CN117550600A - Porous biomass carbon electrode material, preparation method of electrode slice of porous biomass carbon electrode material and electrode slice - Google Patents
Porous biomass carbon electrode material, preparation method of electrode slice of porous biomass carbon electrode material and electrode slice Download PDFInfo
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000007772 electrode material Substances 0.000 title claims abstract description 62
- 239000002028 Biomass Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000003763 carbonization Methods 0.000 claims abstract description 32
- 244000280244 Luffa acutangula Species 0.000 claims description 24
- 235000009814 Luffa aegyptiaca Nutrition 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000006230 acetylene black Substances 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000013543 active substance Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 2
- 238000001994 activation Methods 0.000 abstract description 10
- 230000004913 activation Effects 0.000 abstract description 6
- 230000002745 absorbent Effects 0.000 abstract description 4
- 239000002250 absorbent Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 28
- 238000010438 heat treatment Methods 0.000 description 23
- 238000004458 analytical method Methods 0.000 description 20
- 229910052760 oxygen Inorganic materials 0.000 description 19
- 125000004429 atom Chemical group 0.000 description 12
- 230000006399 behavior Effects 0.000 description 12
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 10
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000001237 Raman spectrum Methods 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 125000004122 cyclic group Chemical group 0.000 description 7
- 230000007547 defect Effects 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 230000001788 irregular Effects 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 125000004430 oxygen atom Chemical group O* 0.000 description 6
- 125000002837 carbocyclic group Chemical group 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 235000003956 Luffa Nutrition 0.000 description 2
- 241000219138 Luffa Species 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000002238 attenuated effect Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000010219 correlation analysis Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000219104 Cucurbitaceae Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application belongs to the technical field of battery electrode design, and in particular relates to a porous biomass carbon electrode material, a preparation method of an electrode plate of the porous biomass carbon electrode material and the electrode plate, wherein KOH is used as a microwave absorbent and a pore-forming agent of the porous biomass carbon electrode material, and the porous biomass carbon electrode material is prepared through microwave carbonization, so that extra pretreatment and activation steps are not needed, carbonization and activation processes are integrated in one step, simplicity, rapidness and energy conservation are realized, the structure of the prepared porous biomass carbon electrode material mainly comprises micropores and macropores and mesopores, the specific surface area is high, and the porous biomass carbon electrode material has high specific capacity, high multiplying power performance and good cycle stability.
Description
Technical Field
The application belongs to the technical field of battery electrode design, and particularly relates to a porous biomass carbon electrode material, a preparation method of an electrode slice of the porous biomass carbon electrode material and the electrode slice.
Background
Clean and renewable energy sources such as solar energy, wind energy, water energy and tidal energy are environment-friendly, but have the problems of intermittence and instability, and in order to replace fossil fuels with serious environmental pollution, the energy storage device is required to be popularized and applied on a large scale.
The super capacitor and the battery pack thereof are novel energy storage devices, have the advantages of high power density, good cycle performance, low cost and the like, and can well meet the requirements of clean and renewable energy source application on the energy storage devices.
The super capacitor and the battery electrode material thereof are mainly made of carbon materials, and natural renewable biomass is mostly selected for preparation in consideration of cost and reproducibility. The loofah sponge is a vascular bundle of dried mature fruits of the loofah belonging to the cucurbitaceae family, has a three-dimensional space reticular structure, and mainly comprises cellulose, hemicellulose and lignin, wherein the cellulose content is generally above 60%, and is an ideal raw material for preparing the porous biomass carbon electrode material.
At present, the porous biomass carbon electrode material prepared by using the luffa needs to be pretreated and activated, the process is complicated, the energy consumption is high, the time consumption is long, the specific surface area of the obtained porous biomass carbon electrode material is small, and the specific surface area is only 868.02 m 2 The specific capacity per gram is only small, the current density per gram is only 201F per gram at 0.5A per gram, and the rate capability and the cycle stability are poor.
The present application has been made in view of the existence of the above-mentioned technical drawbacks.
Disclosure of Invention
The purpose of the application is to provide a porous biomass carbon electrode material, a preparation method of an electrode slice thereof and an electrode slice, so as to overcome or alleviate at least one technical defect existing in the prior art.
The technical scheme of the application is as follows:
in one aspect, a method for preparing a porous biomass carbon electrode material is provided, comprising:
s1, cutting the loofah sponge into small blocks, performing ultrasonic treatment by using deionized water and absolute ethyl alcohol for 20-40 min, and drying at 60-90 ℃;
s2, soaking the loofah sponge in KOH solution with the concentration of 1.0-5.0 mol/L for 1-3 h;
s3, taking out the loofah sponge, and drying at 60-90 ℃;
s4, placing the loofah sponge into a quartz tube of a microwave tube type furnace, performing microwave carbonization in a nitrogen atmosphere, wherein the flow rate of the nitrogen is 100-300 mL/min, the microwave power is 800-1200W, the microwave carbonization temperature is 500-800 ℃, and the heat preservation time is 4-8 min;
s5, taking out the loofah sponge, grinding the loofah sponge into powder, washing the powder with an HCl solution with the concentration of 1-3 mol/L, washing the powder to be neutral with deionized water, and drying the powder at the temperature of 60-90 ℃ to obtain the porous biomass carbon electrode material.
According to at least one embodiment of the present application, in the preparation method of the porous biomass carbon electrode material described above, in S1, the ultrasonic treatment time is 30min;
the drying temperature was 80 ℃.
According to at least one embodiment of the present application, in the preparation method of the porous biomass carbon electrode material, in S2, the concentration of KOH solution is 4.0 mol/L;
the soaking time is 2 hours.
According to at least one embodiment of the present application, in the preparation method of the porous biomass carbon electrode material, in S3, the drying temperature is 80 ℃.
