CN111724999B - Carbon nanotube/activated carbon composite material of core-sheath nano cable structure and preparation method thereof - Google Patents
Carbon nanotube/activated carbon composite material of core-sheath nano cable structure and preparation method thereof Download PDFInfo
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/84—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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a carbon nano tube/activated carbon composite material with a core-sheath nano cable structure and a preparation method thereof, belonging to the technical field of batteries. The preparation method of the carbon nano tube/activated carbon composite material with the core-sheath nano cable structure comprises the following steps: 1) Mixing carbon nano tubes, resorcinol and formaldehyde in water for reaction for 30-80min; 2) Adding oxalic acid into the system after the reaction in the step 1), and reacting for 200-260min; 3) Carrying out solid-liquid separation on the system after the reaction in the step 2), drying, and carrying out heat preservation at 500-600 ℃ for 3.5-4.5h in an inert atmosphere to obtain a carbon nano tube/activated carbon composite material; 4) Mixing the carbon nano tube/activated carbon composite material obtained in the step 3) with potassium hydroxide, and carbonizing at 700-850 ℃ for 2-5 hours to obtain the carbon nano tube/activated carbon composite material. The preparation method of the carbon nano tube/activated carbon composite material with the core-sheath structure has the advantages of environmental friendliness, simple process and the like.
Description
Technical Field
The invention relates to a carbon nano tube/activated carbon composite material with a core-sheath nano cable structure and a preparation method thereof, belonging to the technical field of batteries.
Background
The super capacitor has the advantages of high energy density, high power density, long cycle life, low self-discharge rate and the like, and has wide application prospect. At present, the electrode material of the super capacitor is mainly active carbon with high specific surface. However, activated carbon generally has micropores as the main component, and the pore size distribution is not reasonable and the conductivity is poor, so that the specific capacity of the material is low and the large current rate performance is poor. The preparation process of the high-performance carbon electrode material is developed, the pore size distribution of the high-performance carbon electrode material is optimized, the energy density is improved, the manufacturing cost is reduced, and the preparation process has important significance for developing high-performance super capacitors.
The carbon nano tube has a one-dimensional tubular structure, and the carbon nano tube is mutually wound to form a three-dimensional porous network structure, so that the rapid migration of electrolyte ions and the formation of an electrochemical double layer are facilitated, and the carbon nano tube has the advantage of good rate capability when being used as an electrode material of a super capacitor. However, compared with activated carbon, the specific surface area of carbon nanotubes is not high, which results in low specific capacitance of the material and high preparation cost, limiting practical application thereof.
Therefore, the advantage of high specific surface of the activated carbon is combined with the advantages of three-dimensional porous network structure and high conductivity of the carbon nano tube, the carbon nano tube/activated carbon composite material is developed, the synergistic effect between the two is expected to be exerted, and the carbon electrode material for the super capacitor with lower cost, high specific surface and high performance is prepared.
Disclosure of Invention
The invention provides a preparation method of a carbon nano tube/activated carbon composite material with a core-sheath nano cable structure and the carbon nano tube/activated carbon composite material with the core-sheath nano cable structure prepared by the method. A supercapacitor made from the composite material is also provided.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a carbon nanotube/activated carbon composite material of a core-sheath nano cable structure comprises the following steps:
1) Mixing carbon nano tubes, resorcinol and formaldehyde in water for reaction for 30-80min;
2) Adding oxalic acid into the system after the reaction in the step 1), and reacting for 200-260min;
3) Carrying out solid-liquid separation on the system after the reaction in the step 2), drying, and carrying out heat preservation at 500-600 ℃ for 3.5-4.5h in an inert atmosphere to obtain a carbon nano tube/activated carbon composite material;
4) Mixing the carbon nano tube/activated carbon composite material obtained in the step 3) with potassium hydroxide, and carbonizing at 700-850 ℃ for 2-5h to obtain the carbon nano tube/activated carbon composite material.
The mass ratio of the carbon nano tube to the resorcinol is 0.1-3.37. Preferably, the mass ratio is 0.84-2.5. More preferably, it is 0.1. More preferably, it is 0.1.
The mass ratio of the resorcinol to the formaldehyde is 0.84-3.37. Preferably, the mass ratio is 0.84-2.5. Further preferably, the mass ratio is 0.84-2.16.
The reaction temperature in the step 1) is 55-90 ℃.
In the step 1), the reaction is carried out for 20-50min at 55-65 ℃, and then the reaction is carried out for 10-30min at 80-90 ℃.
