CN113745012B - Preparation method and application of MXene/rGO@biochar hydrogel composite material - Google Patents
Preparation method and application of MXene/rGO@biochar hydrogel composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000000017 hydrogel Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000002028 Biomass Substances 0.000 claims description 14
- 230000003213 activating effect Effects 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000011363 dried mixture Substances 0.000 claims description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000003990 capacitor Substances 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 244000252132 Pleurotus eryngii Species 0.000 description 3
- 235000001681 Pleurotus eryngii Nutrition 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
- H01G11/84—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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- 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
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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
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- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
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Abstract
Preparation method and application of MXene/rGO@biochar hydrogel composite material, wherein the biochar in the composite material and the MXene/rGO form a three-dimensional porous conductive structure. The invention combines the MXene/rGO hydrogel and the biochar framework, the innovative structure can effectively overcome the defect of self stacking of the MXene, provides an active site of a pseudo capacitor, and effectively increases the specific surface area of the composite material by carbonization and KOH activation for pore forming, and improves the specific capacitance and energy density when the composite material is applied to a supercapacitor.
Description
Technical Field
The invention relates to the technical field of electrochemical energy, in particular to a preparation method and application of an MXene/rGO@biochar hydrogel composite material.
Background
Currently, one of the major trends in the electronics industry is miniature, portable and highly integrated electronic devices. Such electronic devices require the use of miniature power supplies and miniature energy storage devices. Among them, flexible electrochemical capacitors (also called supercapacitors) have great commercial potential due to high power density, rapid charge and discharge and long cycle life. Super-capacitors store electrochemical energy by absorbing ions in an electrolyte through the surface of an electrode material having a high specific surface area, and thus, compared with a general rechargeable battery, can store and transport a large amount of charges in a short time, and the service life is generally millions of cycles. However, one of the major challenges in fabricating supercapacitor electrode plates is increasing the energy density of the overall capacitor.
The biochar is used as an important raw material of the double-layer electrochemical capacitor, is easy to collect, has low cost and no pollution to the environment, but has smaller density due to more pores and larger specific surface area, thereby being unfavorable for being used on various miniature super capacitors.
And MXene is used as a novel two-dimensional material and gradually becomes a novel choice of supercapacitor capacitance material. Compared with other two-dimensional materials, the MXene has oxygen-rich surface groups and has extremely high volume specific capacity, so that the energy density is effectively improved. However, MXene has disadvantages like other two-dimensional nanomaterials, which can lead to stacking and accumulation of MXene nanoplatelets, such that electrochemical performance is not fully utilized. Therefore, a suitable electrode structure is needed to combine biochar and MXene materials to increase the specific surface area and energy density of the electrode sheet.
Disclosure of Invention
The invention aims to provide a preparation method and application of an MXene/rGO@biochar hydrogel composite material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of an MXene/rGO@biochar hydrogel composite material comprises the following steps:
firstly, immersing a freeze-dried biomass material into a mixed dispersion liquid of MXene and GO for full absorption, wherein the mass ratio of the biomass material to the MXene to the GO is 100:1-9:9-1;
then adding ethylenediamine into the mixed dispersion liquid, wherein 150-250 mu L of ethylenediamine is required for each 20-30 mg of GO; then carrying out hydrothermal reaction, heating to 80-130 ℃, and preserving heat for 6-48 hours;
after the hydrothermal reaction, washing the incompletely reacted ethylenediamine by using a mixed solution of deionized water and ethanol, heating to 50-70 ℃ in vacuum after washing, preserving heat until drying, cooling to room temperature, and taking out to obtain a dried mixture;
sintering and carbonizing the dried mixture under the protection of inert gas, cooling to room temperature and taking out; wherein the carbonization requirement is that heating to 600-800 ℃ and preserving heat for 1-2 hours;
grinding the carbonized mixture in a ball mill for 20-30 minutes, adding an activating agent and water after grinding, and uniformly mixing, wherein the mass ratio of the activating agent to the carbonized mixture is 2-4: 1, a step of;
then drying at 40-60 ℃, and sintering and activating under the protection of inert gas after drying, wherein the sintering and activating requirement is that the temperature is 600-800 ℃, and the temperature is kept for 1-2 hours;
and finally, grinding the sintered and activated product to obtain the MXene/rGO@biochar hydrogel composite material.