According to at least one embodiment of the present application, in the preparation method of the porous biomass carbon electrode material, in S4, the flow rate of nitrogen is 200 mL/min, the microwave power is 1000W, the microwave carbonization temperature is 600 ℃, and the heat preservation time is 5 min.
According to at least one embodiment of the present application, in the preparation method of the porous biomass carbon electrode material, in S5, the concentration of HCl solution is 2.0 mol/L, and the number of times of washing with HCl solution is 3 times;
the drying temperature was 80 ℃.
In another aspect, a method for preparing an electrode sheet is provided, including:
preparing a porous biomass carbon electrode material based on any one of the preparation methods of the porous biomass carbon electrode material;
dispersing porous biomass carbon electrode material, acetylene black and polytetrafluoroethylene in absolute ethyl alcohol to prepare slurry;
and coating the slurry on a current collector, drying, tabletting by a tablet press, and preparing the electrode slice.
According to at least one embodiment of the present application, in the preparation method of the electrode sheet, the mass ratio of the porous biomass carbon electrode material, the acetylene black and the polytetrafluoroethylene dispersed in the absolute ethyl alcohol is 8:1:1;
when the porous biomass carbon electrode material, the acetylene black and the polytetrafluoroethylene are dispersed into the absolute ethyl alcohol, magnetic stirring or ultrasonic dispersion is used, wherein when the magnetic stirring is used, the stirring speed is 200-400 r/min; when ultrasonic dispersion is used, the ultrasonic power is 400-600W.
According to at least one embodiment of the present application, in the above method for manufacturing an electrode sheet, the current collector is nickel foam, and the loading amount of the active material thereon is 2 to 4 mg;
the tabletting pressure is 8-12 MPa.
In a further aspect, an electrode sheet is provided, and the electrode sheet is prepared by any one of the preparation methods of the electrode sheet.
The application has at least the following beneficial technical effects:
the preparation method of the porous biomass carbon electrode material uses KOH as a microwave absorbent and a pore-forming agent thereof, and the porous biomass carbon electrode material is prepared through microwave carbonization without additional pretreatment and activation steps, integrates carbonization and activation processes in one step, is simple, quick and energy-saving, and has a structure with micropores as a main component and macropores and mesopores, and has high specific surface area, high specific capacity, high multiplying power performance and good cycle stability.
Drawings
FIG. 1 is a graph of temperature versus time during microwave carbonization for LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5 provided in the examples of the present application.
FIG. 2 is an X-ray diffraction pattern XRD of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 3 is a Raman spectrum of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 4 is a schematic view of X-ray photoelectron spectroscopy XPS of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 5 is an SEM image of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 6 is a TEM image of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 7 is an N2 adsorption-desorption isotherm plot of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 8 is a schematic diagram of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 9 is a DFT pore size distribution plot of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided by the examples of the present application.
FIG. 10 is a schematic diagram of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 11 is a comparison of cyclic voltammetric CV curves for LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 provided in the examples of the present application.
FIG. 12 is a graph showing the comparison of the constant current charge and discharge GCD curves of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5 and LSPB-K-C-4 provided in the examples of the present application.
Fig. 13 is a schematic diagram of a method for preparing a porous biomass carbon electrode material according to an embodiment of the present application.
For the purpose of better illustrating the present embodiments, certain elements of the drawings may be omitted, enlarged or reduced and do not represent the actual product dimensions, and furthermore, the drawings are for illustrative purposes only and are not to be construed as limiting the present patent.
Detailed Description
In order to make the technical solution of the present application and the advantages thereof more apparent, the technical solution of the present application will be more fully described in detail below with reference to the accompanying drawings, it being understood that the specific embodiments described herein are only some of the embodiments of the present application, which are for explanation of the present application, not for limitation of the present application. It should be noted that, for convenience of description, only a portion related to the present application is shown in the drawings, and other related portions may refer to a general design.
Furthermore, unless defined otherwise, technical or scientific terms used in the description of this application should be given the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs. The words used in the description of the present application to indicate directions are merely used to indicate relative directions or positional relationships, and when the absolute position of the object to be described is changed, the relative positional relationship may be changed accordingly. As used in this description, the word "comprising" or "comprises" does not exclude the presence of other elements or components than those listed after the word.
The present application is described in further detail below with reference to fig. 1-13.
In one aspect, a method for preparing a porous biomass carbon electrode material is provided, as shown in fig. 13.
S1, cutting the loofah sponge into small blocks with the size of about 1 multiplied by 2 multiplied by 1 cm, weighing about 5.0 g, carrying out ultrasonic treatment by using deionized water and absolute ethyl alcohol for 20-40 min, preferably 30min, and drying at 60-90 ℃, preferably 80 ℃ to avoid overlong drying time and damage to the loofah sponge.
S2, soaking the loofah dried in the step S1 in KOH solution with the concentration of 1.0-5.0 mol/L for 1-3 h, and preferably for 2 hours.
S3, taking out the loofah soaked in the KOH solution in the S2, and drying at 60-90 ℃, preferably 80 ℃, so as to avoid overlong drying time and damage to the loofah.
S4, placing the loofah sponge dried in the S3 into a quartz tube of a microwave tube type furnace, performing microwave carbonization in a nitrogen atmosphere, wherein the nitrogen flow rate is 100-300 mL/min, preferably 200-mL/min, the microwave power is 800-1200W, preferably 1000W, the microwave carbonization temperature is 500-800 ℃, preferably 600 ℃, the heat preservation time is 4-8 min, preferably 5min, the heating rate is about 100-400 ℃ min < -1 >, and the total carbonization time is 6-12 min.
S5, taking out the product obtained by the loofah sponge after the microwave carbonization in S4, grinding the product into powder, washing the powder with an HCl solution with the concentration of 1-3 mol/L for 3 times to remove KOH, wherein the concentration of the HCl solution is preferably 2.0 mol/L, washing the powder with deionized water to be neutral, and drying the powder at 60-90 ℃, preferably 80 ℃, thereby obtaining the porous biomass carbon electrode material from the loofah sponge.
