CN114349002A - Preparation method of cellulose aerogel-MXene porous carbon electrode material - Google Patents
Preparation method of cellulose aerogel-MXene porous carbon electrode material Download PDFInfo
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- CN114349002A CN114349002A CN202111543100.5A CN202111543100A CN114349002A CN 114349002 A CN114349002 A CN 114349002A CN 202111543100 A CN202111543100 A CN 202111543100A CN 114349002 A CN114349002 A CN 114349002A
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- 239000001913 cellulose Substances 0.000 title claims abstract description 46
- 239000007772 electrode material Substances 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000004108 freeze drying Methods 0.000 claims abstract description 16
- 230000004913 activation Effects 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 7
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- 238000005530 etching Methods 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 14
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
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- 101000782621 Bacillus subtilis (strain 168) Biotin carboxylase 2 Proteins 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- -1 Transition metal carbides Chemical class 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
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- 238000004146 energy storage Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000007731 hot pressing Methods 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses a preparation method of a cellulose aerogel-MXene porous carbon electrode material, which comprises the following steps: firstly, adding NaOH and urea powder into deionized water, uniformly stirring, and adding cellulose to obtain a mixed solution; by using HCl/LiF to Ti3AlC2Etching and layering to prepare MXene dispersion liquid; and uniformly mixing the MXene dispersion liquid with the mixed liquid, precooling, freeze-drying, carbonizing, finally mixing the sample with KOH, and activating to obtain the cellulose aerogel-MXene porous carbon electrode material. The method of the invention takes the cellulose aerogel as a carbon source and a framework, and compounds the MXenes material to improve the conductivity, and further improves the specific capacitance through KOH activation. In addition, the method has the advantages of wide raw material source, simple preparation process, low equipment cost, novelty and environmental protection.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a preparation method of a cellulose aerogel-MXene porous carbon electrode material.
Background
The generation mode of cellulose is mainly plant photosynthesis and is the most abundant renewable resource in the ecological environment at present. According to estimation statistics, the growth on the earth is distributed in all plants, the cellulose contained in cotton is the most in nature and is up to about 90%, while in the growing wood, the cellulose source is extremely wide, the cellulose is non-toxic, good in degradability, green and safe, and the cellulose can be renewable resources in various shapes such as sheets, films, threads and powder, and the pressure of using non-renewable resources such as coal, petroleum and the like can be relieved by processing the cellulose to produce the biofuel cell. Research on functional cellulosic materials has received a great deal of attention from researchers in the relevant fields.
Transition metal carbides, nitrides and carbonitrides, collectively referred to as MXenes, are an emerging family of two-dimensional materials that have received much attention since their advent. The graphene material has the performance similar to that of graphene, has excellent conductivity, higher specific surface area, higher toughness and hardness, and is widely applied to multiple directions such as energy storage, sensing, adsorption and the like. Currently, energy storage and conversion devices such as alkali metal ion batteries and supercapacitors hold great promise for renewable energy and electric vehicles, and play a vital role in environmental regulation. The MXenes synergistic heterostructure not only can give full play to the advantages of each component, but also can utilize synergistic effect to improve electrochemical performance.
Disclosure of Invention
The invention aims to provide a preparation method of a cellulose aerogel-MXene porous carbon electrode material, which improves the conductivity and specific capacitance of the electrode material.
The technical scheme adopted by the invention is that the preparation method of the cellulose aerogel-MXene porous carbon electrode material specifically comprises the following steps:
step 3, adopting HCl/LiF to Ti3AlC2Etching and layering to prepare MXene dispersion liquid;
step 4, uniformly mixing the MXene dispersion liquid with the mixed liquid obtained in the step 2, then precooling, freeze-drying and finally carbonizing to obtain a carbonized sample;
and 5, mixing the sample obtained in the step 4 with KOH, and placing the mixture in a tubular furnace for activation treatment to obtain the cellulose aerogel-MXene porous carbon electrode material.
The present invention is also characterized in that,
in the step 1, the drying temperature is 80-100 ℃, and the drying time is 8-40 h.