The relevant content explanation in the technical scheme is as follows:
1. in the above scheme, the biomass material comprises animal or/and plant, and derived material of living body such as microorganism, such as Pleurotus eryngii, folium Nelumbinis, and crab shell.
2. In the scheme, the freeze-drying step is that the frozen product is placed in a freeze dryer for freeze-drying for 24-60 hours after being frozen at the temperature of minus 40 ℃ to minus 60 ℃.
3. In the scheme, the mixed dispersion liquid is formed by ultrasonic mixing of 10mg/mL of MXene dispersion liquid and 2mg/mL of GO dispersion liquid.
4. In the scheme, the ultrasonic frequency of ultrasonic mixing is 35-45 KHz, and the ultrasonic power is 600-800W.
In order to achieve the above purpose, another technical scheme adopted by the invention is as follows:
an electrode sheet for applying an MXene/rgo@biochar hydrogel composite material, comprising:
firstly, uniformly mixing the prepared MXene/rGO@biochar hydrogel composite material, a conductive agent and polyvinylidene fluoride according to a mass ratio of 6-8:2-1:2-1;
then, adding N-methyl pyrrolidone serving as a solvent until the state of the solution is in a critical state between thick and thin, and magnetically stirring for 12-24 hours until the solution is uniformly stirred to obtain MXene/rGO@biochar hydrogel composite material slurry;
and finally, uniformly coating the composite material slurry on the single-side surface of the sheared current collector, and vacuum drying at 50-70 ℃ for 12-24 hours to remove N-methylpyrrolidone, thereby obtaining the composite electrode slice.
The working principle and the advantages of the invention are as follows:
the invention relates to a preparation method of an MXene/rGO@biochar hydrogel composite material, wherein the biochar in the composite material and the MXene/rGO form a three-dimensional porous conductive structure. The invention combines the MXene/rGO hydrogel and the biochar framework, the innovative structure can effectively overcome the defect of self stacking of the MXene, provides an active site of the pseudo capacitor, and effectively increases the specific surface area of the composite material by carbonization and KOH activation for pore forming, and improves the specific capacitance and the energy density of the supercapacitor.
Compared with the prior art, the invention has the following technical effects:
1. the biochar and the MXene/rGO in the composite material form a three-dimensional porous conductive structure, and due to the synergistic effect of the layered structure, the defects of stacking and accumulation of the MXene can be effectively overcome, and the cycling stability of the supercapacitor is greatly improved;
2. in the preparation process of the MXene/rGO hydrogel, a shrinkage effect is generated, so that the hydrogel is attached to the surface of the pleurotus eryngii, the ion transmission of the composite material is not affected by the tight attachment, a new pore size distribution structure is generated, the existence of macropores is reduced, the overall density is increased, and the volume energy density is increased;
3. MXene can provide additional active sites, can promote the pseudo-capacitance characteristic of the electrode surface, and improves the specific capacity of the material;
4. according to the invention, the biomass material is combined with the MXene/rGO hydrogel, the structure of the biochar is filled by the two-dimensional material with higher density, the energy density of the whole device can be obviously improved, and a precondition is created for the biochar to move to a flexible and wearable supercapacitor device.