In five more specific examples, the concentration of KOH solution used in S2 was designed to be 1.0 mol/L, 2.0 mol/L, 3.0 mol/L, 4.0 mol/L, 5.0 mol/L, respectively, and the porous biomass carbon electrode materials obtained were LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, respectively, using the preferred design parameters.
In a specific comparative example, the concentration of KOH solution used in S2 was designed to be 4.0 mol/L, and in S4, the dried retinervus luffae fructus was placed in a quartz tube of a conventional tube furnace, high-temperature carbonization was performed in a nitrogen atmosphere, the nitrogen flow rate was 200 mL/min, the heating rate was 5 ℃/min, the holding temperature was 600 ℃, the holding time was 120 min, and the porous biomass carbon electrode material was obtained as LSPB-K-C-4 by adopting the preferred design parameters.
In LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5 and LSPB-K-C-4, the content of C, O, N elements obtained by X-ray photoelectron spectroscopy is shown in the following table:
specific surface area, pore volume, average pore size of LSPB-K-1, LSPB-K-2, LSPB-K-3, LSPB-K-4, LSPB-K-5, LSPB-K-C-4 are shown in the following table:
as shown in figure 1, the temperature-time curve of LSPB-K-1 in the microwave carbonization process can rapidly enter a heating stage after microwave heating is started, the temperature can be raised from the room temperature of 26 ℃ to the preset temperature of 600 ℃ in 5.25 min, the heating rate is about 109 ℃/min, the heat preservation stage is immediately entered and lasts for 5min, the temperature in the heat preservation stage is maintained at 572-607 ℃, and the total carbonization time is 10.25 min. The X-ray diffraction characterization of LSPB-K-1 was performed as shown in FIG. 2, wherein there were two broad diffraction bands at 21℃and 43℃corresponding to the 002, 101 crystal planes, respectively, of the carbon material, the broad diffraction bands indicating that LSPB-K-1 had an amorphous structure. The Raman spectrum of LSPB-K-1 is shown in FIG. 3, where at 1340 and 1580 cm -1 The scattering peaks at which the ratio IG/ID of the intensities of the G-band and D-band is 1.19 correspond to the D-band induced by defects and disordered structures present in the material and the G-band induced by the stretching motion of all sp2 atom pairs in the carbocyclic or long chain, respectively. The X-ray photoelectron spectrum of LSPB-K-1, as shown in FIG. 4, wherein the characteristic peaks at binding energies 283.4 and 532.3 eV correspond to the binding energies of C1 s and O1 s electrons, respectively, indicates the presence of C and O elements in LSPB-K-1, and further analysis shows that the percentage of C, O and N atoms is 85.75%, 13.39% and 0.85%, respectively, and no distinct characteristic peak of N1 s atoms can be observed in the X-ray photoelectron spectrum due to the low N content. As shown in the SEM image of LSPB-K-1, as shown in FIG. 5, it can be seen that LSPB-K-1 has a porous structure and that 200 to 800 macropores of nm are present. As shown in FIG. 6, a large number of TEM images of LSPB-K-1 were observed below 2 nmIs a micro-pore of (a). As shown in FIG. 7, the N2 adsorption-desorption isotherm of LSPB-K-1 is shown as I type, indicating that LSPB-K-1 is a porous structure mainly comprising micropores, and the specific surface area is 688.22 m 2 And/g. The pore size distribution of LSPB-K-1, as shown in FIG. 8, from which it was seen that the LSPB-K-1 had 3 peaks at 0.50, 0.80 and 1.19. 1.19 nm, indicating that the micropores were predominantly of these 3 sizes and that the total pore volume was 0.30 cm 3 Per g, the volumes of micropores, mesopores and macropores are 0.23, 0.02 and 0.05. 0.05 cm, respectively 3 The volume ratio of the micropores reaches 76.7 percent, and the average pore diameter is about 1.73 and nm. At a scan rate of 20 mV/s, the cyclic voltammetric CV curve of LSPB-K-1 is shown in FIG. 9, from which it can be seen that the CV curve of LSPB-K-1 presents an irregular rectangle, indicating that the capacitive behavior of LSPB-K-1 has some pseudocapacitive component, mainly due to its higher oxygen content. When the current density is 2A/g, as shown in FIG. 10, the GCD curve of LSPB-K-1 is basically symmetrical in shape, but has a certain degree of bending, which indicates that the charging and discharging behaviors have higher coulomb efficiency, but has a certain pseudocapacitance component, and is consistent with the analysis result of CV curve, and the specific capacity of LSPB-K-1 at the current density is about 146F/g can be calculated from the discharging time. As shown in FIG. 11, the specific capacity of LSPB-K-1 was 165F/g when the current density was 0.5A/g, 99F/g when the current density was increased to 20A/g, and 67.81% when the specific capacity was maintained, and the rate performance was excellent. As shown in FIG. 12, the cycle stability curve of LSPB-K-1 shows that the specific capacity of LSPB-K-1 hardly decays after 10000 charge and discharge cycles at a current density of 5A/g, and the LSPB-K-1 has good cycle stability.