In step 3, the method specifically comprises the following steps: mixing LiF and HCl to react for 30min, and adding Ti3AlC2Slowly adding the powder into a uniform mixture of LiF and HCl, and stirring for 24 hours at 35 ℃ to obtain a mixed dispersion liquid after full reaction; then washing the mixed dispersion with deionized water at a centrifugal speed of 3500rpm until the pH of the supernatant reaches 6.0, performing ultrasonic treatment for 20min at 180W, and finally centrifuging at a speed of 3500rpm for 1h to obtain MXene dispersion.
In the step 4, the precooling temperature is-25 ℃, and the precooling time is 15-30 h; the freeze drying temperature is-40 to-60 ℃; the freeze drying time is 24-80 h.
In step 4, the carbonization conditions are specifically as follows: introducing nitrogen at a rate of 5-100 mL/s, heating to 500-.
In step 5, the mass ratio of the sample to KOH is 0.5-1: 1-3.
In step 5, the activation conditions are specifically: introducing nitrogen at a rate of 5-100 mL/s, heating to 500-.
The invention has the beneficial effects that: the cellulose aerogel is used as a carbon source and a framework, and is compounded with the MXenes material to improve the conductivity, and the specific capacitance is further improved by KOH activation. In addition, the method has the advantages of wide raw material source, simple preparation process, low equipment cost, novelty and environmental protection.
Drawings
FIG. 1 is a constant current charge-discharge test spectrum (GCD) of the electrode material obtained in example 1 of the present invention;
FIG. 2 is a constant current charge/discharge test spectrum (GCD) of the electrode material obtained from the control group in example 1 of the present invention;
FIG. 3 is an Electrochemical Impedance Spectroscopy (EIS) of the electrode material obtained in example 2 of the present invention;
FIG. 4 is an Electrochemical Impedance Spectroscopy (EIS) of the electrode material obtained from the control group in example 2 of the present invention;
FIG. 5 is a chart showing cyclic voltammetry test spectra (CV) of electrode materials obtained from experimental group and control group in example 3 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following detailed description and accompanying drawings.
The preparation method of the cellulose aerogel-MXene porous carbon electrode material specifically comprises the following steps:
the drying temperature is 80-100 ℃, and the drying time is 8-40 h;
the mass ratio of NaOH to urea powder to deionized water is 1-10: 1-10: 50-150;
step 3, adopting HCl/LiF to Ti3AlC2Etching and layering to prepare MXene dispersion liquid;
the method specifically comprises the following steps: mixing LiF and HCl to react for 30min, and adding Ti3AlC2Slowly adding the powder into a uniform mixture of LiF and HCl, and stirring for 24 hours at 35 ℃ to obtain a mixed dispersion liquid after full reaction; then washing the mixed dispersion with deionized water at a centrifugal speed of 3500rpm until the pH of the supernatant reaches 6.0, performing ultrasonic treatment for 20min at 180W, and finally centrifuging at a speed of 3500rpm for 1h to obtain MXene dispersion;
step 4, uniformly mixing the MXene dispersion liquid with the mixed liquid obtained in the step 2, then precooling, freeze-drying and finally carbonizing to obtain a carbonized sample;
pre-cooling temperature is-25 ℃, and pre-cooling time is 15-30 h; the freeze drying temperature is-40 to-60 ℃; the freeze drying time is 24-80 h;
the carbonization conditions are specifically as follows: introducing nitrogen at the rate of 5-100 mL/s, raising the temperature to 500-900 ℃ at the rate of 2-10 ℃/min, preserving the heat for 2h, and cooling to the room temperature;
the mass ratio of the sample to KOH is 0.5-1: 1-3;
the activation conditions are specifically as follows: introducing nitrogen at a rate of 5-100 mL/s, raising the temperature to 500-900 ℃ at a rate of 2-10 ℃/min, preserving the heat for 1h, and cooling to room temperature.
