And (3) testing the battery performance: constant current charge and discharge test is carried out on the foamed nickel coated with the active substance at the current of 1mA to obtain a charge and discharge curve of which the voltage changes along with the time and the voltage changes at 2mV s-1The CV test was performed to obtain a current versus voltage curve.
The difference between the first embodiment and the second embodiment is that: the graphitized carbon material is successfully prepared, has good mechanical property and ionic conductivity, and can be applied to a super capacitor. The graphitized carbon material synthesized by different carbon sources is assembled into the super capacitor for constant current charge and discharge test, and the result shows that the capacity of the super capacitor prepared by the phenolic resin carbon source is higher.
Example 3: taking graphitized phenolic resin carbon as an example:
the embodiment of the invention provides a preparation method of a material for a super capacitor, which comprises the following steps:
(1) preparation of graphitized phenolic resin carbon: weighing 8% of hydroquinone, 0.5% of formaldehyde and 5% of nickel nitrate hexahydrate by mass percent, stirring and dissolving in water for 10 minutes, transferring the mixture into a polytetrafluoroethylene reaction kettle, reacting in a vacuum drying box at 160 ℃ for 12 hours, and taking out after cooling to room temperature. Carbonizing the obtained phenolic resin precursor in a tube furnace under the argon atmosphere, wherein the heating rate is 5 ℃ for min-1And keeping the temperature at 600 ℃ for 4 hours, taking out after cooling to room temperature, washing out nickel by using a hydrochloric acid solution, and then centrifugally washing for three times to obtain the graphitized phenolic resin carbon.
(2) The slurry was prepared according to the ratio of phenolic resin carbon to acetylene black to PVDF 80: 10. 10 x 10cm of nickel foam was cut and weighed, and the slurry stirred for 12 hours was uniformly coated on the nickel foam. Putting the mixture into an oven at 60 ℃ and taking the mixture out for 12 hours.
(3) And (3) testing the battery performance: and (3) carrying out constant current charge and discharge test on the foamed nickel coated with the active substance at a current of 1mA to obtain a charge and discharge curve of which the voltage changes along with time.
Example 4: taking graphitized phenolic resin carbon as an example:
the embodiment of the invention provides a preparation method of a material for a super capacitor, which comprises the following steps:
(1) preparation of graphitized phenolic resin carbon: weighing 5% of hydroquinone, 3% of formaldehyde and 15% of nickel nitrate hexahydrate according to the mass percentage, stirring and dissolving the hydroquinone, the formaldehyde and the nickel nitrate hexahydrate in water for 10 minutes, transferring the mixture into a polytetrafluoroethylene reaction kettle, reacting the mixture in a vacuum drying oven at 160 ℃ for 12 hours, and taking the mixture out after cooling to room temperature. Carbonizing the obtained phenolic resin precursor in a tube furnace under the argon atmosphere, wherein the heating rate is 5 ℃ for min-1To 750 ℃ CKeeping the temperature for 2 hours, taking out after cooling to room temperature, washing nickel by using a hydrochloric acid solution, and then centrifugally washing for three times to obtain the graphitized phenolic resin carbon.
(2) The slurry was prepared according to the ratio of phenolic resin carbon to acetylene black to PVDF 80: 10. 10 x 10cm of nickel foam was cut and weighed, and the slurry stirred for 12 hours was uniformly coated on the nickel foam. Putting the mixture into an oven at 60 ℃ and taking the mixture out for 12 hours.
(3) And (3) testing the battery performance: and (3) carrying out constant current charge and discharge test on the foamed nickel coated with the active substance at a current of 1mA to obtain a charge and discharge curve of which the voltage changes along with time.
Claims (4)
1. A method for producing a carbon material usable for a supercapacitor, the method comprising:
synthesizing a phenolic resin carbon precursor by a hydrothermal method, and then graphitizing at high temperature; preparing a super capacitor by using foamed nickel as a carrier; wherein:
the raw materials for synthesizing the phenolic resin precursor by a hydrothermal method are as follows: 1-8% of hydroquinone, 0.5-5% of formaldehyde, 5-28% of nickel nitrate hexahydrate and the balance of water by mass percentage;
the high-temperature graphitization temperature is 600-800 ℃, and the time is 1-4 hours.
2. The method for preparing a carbon material for a supercapacitor according to claim 1, comprising the steps of:
(1) weighing hydroquinone, formaldehyde and nickel nitrate hexahydrate, stirring and dissolving in water for 10 minutes, transferring to a polytetrafluoroethylene reaction kettle, reacting in a vacuum drying oven at 160 ℃ for 12 hours, and taking out after cooling to room temperature to obtain a phenolic resin precursor;
(2) carbonizing the obtained phenolic resin precursor in a tubular furnace under the argon atmosphere at the heating rate of 5 ℃/min, preserving the heat for 1-4 hours at the temperature of 600-800 ℃, taking out the phenolic resin precursor after cooling to the room temperature, washing nickel by using a hydrochloric acid solution, and then centrifugally washing for three times to obtain graphitized phenolic resin carbon;
(3) according to the graphitized phenolic resin carbon: acetylene black: PVDF 80: 10: 10, preparing slurry; cutting the foamed nickel, weighing the cut foamed nickel to obtain the mass, and uniformly coating the slurry stirred for 12 hours on the foamed nickel; putting the mixture into a 60 ℃ oven and taking the mixture out for 12 hours;
(4) constant current charge and discharge tests are carried out on the foamed nickel coated with the active material at a current of 1mA to obtain a charge and discharge curve of voltage changing along with time, and CV tests are carried out at a scanning rate of 2mVs-1 to obtain a curve of current changing along with voltage.
3. The method for preparing a carbon material for a supercapacitor according to claim 2, wherein the temperature for the holding in the step (2) is 800 ℃.
4. The method for preparing a carbon material for a supercapacitor according to claim 2, wherein the size of the nickel foam in the step (3) is 10 x 10 cm.
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| US9911545B2 (en) * | 2015-01-30 | 2018-03-06 | Corning Incorporated | Phenolic resin sourced carbon anode in a lithium ion capacitor |
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