As shown in FIG. 1, the temperature-time curve of LSPB-K-2 is shown, after microwave heating is started, the temperature is quickly increased to 600 ℃ from 25 ℃ to the preset temperature within 4.5 min, the temperature increasing rate is about 128 ℃/min, the temperature increasing rate is higher than LSPB-K-1, the analysis is that KOH can play a role of a microwave absorbent in the microwave carbonization process, the more the KOH amount adsorbed by the loofah sponge is, the higher the temperature increasing rate is, after the temperature increasing stage is finished,then the process enters a heat preservation stage and lasts for 5min, the temperature in the heat preservation stage is maintained between 578 and 604 ℃, and the total carbonization time is 9.5 min. The X-ray diffraction spectrum characterization of LSPB-K-2 was performed as shown in FIG. 2, wherein there were two broad diffraction bands at 21℃and 43℃corresponding to the 002, 101 crystal planes, respectively, of the carbon material, the broad diffraction bands indicating that LSPB-K-2 had an amorphous structure. The Raman spectrum of LSPB-K-2 is shown in FIG. 3, where at 1340 and 1580 cm -1 The scattering peaks at which the ratio IG/ID of the intensities of the G-band and D-band is 1.10 correspond to the D-band induced by defects and disordered structures present in the material and the G-band induced by the stretching motion of all sp2 atom pairs in the carbocyclic or long chain, respectively. The X-ray photoelectron spectrum of LSPB-K-2 is shown in FIG. 4, wherein characteristic peaks at binding energies 283.4 and 532.3 eV correspond to the binding energies of C1 s and O1 s electrons, respectively, indicating the presence of C and O elements in LSPB-K-2, and further analysis shows that C, O and N atoms account for 88.96%, 9.94% and 1.10% respectively, and no distinct characteristic peak of N1 s atoms can be observed in the X-ray photoelectron spectrum due to the low N content. As shown in the SEM image of LSPB-K-2, as shown in FIG. 5, it can be seen that LSPB-K-2 has a porous structure and the presence of macropores ranging from 200 to 600 nm can be observed. As shown in FIG. 6, a TEM image of the electrode material of LSPB-K-2 shows that a large number of micropores of 2 nm or less can be observed. As shown in FIG. 7, the N2 adsorption-desorption isotherm of LSPB-K-2 is shown as I type, which shows that the LSPB-K-2 is a porous structure mainly comprising micropores, and the specific surface area is 868.88 m 2 And/g, which is higher than LSPB-K-1, because KOH can play a role of a pore-forming agent in the microwave carbonization process, and the larger the KOH amount adsorbed by the loofah sponge is, the larger the specific surface area and the pore volume of the obtained material are. As shown in FIG. 8, the pore size distribution of LSPB-K-2 shows that LSPB-K-2 has 3 peaks at 0.50, 0.80 and 1.29. 1.29 nm, indicating that the micropores predominate in these 3 sizes and the total pore volume is 0.39 cm 3 Per g, the volumes of micropores, mesopores and macropores are 0.28, 0.03 and 0.08, cm, respectively 3 The volume ratio of the micropores reaches 71.8%, and the average pore diameter is about 1.81 and nm. At a tracing rate of 20 mV/s, the cyclic voltammetric CV curve of LSPB-K-2 is shown in FIG. 9, from which C of LSPB-K-2 can be seenThe V curve presents an irregular rectangle, which shows that the capacitance behavior of LSPB-K-2 has a certain pseudocapacitance component, which is mainly caused by the higher oxygen content of the LSPB-K-2, and the area enclosed by the CV curve is larger than LSPB-K-1, which shows that the specific capacity of the LSPB-K-2 is higher than LSPB-K-1. When the current density is 2A/g, as shown in fig. 10, the constant-current charge-discharge GCD curve of LSPB-K-2 shows that the shape of the GCD curve of LSPB-K-2 is basically symmetrical, but has a certain degree of bending, which shows that the charge-discharge behavior of the GCD curve has higher coulomb efficiency, but has a certain pseudocapacitance component, which is matched with the analysis result of a CV curve, the specific capacity of LSPB-K-2 at the current density is about 190F/g, the specific capacity is higher than that of LSPB-K-1, and the analysis result of the CV curve is matched. As shown in FIG. 11, the specific capacity of LSPB-K-2 was 205F/g when the current density was 0.5A/g, 143F/g when the current density was increased to 20A/g, 69.76% and the rate retention was slightly better than that of LSPB-K-1. As shown in FIG. 12, the LSPB-K-2 had a cycle stability curve, and it was found that the specific capacity of LSPB-K-2 was hardly attenuated after 10000 charge/discharge cycles at a current density of 5A/g, and had good cycle stability.