The mass ratio of the oxalic acid in the step 2) to the resorcinol in the step 1) is 0.21-0.86:0.84-3.37. Preferably, the mass ratio is 0.21-0.65:0.84-2.5.
And 4), the mass ratio of the carbon nanotube/activated carbon composite material to the potassium hydroxide is 1.
A carbon nano tube/active carbon composite material with a core-sheath nano cable structure prepared by the method.
A super capacitor comprises a positive plate, a negative plate, a diaphragm and electrolyte, wherein the positive plate comprises a positive current collector and a positive material layer coated on the surface of the positive current collector, the positive material layer comprises a positive active substance, a conductive agent and a binder, and the positive active substance is the carbon nano tube/activated carbon composite material with the core-sheath nano cable structure. Further, the negative electrode material layer comprises a negative electrode active material, a conductive agent and a binder, wherein the negative electrode active material is the carbon nano tube/activated carbon composite material with the core-sheath nano cable structure
The invention has the beneficial effects that:
the preparation method of the carbon nano tube/activated carbon composite material with the core-sheath nano cable structure comprises the steps of coating phenolic resin on the surface of a carbon nano tube by adopting an in-situ polymerization method to form the carbon nano tube/phenolic resin composite material with the core-sheath structure, and then carrying out carbonization and activation processes to obtain the carbon nano tube/activated carbon composite material with the core-sheath structure.
The invention relates to a preparation method of a carbon nano tube/activated carbon composite material with a core-sheath structure, which is characterized in that carbon nano tube cores are mutually wound together to form a three-dimensional network-shaped porous structure, and activated carbon is uniformly coated on the side wall of the carbon nano tube to form a nano sheath layer, so that the specific surface of the composite material is favorably improved, the migration distance of ions migrating into micropores to form an electrochemical double layer is favorably shortened, the conductivity of the material is favorably improved, the synergistic effect between the carbon nano tube and the activated carbon is exerted, and the carbon nano tube/activated carbon composite material can be used as a high-performance supercapacitor electrode material.
When the thickness of the porous carbon sheath layer is 30 nm, the highest specific surface area of the material prepared by the preparation method of the carbon nano tube/activated carbon composite material with the core-sheath structure is 2222.1 m 2 (ii)/g as supercapacitor electrode material at 1 Ag -1 The specific capacitance of the organic electrolyte is 121 Fg under the current density -1 And has excellent cycle stability and rate capability.
The preparation method of the carbon nano tube/activated carbon composite material with the core-sheath structure has the advantages of environmental friendliness, simple process and the like, and is easy to realize industrial application.
Drawings
FIG. 1 is a TEM image of a core-sheath carbon nanotube/activated carbon composite prepared in example 3 of the present invention.
Fig. 2 is an SEM image of the core-sheath carbon nanotube/activated carbon composite material prepared in example 3 of the present invention.
Fig. 3 is a low-temperature nitrogen adsorption and desorption curve of the carbon nanotube/activated carbon composite material with the core-sheath structure prepared in examples 1 to 5 of the present invention.
FIG. 4 is a graph showing the capacitance performance of the carbon nanotube/activated carbon composite material having a core-sheath structure prepared in examples 1 to 5 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention easier to understand, the present invention will be described in detail with reference to specific embodiments.
Example 1
The preparation method of the carbon nanotube/activated carbon composite material with the core-sheath structure comprises the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1;
2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then 0.84 g of resorcinol is weighed and added into the dispersion liquid, and ultrasonic wave is carried out to fully dissolve the resorcinol; then, 1.23 g of formaldehyde solution (37%) was weighed into the dispersion and sufficiently dissolved by sonication.
3) Transferring the dispersion prepared in the step 2) into a 250 mL three-neck flask, heating the three-neck flask in a water bath to 60 ℃, carrying out magnetic stirring reaction for 30min, adjusting the temperature to 85 ℃, and carrying out magnetic stirring reaction for 20 min; weighing 0.21 g of oxalic acid, adding into a three-neck flask, and carrying out polymerization reaction for 220 min; after the reaction is finished, vacuum filtration and washing are carried out until the reaction is neutral, and then the reaction product is dried for later use.
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tube furnace and in a nitrogen atmosphere, and naturally cooling to room temperature.
5) And (2) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide according to the mass ratio of 1.
Example 2
The preparation method of the carbon nanotube/activated carbon composite material with the core-sheath structure comprises the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1;
2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then weighing 1.68 g of resorcinol, adding into the dispersion liquid, and carrying out ultrasonic full dissolution; then 2.46 g of formaldehyde solution (37%) was weighed into the dispersion and dissolved thoroughly with ultrasound.