Example 1
Weighing 1g of cellulose, drying the cellulose for 12h in an environment at 60 ℃, and then adding NaOH: urea: the water content is 7: 12: 81 is prepared into 30ml of transparent solution in proportion, and then the cellulose is dissolved into the solution; slowly adding 1g of MAX powder into a uniform mixture of 10g of LiF and 2g of HCl, and stirring for 24 hours at 35 ℃ to obtain a fully reacted mixed solution; then, the mixed solution was washed with deionized water at a centrifugal speed of 3500rpm until the pH of the supernatant reached 6.0, sonicated at 180W for 20min, and finally centrifuged at 3500rpm for 1h to obtain an MXenes dispersion. Then mixing the two solutions in a ratio of 10:1, uniformly dispersing, and freezing the prepared dissolving system for 15 hours in a refrigerator environment at-25 ℃; and then, carrying out freeze drying for 72h by using a freeze dryer, and obtaining the composite cellulose aerogel after the freeze drying is finished. Then putting the aerogel into a tube furnace for carbonization, wherein the carbonization conditions are as follows: heating to 700 deg.C at a rate of 5 deg.C/min under the condition of introducing nitrogen, maintaining for 120min, and cooling to room temperature; the flow rate of nitrogen was 40 mL/min. After carbonization, mixing the sample with KOH, putting the mixture into a tube furnace for activation, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 1h, and finally cooling to room temperature; the flow rate of nitrogen was 40 mL/min. Finally preparing an electrode material ACC, and naming the carbon material without activation treatment as CC.
And washing and drying the obtained material to obtain the activated carbon-based supercapacitor electrode material. And mixing the active materialMaterial preparation: acetylene black: the polytetrafluoroethylene suspension was mixed at 16: 3: 1, uniformly coating the mixture on the surface of foamed nickel, drying, tabletting an electrode with similar load capacity, hot-pressing the electrode into a super capacitor under the pressure of 15MPa, representing the electrochemical performance of the super capacitor by using a Cowster CS150H electrochemical workstation, carrying out constant-current charge-discharge test on the electrode in a 6M KOH electrolyte solution, and measuring the electrochemical performance of the obtained product, wherein the constant-current charge-discharge test spectrum of ACC is shown in figure 1, and the curves are symmetrical isosceles triangles, which indicates that the ACC electrode has better reversibility in application. And the constant current charge-discharge test spectrum of the CC electrode is shown in figure 2, the ACC discharge time is observed to be obviously longer than that of the CC electrode, which shows that the ACC has higher specific capacitance through activation treatment, the electrode performance is improved to a certain extent, and the ACC specific capacitance 152.4F g is obtained through calculation-190.8F g above CC-1。
Example 2
Weighing 1g of cellulose, drying the cellulose for 12h in an environment at 60 ℃, and then adding NaOH: urea: the water content is 7: 12: 81 is prepared into 30ml of transparent solution in proportion, and then the cellulose is dissolved into the solution; slowly adding 1g of MAX powder into a uniform mixture of 5g of LiF and 2g of HCl, and stirring for 24 hours at 35 ℃ to obtain a fully reacted mixed solution; then, the mixed solution was washed with deionized water at a centrifugal speed of 3500rpm until the pH of the supernatant reached 6.0, sonicated at 180W for 20min, and finally centrifuged at 3500rpm for 1h to obtain an MXenes dispersion. Then mixing the two solutions in a ratio of 5:1, uniformly dispersing, and freezing the prepared dissolving system for 20 hours in a refrigerator environment at the temperature of-25 ℃; and then, carrying out freeze drying for 72h by using a freeze dryer, and obtaining the composite cellulose aerogel after the freeze drying is finished. Then putting the aerogel into a tube furnace for carbonization, wherein the carbonization conditions are as follows: heating to 800 ℃ at the speed of 5 ℃/min under the condition of introducing nitrogen, preserving heat for 2h, and finally cooling to room temperature; the flow rate of nitrogen is 40-60 mL/min. Mixing the obtained sample with KOH, and placing the mixture in a tubular furnace for activation treatment; finally preparing an electrode material ACC-1, and naming the carbon material without activation treatment as CC.
The ACC-1 electrochemical impedance spectrum is shown in fig. 3, and it can be seen that in the high frequency region, the intercept of the spectrum on the x-axis is called the equivalent resistance, which includes the electrolyte resistance, the active material, the substrate internal resistance, and the contact resistance of the active material and the current collector. Meanwhile, the ion transfer capability of the electrode material can be clearly observed through the slope of the image, and the larger the slope is, the larger the ion transfer capability is. Thus, the ACC-1 has better ion transfer capability. The CC electrochemical impedance spectrogram is shown in fig. 4, meanwhile, due to the appearance of a small semicircle image of a high-frequency region caused by the formation of an electric double layer of the electrode and the electrolyte, the diameter of the small semicircle represents the transfer resistance of electrons, the diameter of the semicircle of the ACC-1 can be observed to be obviously smaller than the CC, and the ACC-1 is shown to have smaller electron transfer resistance and be more favorable for the rapid passing of the electrons.