The temperature-time curve of LSPB-K-3 is shown in figure 1, microwave heating is started, then the microwave heating is quickly started to enter a heating stage, the temperature is raised from the room temperature 27 ℃ to the preset temperature 600 ℃ at the heating rate of about 164 ℃/min, the heating rate is higher than that of LSPB-K-1 and LSPB-K-2, the specific reasons refer to the related analysis in LSPB-K-2, the heating stage is ended, the microwave heating is immediately started to enter a heat preservation stage and is continued for 5min, the temperature in the heat preservation stage is maintained at 586-612 ℃, and the total carbonization time is 8.5 min. The X-ray diffraction spectrum characterization of LSPB-K-3 was performed as shown in FIG. 2, wherein there were two broad diffraction bands at 21℃and 43℃corresponding to the 002, 101 crystal planes of the carbon material, respectively, the broad diffraction bands indicating that the resulting LSPB-K-3 had an amorphous structure. The Raman spectrum of LSPB-K-3 is shown in FIG. 3, where at 1340 and 1580 cm -1 Scattering peaks at which correspond to D-band induced by defects and disordered structures present in the material and G-band induced by stretching motion of all sp2 atom pairs in a carbocyclic or long chain, respectively, the intensities of which G-band and D-bandThe ratio IG/ID was 1.08. The X-ray photoelectron spectrum of LSPB-K-3, as shown in FIG. 4, wherein the characteristic peaks at binding energies 283.4 and 532.3 eV correspond to the binding energies of C1 s and O1 s electrons, respectively, indicates the presence of C and O elements in LSPB-K-3, and further analysis shows that the percentages of C, O and N atoms are 88.87%, 9.92% and 1.21%, respectively, and that no distinct characteristic peak of N1 s atoms can be observed in the X-ray photoelectron spectrum due to the low N content. As shown in the SEM image of LSPB-K-3, as shown in FIG. 5, it can be seen that LSPB-K-3 has a porous structure and the presence of macropores ranging from 200 to 1000 nm can be observed. As shown in FIG. 6, a TEM image of LSPB-K-3 shows that a large number of micropores of 2 nm or less can be observed. The N2 adsorption-desorption isotherm of LSPB-K-3, as shown in FIG. 7, from which the N2 adsorption-desorption isotherm of LSPB-K-3 is known to be type I, shows that it is a microporous-based porous structure with a specific surface area of 1035.03 m2/g, which is higher than that of LSPB-K-1 and LSPB-K-2, for specific reasons, reference is made to the correlation analysis in LSPB-K-2. As shown in FIG. 8, the pore size distribution of LSPB-K-3 shows that LSPB-K-3 has 3 peaks at 0.50, 0.80 and 1.21 and nm, indicating that the micropores predominate in these 3 sizes and the total pore volume is 0.46 and 0.46 cm 3 Per g, the volumes of micropores, mesopores and macropores are 0.33, 0.03 and 0.10. 0.10 cm, respectively 3 The volume ratio of micropores per gram reaches 71.7%, and the average pore diameter is about 1.76 and nm. At a scan rate of 20 mV/s, the cyclic voltammetric CV curve of LSPB-K-3, as shown in FIG. 9, can be seen from which the CV curve of LSPB-K-3 presents an irregular rectangle, indicating that the capacitive behavior of LSPB-K-3 has a pseudocapacitive component that is primarily due to its higher oxygen content, and the area enclosed by its CV curve is greater than LSPB-K-1 and LSPB-K-2, indicating that its specific capacity is higher than LSPB-K-1 and LSPB-K-2. When the current density is 2A/g, as shown in fig. 10, the constant-current charge-discharge GCD curve of LSPB-K-3 shows that the shape of the GCD curve of LSPB-K-3 is basically symmetrical, but has a certain degree of bending, which shows that the charge-discharge behavior of the GCD curve has higher coulomb efficiency, but has a certain pseudocapacitance component, which is matched with the analysis result of a CV curve, the specific capacity of LSPB-K-3 at the current density is about 232F/g, the specific capacity is higher than that of LSPB-K-1 and LSPB-K-2, and the analysis result of the CV curve is matched. L (L)As shown in FIG. 11, the specific capacity of SPB-K-3 was 252F/g at a current density of 0.5A/g, and 184F/g at a current density of 20A/g, the specific capacity retention rate was 73.02%, and the rate performance was slightly better than those of LSPB-K-1 and LSPB-K-2. As shown in FIG. 12, the LSPB-K-3 had a cycle stability curve, and it was found that the specific capacity of LSPB-K-3 was hardly attenuated after 10000 charge/discharge cycles at a current density of 5A/g, and had good cycle stability.
The temperature-time curve of LSPB-K-4 is shown in figure 1, microwave heating is started, then the microwave heating is quickly started to enter a heating stage, the temperature is raised from the room temperature of 26 ℃ to the preset temperature of 600 ℃ for 2.5 min, the heating rate is about 230 ℃ min-1, the heating rate is higher than that of LSPB-K-1, LSPB-K-2 and LSPB-3, the specific reasons refer to related analysis in LSPB-K-2, the microwave heating stage is started immediately after the heating stage is ended, the microwave heating stage lasts for 5min, the temperature in the heating stage is kept between 581 and 622 ℃, and the total carbonization time is 7.5 min. X-ray diffraction spectrum characterization is carried out on LSPB-K-4, as shown in FIG. 2, two wider diffraction bands are arranged at 21 degrees and 43 degrees, and the wider diffraction bands respectively correspond to 002 crystal faces and 101 crystal faces of the carbon material, so that the LSPB-K-4 has an amorphous structure. The Raman spectrum of LSPB-K-4 is shown in FIG. 3, where at 1340 and 1580 cm -1 The scattering peaks at which correspond to D-band induced by defects and disordered structures present in the material and G-band induced by stretching motion of all sp2 atom pairs in the carbocycle or long chain, respectively, the ratio IG/ID of the intensities of G-band and D-band being 1.05. The X-ray photoelectron spectrum of LSPB-K-4 is shown in FIG. 4, wherein characteristic peaks at binding energies 283.4 and 532.3 eV correspond to the binding energies of C1 s and O1 s electrons, respectively, indicating the presence of C and O elements in LSPB-K-4, and further analysis shows that the percentages of C, O and N atoms are 90.27%, 8.80% and 0.93%, respectively, and no distinct characteristic peak of N1 s atoms can be observed in the X-ray photoelectron spectrum due to the low N content. As shown in the SEM image of LSPB-K-4, as shown in FIG. 5, it can be seen that LSPB-K-4 has a porous structure and the presence of macropores ranging from 200 to 1000 nm can be observed. As shown in FIG. 6, a TEM image of LSPB-K-4 shows that a large number of micropores of 2 nm or less can be observed. N2 adsorption-desorption isotherms of LSPB-K-4 as shown in FIG. 7From the above, it was found that the N2 adsorption-desorption isotherm of LSPB-K-4 was of type I, indicating that it was a microporous-based porous structure with a specific surface area of 1207.26m 2 And/g, above LSPB-K-1, LSPB-K-2 and LSPB-3, for specific reasons with reference to the correlation analysis in LSPB-K-2. As shown in FIG. 8, the pore size distribution of LSPB-K-4 shows that there are 4 peaks at 0.46, 0.68, 0.82 and 1.22 nm for LSPB-K-4, indicating that the micropores predominate in these 4 sizes and that the total pore volume is 0.55 cm 3 Per g, the volumes of micropores, mesopores and macropores are 0.40, 0.04 and 0.11. 