Drawings
FIG. 1 is a flow chart of a method for preparing an MXene/rGO@biochar hydrogel composite electrode sheet in an embodiment of the invention;
FIG. 2 is an electrochemical test chart-CV chart of an MXene/rGO@biochar hydrogel composite electrode sheet in an embodiment of the invention;
FIG. 3 is an electrochemical test chart-GCD chart of an MXene/rGO@biochar hydrogel composite electrode sheet in an embodiment of the invention;
FIG. 4 is an electrochemical test chart-EIS chart of an MXene/rGO@biochar hydrogel composite electrode sheet in an embodiment of the invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples:
examples: the present invention will be described in detail with reference to the drawings, wherein modifications and variations are possible in light of the teachings of the present invention, without departing from the spirit and scope of the present invention, as will be apparent to those of skill in the art upon understanding the embodiments of the present invention.
As used herein, the terms "comprising," "including," "having," and the like are intended to be open-ended terms, meaning including, but not limited to.
The term (terms) as used herein generally has the ordinary meaning of each term as used in this field, in this disclosure, and in the special context, unless otherwise noted. Certain terms used to describe the present disclosure are discussed below, or elsewhere in this specification, to provide additional guidance to those skilled in the art in connection with the description herein.
The preparation method of the MXene/rGO@biochar hydrogel composite electrode sheet comprises the following steps:
step one, preparation of MXene/rGO@biochar hydrogel composite material
First, the biomass material was lyophilized at-60 ℃ for 48 hours and then removed. The biomass material comprises animal or/and plant, and derived materials of organism such as microorganism, such as Pleurotus eryngii, folium Nelumbinis, and crab shell.
Immersing the freeze-dried biomass material into a mixed dispersion liquid of MXene and GO for full absorption, wherein the mass ratio of the biomass material to the freeze-dried biomass material is 100: 1-9: 9~1. The mixed dispersion liquid is formed by ultrasonic mixing of 10mg/mL of MXene dispersion liquid and 2mg/mL of GO dispersion liquid. The ultrasonic frequency of ultrasonic mixing is 35-45 KHz, and the ultrasonic power is 600-800W.
Then, adding Ethylenediamine (EDA) into the mixed dispersion liquid, wherein 150-250 mu L of ethylenediamine is required for each 20-30 mg of GO; and then carrying out hydrothermal reaction, heating to 80-130 ℃, and preserving heat for 6-48 hours.
After the hydrothermal reaction, washing and drying to obtain a dried mixture; wherein the volume ratio of the cleaning is 9:1, washing off the incompletely reacted ethylenediamine, cleaning, heating to 60 ℃ in vacuum, preserving heat until drying, cooling to room temperature, and taking out.
Sintering and carbonizing the dried mixture under the protection of inert gas (such as nitrogen or argon) and cooling to room temperature, and taking out; wherein the carbonization requirement is heating to 600-800 ℃ and preserving heat for 1-2 hours.
Grinding the carbonized mixture in a ball mill for 20-30 minutes, adding an activating agent and water after grinding, and uniformly mixing, wherein the mass ratio of the activating agent to the carbonized mixture is 2-4: 1, a step of; the added water needs to go over the surface of the mixture and after mixing well the particles in the solution are evenly distributed. The activator can be potassium hydroxide, potassium bicarbonate, etc.
And then continuously drying, and sintering and activating under the protection of inert gas, wherein the sintering and activating requirement is that the sintering and activating is heated to 600-800 ℃, and the sintering and activating is carried out for 1-2 hours.
Finally, grinding the sintered and activated product to obtain the MXene/rGO@biochar hydrogel composite material.
Step two, preparation of composite electrode slice
Firstly, uniformly mixing the prepared MXene/rGO@biochar hydrogel composite material, a conductive agent and polyvinylidene fluoride according to a mass ratio of 6-8:2-1:2-1; the conductive agent can be carbon black.
Then, N-methyl pyrrolidone is taken as a solvent and added until the state of the solution is in a critical state between thick and thin, and the solution is magnetically stirred for 12-24 hours until the solution is uniformly stirred, so as to obtain the MXene/rGO@biochar hydrogel composite material slurry.