Example 3
The invention relates to a preparation method of a porous carbon electrode material compounded by Mxenes and cellulose aerogel, which is implemented according to the following steps:
weighing 2g of cellulose, drying the cellulose for 12h in an environment at 60 ℃, and then adding NaOH: urea: the water content is 7: 12: 81 is prepared into 30ml of transparent solution in proportion, and then the cellulose is dissolved into the solution; slowly adding 2g of MAX powder into a uniform mixture of 10g of LiF and 2g of HCl, and stirring for 24 hours at 35 ℃ to obtain a fully reacted mixed solution; then, the mixed solution was washed with deionized water at a centrifugation speed of 4000rpm until the pH of the supernatant reached 6.0, sonicated at 180W for 20min, and finally centrifuged at 4000rpm for 1h to obtain an MXenes dispersion. Then mixing the two solutions in a ratio of 10:1, uniformly dispersing, and freezing the prepared dissolving system for 30 hours in a refrigerator environment at the temperature of-25 ℃; and then, carrying out freeze drying for 72h by using a freeze dryer, and obtaining the composite cellulose aerogel after the freeze drying is finished. Then putting the aerogel into a tube furnace for carbonization, wherein the carbonization conditions are as follows: heating to 700 deg.C at a rate of 3 deg.C/min under the condition of introducing nitrogen, maintaining the temperature for 150min, and cooling to room temperature; the flow rate of nitrogen is 40-60 mL/min. Mixing a sample with KOH, and placing the mixture in a tubular furnace for activation treatment; finally preparing an electrode material ACC-2, and naming the carbon material without activation treatment as CC.
Fig. 5 shows that both materials are in a rectangular-like shape in a cyclic voltammetry test spectrogram, the capacitance performance of the materials is represented by the size of the integrated area of the cyclic voltammetry test spectrogram, the area of ACC-2 is obviously far larger than CC, and the modified materials have larger specific capacitance.
Claims (7)
1. The preparation method of the cellulose aerogel-MXene porous carbon electrode material is characterized by comprising the following steps:
step 1, drying cellulose;
step 2, adding NaOH and urea powder into deionized water, uniformly stirring, and then adding cellulose to obtain a mixed solution;
step 3, adopting HCl/LiF to Ti3AlC2Etching and layering to prepare MXene dispersion liquid;
step 4, uniformly mixing the MXene dispersion liquid with the mixed liquid obtained in the step 2, then precooling, freeze-drying and finally carbonizing to obtain a carbonized sample;
and 5, mixing the sample obtained in the step 4 with KOH, and placing the mixture in a tubular furnace for activation treatment to obtain the cellulose aerogel-MXene porous carbon electrode material.
2. The preparation method of the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 1, the drying temperature is 80-100 ℃ and the drying time is 8-40 h.
3. The method for preparing the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 3, specifically: mixing LiF and HCl to react for 30min, and adding Ti3AlC2Slowly adding the powder into a uniform mixture of LiF and HCl, and stirring for 24 hours at 35 ℃ to obtain a mixed dispersion liquid after full reaction; then the mixture was centrifuged at 3500rpm using deionized waterWashing the dispersion until the pH of the supernatant reaches 6.0, performing ultrasonic treatment at 180W for 20min, and finally centrifuging at 3500rpm for 1h to obtain MXene dispersion.
4. The preparation method of the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 4, the pre-cooling temperature is-25 ℃ and the pre-cooling time is 15-30 h; the freeze drying temperature is-40 to-60 ℃; the freeze drying time is 24-80 h.
5. The method for preparing the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 4, the carbonization conditions are specifically as follows: introducing nitrogen at a rate of 5-100 mL/s, heating to 500-.
6. The method for preparing the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 5, the mass ratio of the sample to KOH is 0.5-1: 1-3.
7. The method for preparing the cellulose aerogel-MXene porous carbon electrode material according to claim 1, wherein in the step 5, the activation conditions are specifically as follows: introducing nitrogen at a rate of 5-100 mL/s, heating to 500-.
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| CN114804101A (en) * | 2022-06-10 | 2022-07-29 | 南京林业大学 | Method for preparing straw-based activated carbon by MXene assisted microwave radiation |
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