3) Transferring the dispersion prepared in the step 2) into a 500 mL three-neck flask, heating the mixture in a water bath kettle to 60 ℃, carrying out magnetic stirring reaction for 30min, adjusting the temperature to 85 ℃, and carrying out magnetic stirring reaction for 20 min; weighing 0.43 g of oxalic acid, adding into a three-neck flask, and carrying out polymerization reaction for 220 min; after the reaction is finished, vacuum filtration is carried out, and the mixture is washed to be neutral and then dried for standby.
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tube furnace and in a nitrogen atmosphere, and naturally cooling to room temperature.
5) And (2) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide according to the mass ratio of 1.
Example 3
The preparation method of the carbon nanotube/activated carbon composite material with the core-sheath structure comprises the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1;
2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then 2.16 g of resorcinol is weighed and added into the dispersion liquid, and ultrasonic wave is carried out to fully dissolve the resorcinol; then 3.14 g of formaldehyde solution (37%) were weighed into the dispersion and dissolved thoroughly with ultrasound.
3) Transferring the dispersion prepared in the step 2) into a 500 mL three-neck flask, heating the mixture in a water bath to 60 ℃, carrying out magnetic stirring reaction for 30min, adjusting the temperature to 85 ℃, and carrying out magnetic stirring reaction for 20 min; 0.53 g of oxalic acid is weighed and added into a three-neck flask for polymerization reaction for 220 min; after the reaction is finished, vacuum filtration is carried out, and the mixture is washed to be neutral and then dried for standby.
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tube furnace and in a nitrogen atmosphere, and naturally cooling to room temperature.
5) And (2) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide according to the mass ratio of 1.
Example 4
The preparation method of the carbon nanotube/activated carbon composite material with the core-sheath structure comprises the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1;
2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then 2.50 g of resorcinol is weighed and added into the dispersion liquid, and ultrasonic wave is carried out to fully dissolve the resorcinol; then 3.78 g of formaldehyde solution (37%) were weighed into the dispersion and dissolved thoroughly with ultrasound.
3) Transferring the dispersion prepared in the step 2) into a 250 mL three-neck flask, heating the three-neck flask in a water bath to 60 ℃, reacting for 30min by magnetic stirring, adjusting the temperature to 85 ℃, and reacting for 20 min by magnetic stirring; 0.65 g of oxalic acid is weighed and added into a three-neck flask for polymerization reaction for 220 min; after the reaction is finished, vacuum filtration and washing are carried out until the reaction is neutral, and then the reaction product is dried for later use.
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tube furnace and in a nitrogen atmosphere, and naturally cooling to room temperature.
5) And (2) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide according to the mass ratio of 1.
Example 5
The preparation method of the carbon nanotube/activated carbon composite material with the core-sheath structure comprises the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1;
2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then 3.37 g of resorcinol is weighed and added into the dispersion liquid, and ultrasonic wave is carried out to fully dissolve the resorcinol; then 4.9 g of formaldehyde solution (37%) were weighed into the dispersion and dissolved thoroughly with ultrasound.
3) Transferring the dispersion prepared in the step 2) into a 250 mL three-neck flask, heating the three-neck flask in a water bath to 60 ℃, carrying out magnetic stirring reaction for 30min, adjusting the temperature to 85 ℃, and carrying out magnetic stirring reaction for 20 min; weighing 0.86 g of oxalic acid, adding into a three-neck flask, and carrying out polymerization reaction for 220 min; after the reaction is finished, vacuum filtration and washing are carried out until the reaction is neutral, and then the reaction product is dried for later use.
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tube furnace and in a nitrogen atmosphere, and naturally cooling to room temperature.
5) And (3) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide in a mass ratio of 1.
Example 6
The embodiment of this embodiment is the ultracapacitor system's that adopts organic electrolyte embodiment, and the ultracapacitor system of this embodiment is knot formula ultracapacitor system, including positive plate, negative pole piece, diaphragm, electrolyte, and the negative pole piece adopts the copper foil mass flow body, and the positive plate adopts the aluminium foil mass flow body, and positive pole and negative pole all contain the mass flow body and coat the electrode material layer on the mass flow body surface, and the electrode material layer includes active material, binder and binder. The active material is the carbon nanotube/activated carbon composite material with the core-sheath structure prepared in the embodiment 1-5, the binder is PTFE, the conductive agent is acetylene black, and the diaphragm and the electrolyte are the diaphragm and the electrolyte in the prior art.