And finally, uniformly coating the composite material slurry on the single-side surface of the sheared current collector, and vacuum drying at 50-70 ℃ for 12-24 hours to remove N-methylpyrrolidone, thereby obtaining the composite electrode slice. The current collector can be carbon paper, carbon cloth, foam nickel, foam copper and the like.
The invention also relates to a super capacitor, which comprises the composite material prepared by the preparation method provided by the invention as a working electrode.
The general formula of MXene is Mn+1XnTx or Mn+1Xn, wherein M represents a transition metal, X represents carbon or nitrogen, tx represents a surface functional group comprising-O, -OH and-F, and n is 1, 2 or 3.
The following is a selection of Ti for MXene 3 C 2 T x The specific case is described:
the preparation method of the super capacitor comprises the following steps:
step one, ti 3 C 2 T x The preparation process of the rGO@biochar hydrogel composite material is shown in the figure 1:
the biomass material was lyophilized at-60 ℃ for 48 hours and then removed. Immersing biomass material into Ti 3 C 2 T x And GO mixed dispersion liquid, the mass ratio is 100:9:1, fully absorbing, adding EDA to carry out hydrothermal reaction, heating to 95 ℃, and preserving heat for 12 hours.
After the hydrothermal reaction, the product was washed with a mixed solution of deionized water and alcohol and dried in vacuo at 60 ℃. After cooling to room temperature, sintering and carbonizing the dried mixture under the protection of nitrogen or argon, heating to 600 ℃ and preserving heat for 1 hour, cooling to room temperature, and taking out.
Grinding, mixing with activator, drying, sintering under nitrogen or argon protection, heating to 700 deg.C, maintaining for 1 hr, and grinding to obtain Ti 3 C 2 T x A rGO@biochar hydrogel composite material.
Step two, preparing a composite electrode sheet, wherein the flow is shown in figure 1:
ti is mixed with 3 C 2 T x Uniformly mixing the rGO@biochar hydrogel composite material, carbon black and polyvinylidene fluoride according to the mass ratio of 8:1:1, adding N-methylpyrrolidone as a solvent, and fully and uniformly stirring to obtain Ti 3 C 2 T x rGO@biochar hydrogel composite material slurry;
the Ti is mixed with 3 C 2 T x Uniformly coating the rGO@biochar hydrogel composite material slurry on the surface of sheared carbon paper, and drying in vacuum at 60 ℃ for 12 hours to thoroughly remove N-methylpyrrolidone, thereby obtaining the composite electrode slice.
Step three, assembling a three-electrode system, wherein the flow is shown in fig. 1:
ti for three-electrode test system 3 C 2 T x The rGO@biochar hydrogel composite electrode sheet is used for a working electrode, high-purity graphite is used for a counter electrode, and Ag/AgCl is used for a reference electrode; test system adopts 3M H 2 SO 4 As an electrolyte.
The electrochemical performance of the super capacitor is tested by adopting a current battery testing instrument and method as follows: the specific capacitance was about 238F/g at a sweep rate of 2 mv/s. After the sweeping speed is increased to 50 times (100 mv/s), the specific capacitance is about 234F/g, the electrochemical cycle charge-discharge performance is stable, the internal resistance is smaller, the CV curve is shown in figure 2, the GCD curve is shown in figure 3, and the EIS curve is shown in figure 4.