0.11 cm, respectively 3 The volume ratio of the micropores reaches 72.7 percent, and the average pore diameter is about 1.80 and nm. At a scan rate of 20 mV/s, the cyclic voltammetric CV curve for LSPB-K-4 is shown in FIG. 9, from which it can be seen that the CV curve for LSPB-K-4 presents an irregular rectangle, indicating that there is some pseudocapacitive component of the capacitive behavior of LSPB-K-4, which is mainly caused by its higher oxygen content, and that the area enclosed by its CV curves is greater than LSPB-K-1, LSPB-K-2 and LSPB-K-3, indicating that its specific capacity is higher than LSPB-K-1, LSPB-K-2 and LSPB-K-3. The constant current charge-discharge GCD curve of LSPB-K-4 with current density of 2A/g is shown in figure 10, the GCD curve of LSPB-K-4 is basically symmetrical in shape, but has a certain degree of bending, which shows that the charge-discharge behavior of the GCD curve has higher coulomb efficiency, but has a certain pseudocapacitance component, is matched with the analysis result of a CV curve, the specific capacity of LSPB-K-4 at the current density is about 274F/g, the specific capacity is higher than LSPB-K-1, LSPB-K-2 and LSPB-K-3 according to the analysis result of the CV curve can be calculated by the discharge time. As shown in FIG. 11, the specific capacity of LSPB-K-4 was 294F/g at a current density of 0.5A/g, 220F/g at an increase of 20A/g, 74.83% at a specific capacity retention, and slightly better rate properties than LSPB-K-1, LSPB-K-2, and LSPB-K-3. As shown in FIG. 12, the cycle stability curve of LSPB-K-4 shows that the specific capacity of LSPB-K-4 has almost no attenuation after 10000 charge and discharge cycles at a current density of 5A/g, and has good cycle stability.
The temperature-time curve of LSPB-K-5 is shown in figure 1, and the temperature is rapidly raised after microwave heating is started for 1.5 minThe temperature is raised from the room temperature of 24 ℃ to the preset temperature of 600 ℃, the temperature raising rate is about 384 ℃/min, the temperature raising rate is higher than LSPB-K-1, LSPB-K-2, LSPB-3 and LSPB-4, specific reasons refer to related analysis in LSPB-K-2, the temperature raising stage is ended, the temperature is immediately kept for 5min, the temperature is kept at 577-666 ℃ in the temperature keeping stage, and the total carbonization time is 6.5 min. The X-ray diffraction spectrum characterization of LSPB-K-4 was performed as shown in FIG. 2, wherein there were two broad diffraction bands at 21℃and 43℃corresponding to the 002, 101 crystal planes, respectively, of the carbon material, the broad diffraction bands indicating that LSPB-K-5 had an amorphous structure. LSPB-K-5 Raman spectrum, as shown in FIG. 3, wherein the scattering peaks at 1340 and 1580 cm-1 correspond to the D-band induced by defects and disordered structures present in the material and the G-band induced by the stretching motion of all sp2 atom pairs in the carbocyclic or long chain, respectively, with a G-band to D-band intensity ratio IG/ID of 1.09. The ray photoelectron spectra of LSPB-K-5, as shown in FIG. 4, wherein the characteristic peaks at binding energies 283.4 and 532.3 eV correspond to the binding energies of C1 s and O1 s electrons, respectively, indicate the presence of C and O elements for LSPB-K-5, and further analysis shows that the percentages of C, O and N atoms are 88.28%, 11.08% and 0.64%, respectively, and that no distinct characteristic peak of N1 s atoms is observed in the X-ray photoelectron spectra due to the low N content. As shown in the SEM image of LSPB-K-5, as shown in FIG. 5, LSPB-K-5 is porous, and the presence of macropores of 200 to 600 nm can be observed. As shown in FIG. 6, a TEM image of LSPB-K-5 shows that a large number of micropores of 2 nm or less can be observed. As shown in FIG. 7, the N2 adsorption-desorption isotherm of LSPB-K-5 is shown as I type, which shows that the LSPB-K-5 is a porous structure mainly comprising micropores, the specific surface area is 894.89 m & g & lt-1 & gt, and the specific surface area is lower than LSPB-K-1, LSPB-K-2, LSPB-K-3 and LSPB-K-4, and the reason is probably due to the fact that the excessive KOH amount of the component adsorbed by the luffa reacts with KOH. As shown in FIG. 8, the pore size distribution of LSPB-K-5 shows that the pore size of LSPB-K-5 has 3 peaks at 0.49, 0.80 and 1.18 nm, indicating that the micropores predominate in these 3 sizes and the total pore volume is 0.40 cm 3 The volumes of the micropores, the mesopores and the macropores are respectively 0.29, 0.03 and 0.08 cm < 3 >. G < -1 >, and the volume ratio of the micropores reaches 72.5%The average pore size was about 1.78 and nm. At a scan rate of 20 mV/s, the cyclic voltammetric CV curve of LSPB-K-5, as shown in FIG. 9, can be seen from which the CV curve of LSPB-K-5 presents an irregular rectangle, indicating that there is some pseudocapacitive component of the capacitive behavior of LSPB-K-5, which is mainly caused by its higher oxygen content, and the area enclosed by its CV curve is greater than LSPB-K-1 and LSPB-K-2, but less than LSPB-K-3 and LSPB-K-4, indicating that its specific capacity is greater than LSPB-K-1 and LSPB-K-2, but less than LSPB-K-3 and LSPB-K-4. When the current density is 2A/g, the GCD curve of LSPB-K-5 is basically symmetrical in shape, but has a certain degree of bending, which shows that the charging and discharging behaviors of the GCD curve have higher coulomb efficiency, but has a certain pseudocapacitance component, which is matched with the analysis result of a CV curve, and the specific capacity of LSPB-K-5 at the current density is about 202F/g, which is higher than LSPB-K-1 and LSPB-K-2, but is smaller than LSPB-K-3 and LSPB-K-4, which is matched with the analysis result of the CV curve, can be calculated by the discharging time, as shown in the figure 10. As shown in FIG. 11, the specific capacity of LSPB-K-5 was 221F/g at a current density of 0.5A/g, and 157F/g at an increase in current density to 20A/g, with a specific capacity retention of 71.04%, slightly better than LSPB-K-1 and LSPB-K-2, but worse than LSPB-K-3 and LSPB-K-4. As shown in FIG. 12, the LSPB-K-5 cycle stability curve shows that the specific capacity of LSPB-K-5 has almost no attenuation after 10000 charge and discharge cycles at a current density of 5A/g, and has good cycle stability.