Test examples
(1) Physical Property test
TEM and SEM tests were performed on the carbon nanotube/activated carbon composite material of the core-sheath nano-cable structure prepared in example 3, and the results are shown in fig. 1 and 2.
As can be seen from fig. 1: the one-dimensional nuclear sheath nano cables are mutually wound together to form a three-dimensional porous shape; meanwhile, the tube diameters of the carbon nanotubes are relatively uniform, which shows that the coating thickness of the porous carbon shell layer is uniform.
As can be seen from fig. 2, the carbon nanotube/activated carbon composite material with the core-sheath nano-cable structure is prepared by the in-situ polymerization method and the subsequent carbonization activation process, wherein the porous carbon sheath layer is uniformly coated on the surface of the sidewall of the carbon nanotube, so that a unique core-sheath nano-cable structure is formed.
Fig. 3 is a low-temperature nitrogen adsorption and desorption isotherm and a pore size distribution curve of the carbon nanotube/activated carbon composite material of the core-sheath nano-cable structure prepared in examples 1 to 5. Wherein the specific surface area of the sample of the embodiment 3 is up to 2222.1 m 2 /g。
The results show that the sample inherits the advantages of the high specific surface of the porous carbon and the appearance of the three-dimensional porous network structure of the carbon nano tube.
(2) Electrochemical testing
Weighing according to the mass ratio of 8The preparation method comprises the following steps of (1) fully grinding and uniformly mixing an active material (a carbon nano tube/active carbon composite material of a core-sheath nano cable structure obtained in embodiment examples 1-5), conductive carbon black (SP) and a binder Polytetrafluoroethylene (PVDF) by using an agate mortar, adding a solvent N-methyl pyrrolidone (NMP) to finally form uniform slurry, coating the obtained slurry on a current collector, coating an aluminum foil on a positive current collector, coating a copper foil on a negative current collector, drying the coated current collector in the air after coating, and drying the current collector in an oven at 120 ℃ for 12 hours; after taking out, the pellets were cut into 14 mm round pieces by a cutter and pressed into tablets under 10 MPa. Finally, the button cell was assembled in a vacuum glove box using 1M tetraethylammonium tetrafluoroborate (Et) 4 NBF 4 /AN)。
The supercapacitors assembled by the carbon nanotube/activated carbon composite material of the core-sheath nano-cable structure in examples 1-5 were subjected to constant current charge and discharge test at a current density of 1A/g, and the test results are shown in fig. 4. Among them, the sample of embodiment 3 has a specific capacitance of up to 121F/g in the organic electrolyte and has excellent cycle stability.
The above description is only one embodiment of the present invention, and not all or only one embodiment, and any equivalent alterations to the technical solutions of the present invention, which are made by those skilled in the art through reading the present specification, are covered by the claims of the present invention.
Claims (1)
1. A super capacitor comprises a positive plate, a negative plate, a diaphragm and electrolyte, wherein the positive plate comprises a positive current collector and a positive material layer coated on the surface of the positive current collector, and the positive material layer comprises a positive active substance, a conductive agent and a binder, and is characterized in that the positive active substance is a carbon nano tube/activated carbon composite material with a core-sheath nano cable structure for the super capacitor, which is prepared by the method comprising the following steps:
1) Adding carbon nanotubes into concentrated nitric acid, wherein the mass ratio of the carbon nanotubes to the concentrated nitric acid is 1; 2) Weighing 0.1 g of activated carbon nano tube, and ultrasonically dispersing in 100 mL of deionized water for 60min; then 2.16 g of resorcinol is weighed and added into the dispersion liquid, and ultrasonic wave is carried out to fully dissolve the resorcinol; then 3.14 g of formaldehyde solution with the mass fraction of 37% is weighed and added into the dispersion liquid, and the mixture is fully dissolved by ultrasonic;
3) Transferring the dispersion prepared in the step 2) into a 500 mL three-neck flask, heating the mixture in a water bath to 60 ℃, carrying out magnetic stirring reaction for 30min, adjusting the temperature to 85 ℃, and carrying out magnetic stirring reaction for 20 min; weighing 0.53 g of oxalic acid, adding into a three-neck flask, and carrying out polymerization reaction for 220 min; after the reaction is finished, performing vacuum filtration, washing to be neutral, and drying for later use;
4) Placing the material obtained in the step 3) in a crucible, preserving the heat for 4 hours at 550 ℃ in a tubular furnace and a nitrogen atmosphere, and naturally cooling to room temperature;
5) And (3) uniformly mixing the carbon nanotube/activated carbon composite material obtained in the step 4) with potassium hydroxide according to the mass ratio of 1.
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