The invention relates to a preparation method of an MXene/rGO@biochar hydrogel composite electrode slice for a supercapacitor, wherein the biochar in a composite material and the MXene/rGO form a three-dimensional porous conductive structure. The invention combines the MXene/rGO hydrogel and the biochar framework, the innovative structure can effectively overcome the defect of self stacking of the MXene, provides an active site of the pseudo capacitor, and effectively increases the specific surface area of the composite material by carbonization and KOH activation for pore forming, and improves the specific capacitance and the energy density of the supercapacitor.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (6)
1. A preparation method of an MXene/rGO@biochar hydrogel composite material is characterized by comprising the following steps of: comprising the following steps:
firstly, immersing a freeze-dried biomass material into a mixed dispersion liquid of MXene and GO for full absorption, wherein the mass ratio of the biomass material to the MXene to the GO is 100:1-9:9-1;
then adding ethylenediamine into the mixed dispersion liquid, wherein 150-250 mu L of ethylenediamine is required for each 20-30 mg of GO; then carrying out hydrothermal reaction, heating to 80-130 ℃, and preserving heat for 6-48 hours;
after the hydrothermal reaction, washing the incompletely reacted ethylenediamine by using a mixed solution of deionized water and ethanol, heating to 50-70 ℃ in vacuum after washing, preserving heat until drying, cooling to room temperature, and taking out to obtain a dried mixture;
sintering and carbonizing the dried mixture under the protection of inert gas, cooling to room temperature and taking out; wherein the carbonization requirement is that heating to 600-800 ℃ and preserving heat for 1-2 hours;
grinding the carbonized mixture in a ball mill for 20-30 minutes, adding an activating agent and water after grinding, and uniformly mixing, wherein the mass ratio of the activating agent to the carbonized mixture is 2-4: 1, a step of;
then drying at 40-60 ℃, and sintering and activating under the protection of inert gas after drying, wherein the sintering and activating requirement is that the temperature is 600-800 ℃, and the temperature is kept for 1-2 hours;
and finally, grinding the sintered and activated product to obtain the MXene/rGO@biochar hydrogel composite material.
2. The method of manufacturing according to claim 1, characterized in that: the biomass material includes animal or/and plant derived materials.
3. The method of manufacturing according to claim 1, characterized in that: the freeze-drying step is that the frozen product is placed in a freeze dryer for freeze-drying for 24-60 hours after being frozen at the temperature of minus 40 to minus 60 ℃.
4. The method of manufacturing according to claim 1, characterized in that: the mixed dispersion liquid is formed by ultrasonic mixing of 10mg/mL of MXene dispersion liquid and 2mg/mL of GO dispersion liquid.
5. The method of manufacturing according to claim 4, wherein: the ultrasonic frequency of ultrasonic mixing is 35-45 KHz, and the ultrasonic power is 600-800W.
6. An electrode plate applying MXene/rGO@biochar hydrogel composite material is characterized in that: comprising the following steps:
firstly, uniformly mixing the MXene/rGO@biochar hydrogel composite material prepared according to claim 1, a conductive agent and polyvinylidene fluoride according to a mass ratio of 6-8:2-1:2-1;
then, adding N-methyl pyrrolidone serving as a solvent until the state of the solution is in a critical state between thick and thin, and magnetically stirring for 12-24 hours until the solution is uniformly stirred to obtain MXene/rGO@biochar hydrogel composite material slurry;
and finally, uniformly coating the composite material slurry on the single-side surface of the sheared current collector, and vacuum drying at 50-70 ℃ for 12-24 hours to remove N-methylpyrrolidone, thereby obtaining the composite electrode slice.
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| WO2018184235A1 (en) * | 2017-04-08 | 2018-10-11 | 深圳市佩成科技有限责任公司 | Ti3c2tx/graphene oxide/celgard composite separator |
| CN109928713B (en) * | 2019-04-09 | 2021-11-26 | 天津大学 | MXene hydrogel and liquid phase assembly method thereof |
| CN111091976B (en) * | 2019-12-30 | 2022-03-01 | 青岛科技大学 | Biomass/graphene oxide carbon composite material for electrode material and preparation method thereof |
| CN111883314A (en) * | 2020-09-03 | 2020-11-03 | 南京林业大学 | Preparation method of oxidized cellulose-graphene nanoribbon-MXene composite conductive film |
| CN113035578A (en) * | 2021-03-03 | 2021-06-25 | 武汉理工大学 | Graphene/carbon aerogel composite material and preparation method thereof |
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