The X-ray diffraction spectrum characterization of LSPB-K-C-4 was performed as shown in FIG. 2, wherein there were two broad diffraction bands at 21℃and 43℃corresponding to the 002, 101 crystal planes, respectively, of the carbon material, the broad diffraction bands indicating that LSPB-K-C-4 had an amorphous structure. The Raman spectrum of LSPB-K-C-4 is shown in FIG. 3, where at 1340 and 1580 cm -1 The scattering peaks at which the ratio IG/ID of the intensities of the G-band and D-band is 1.11 correspond to the D-band induced by defects and disordered structures present in the material and the G-band induced by the stretching motion of all sp2 atom pairs in the carbocyclic or long chain, respectively. X-ray photoelectron spectroscopy of LSPB-K-C-4 as shown in FIG. 4, wherein the binding energies are 283.4 and 532.3 eVCharacteristic peaks corresponding to the binding energy of C1 s and O1 s electrons, respectively, indicate the existence of C and O elements in LSPB-K-C-4, and further analysis shows that the percentage of C, O and N atoms is 87.87%, 10.82% and 1.31%, respectively, and no obvious characteristic peak of N1 s atoms can be observed in the X-ray photoelectron spectrum due to the low N content. As shown in the SEM image of LSPB-K-C-4, as shown in FIG. 5, it can be seen that LSPB-K-C-4 has a porous structure and the presence of macropores of 200 to 800. 800 nm can be observed. As shown in FIG. 6, a TEM image of LSPB-K-C-4 shows that a large number of micropores of 2 nm or less can be observed. As shown in FIG. 7, the N2 adsorption-desorption isotherm of LSPB-K-C-4 shows that the N2 adsorption-desorption isotherm of LSPB-K-C-4 is of type I, and shows that the LSPB-K-C-4 is of a porous structure mainly comprising micropores, and the specific surface area of the LSPB-K-C-4 is 868.02 m 2 And/g, the specific surface area of the material is obviously lower than that of an electrode material LSPB-K-4 prepared by microwave carbonization under the same activation condition, which shows that compared with common high-temperature carbonization, the microwave carbonization is fast and energy-saving, and the obtained material has larger specific surface area. As shown in FIG. 8, the pore size distribution of LSPB-K-C-4 shows that there are 3 peaks at 0.48, 0.80 and 1.22 nm for LSPB-K-C-4, indicating that the micropores predominate over these 3 sizes and that the total pore volume is 0.36 cm 3 Per g, the volumes of micropores, mesopores and macropores are 0.28, 0.01 and 0.07, cm, respectively 3 The volume ratio of the micropores reaches 77.8%, the average pore diameter is about 1.65 and nm, and the pore volume and the average pore diameter are lower than those of the electrode material LSPB-K-4 obtained by common high-temperature carbonization. At a scan rate of 20 mV/s, the cyclic voltammetric CV curve of LSPB-K-C-4, as shown in FIG. 9, can be seen from which the CV curve of LSPB-K-C-4 presents an irregular rectangle, indicating that the capacitive behavior of LSPB-K-C-4 has a certain pseudocapacitive component, which is mainly caused by its higher oxygen content, and the area enclosed by its CV curve is significantly smaller than that of LSPB-K-4, indicating that its specific capacity is lower than that of LSPB-K-4, indicating that the electrode material prepared by microwave carbonization under the same activation conditions has higher specific capacity. When the current density is 2A/g, the GCD curve of LSPB-K-C-4 is constant-current charge and discharge, as shown in figure 10, the GCD curve of LSPB-K-C-4 is basically symmetrical in shape, but has a certain degree of bending, which shows that the charge and discharge behaviors have higher coulomb efficiency but existThe specific capacity of LSPB-K-C-4 under the current density is about 187F/g and is obviously lower than that of LSPB-K-4, and the specific capacity is consistent with the analysis result of the CV curve. As shown in FIG. 11, the specific capacity of LSPB-K-C-4 is 201F/g when the current density is 0.5A/g, and is 131F/g when the current density is increased to 20A/g, the specific capacity retention rate is 65.17%, and the rate capability is obviously lower than that of LSPB-K-4, which indicates that the electrode material prepared by microwave carbonization under the same activation condition has higher rate capability. As shown in FIG. 12, the LSPB-K-C-4 cycle stability curve shows that the specific capacity of LSPB-K-C-4 hardly decays after 10000 charge and discharge cycles at a current density of 5A/g, and has good cycle stability.
The porous biomass carbon electrode material is prepared by using KOH as a microwave absorbent and a pore-forming agent thereof and performing microwave carbonization, and has a three-dimensional porous structure, wherein the porous structure mainly comprises micropores and macropores and mesopores, and the specific surface area of the porous biomass carbon electrode material can reach 1207.26m 2 Per gram, pore volume of 0.55 cm 3 The average pore diameter per gram is 1.80 and nm, the high specific capacity, the high rate capability and the good cycle stability are realized, the specific capacity can reach 294F/g when the current density is 0.5A/g, the retention rate of the specific capacity can reach 75% when the current density is increased to 20A/g, and the specific capacity has almost no attenuation compared with the initial capacity after 10000 charge and discharge cycles when the current density is 5A/g.
The preparation method of the porous biomass carbon electrode material disclosed by the embodiment does not need additional pretreatment and activation steps, integrates carbonization and activation processes in one step, and only needs 6-12 min in the whole carbonization-activation process, so that the preparation method is simple, quick and energy-saving.
In another aspect, a method for preparing an electrode sheet is provided, including:
dispersing an ethanol solution of the porous biomass carbon electrode material, the acetylene black and the polytetrafluoroethylene prepared based on the porous biomass carbon electrode material into absolute ethanol to prepare slurry, wherein the mass ratio of the porous biomass carbon electrode material to the acetylene black to the polytetrafluoroethylene can be 8:1:1, and when the porous biomass carbon electrode material, the acetylene black and the polytetrafluoroethylene are dispersed into the absolute ethanol, magnetic stirring or ultrasonic can be used for uniformly dispersing, the stirring rate is 200-400 r/min, and the ultrasonic power is 400-600W; the porous biomass carbon electrode material in the slurry is an active substance, acetylene black is a conductive agent, polytetrafluoroethylene is an adhesive, the mass ratio of the porous biomass carbon electrode material to the acetylene black to the polytetrafluoroethylene can be 8:1:1, the active substance can be ensured to be a main component, and meanwhile, the consumption of the conductive agent and the adhesive can be ensured to meet the minimum requirement;
coating the slurry on a current collector, drying, tabletting by a tabletting machine to prepare the electrode slice, wherein the current collector is foamed nickel, the loading amount of active substances on the current collector is 2-4 mg, and the pressure of the tabletting machine is 8-12 MPa so as to ensure the contact performance between the active substances and the current collector.
In a further aspect, an electrode sheet is provided, and the electrode sheet is prepared by the preparation method.
In the description, each embodiment is described in a progressive manner, and each embodiment is mainly described to be different from other embodiments, so that the same and similar parts of each embodiment are mutually referred to, and the embodiments and technical features in the embodiments can be mutually combined to obtain a new embodiment without conflict.
Having thus described the technical aspects of the present application with reference to the preferred embodiments illustrated in the accompanying drawings, it should be understood by those skilled in the art that the scope of the present application is not limited to the specific embodiments, and those skilled in the art may make equivalent changes or substitutions to the relevant technical features without departing from the principles of the present application, and those changes or substitutions will now fall within the scope of the present application.
Claims (10)
1. The preparation method of the porous biomass carbon electrode material is characterized by comprising the following steps of:
s1, cutting the loofah sponge into small blocks, performing ultrasonic treatment by using deionized water and absolute ethyl alcohol for 20-40 min, and drying at 60-90 ℃;
s2, soaking the loofah sponge in KOH solution with the concentration of 1.0-5.0 mol/L for 1-3 h;
s3, taking out the loofah sponge, and drying at 60-90 ℃;
s4, placing the loofah sponge into a quartz tube of a microwave tube type furnace, performing microwave carbonization in a nitrogen atmosphere, wherein the flow rate of the nitrogen is 100-300 mL/min, the microwave power is 800-1200W, the microwave carbonization temperature is 500-800 ℃, and the heat preservation time is 4-8 min;
and S5, taking out the loofah sponge, grinding the loofah sponge into powder, washing the powder with an HCl solution with the concentration of 1-3 mol/L, washing the powder to be neutral with deionized water, and drying the powder at the temperature of 60-90 ℃ to obtain the porous biomass carbon electrode material.
2. The method for preparing the porous biomass carbon electrode material according to claim 1, wherein,
s1, performing ultrasonic treatment for 30min;
the drying temperature was 80 ℃.
3. The method for preparing the porous biomass carbon electrode material according to claim 1, wherein,
in S2, the concentration of KOH solution is 4.0 mol/L;
the soaking time is 2 hours.
4. The method for preparing the porous biomass carbon electrode material according to claim 1, wherein,
in S3, the drying temperature is 80 ℃.
5. The method for preparing the porous biomass carbon electrode material according to claim 1, wherein,
in S4, the flow rate of nitrogen is 200 mL/min, the microwave power is 1000W, the microwave carbonization temperature is 600 ℃, and the heat preservation time is 5 min.
6. The method for preparing the porous biomass carbon electrode material according to claim 1, wherein,
in S5, the concentration of the HCl solution is 2.0 mol/L, and the times of washing with the HCl solution are 3 times;
the drying temperature was 80 ℃.
7. A method for producing an electrode sheet, comprising:
preparing a porous biomass carbon electrode material based on the porous biomass carbon electrode material preparation method of any one of claims 1 to 6;
dispersing porous biomass carbon electrode material, acetylene black and polytetrafluoroethylene in absolute ethyl alcohol to prepare slurry;
and coating the slurry on a current collector, drying, tabletting by a tablet press, and preparing the electrode slice.
8. The method for producing an electrode sheet according to claim 7, wherein,
the mass ratio of the biomass carbon electrode material dispersed into the absolute ethyl alcohol to the acetylene black to the polytetrafluoroethylene is 8:1:1;
when the porous biomass carbon electrode material, the acetylene black and the polytetrafluoroethylene are dispersed into the absolute ethyl alcohol, magnetic stirring or ultrasonic dispersion is used, wherein when the magnetic stirring is used, the stirring speed is 200-400 r/min; when ultrasonic dispersion is used, the ultrasonic power is 400-600W.
9. The method for producing an electrode sheet according to claim 7, wherein,
the current collector is foam nickel, and the loading amount of active substances on the current collector is 2-4 mg;
the tabletting pressure is 8-12 MPa.
10. An electrode sheet prepared by the method of any one of claims 7 to 9.
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