CN109437174B - Doping carbonization C60Preparation method of microstrip graphene aerogel composite electrode material - Google Patents
Doping carbonization C60Preparation method of microstrip graphene aerogel composite electrode material Download PDFInfo
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- CN109437174B CN109437174B CN201811344041.7A CN201811344041A CN109437174B CN 109437174 B CN109437174 B CN 109437174B CN 201811344041 A CN201811344041 A CN 201811344041A CN 109437174 B CN109437174 B CN 109437174B
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Abstract
Doping carbonization C60The invention discloses a preparation method of a microstrip graphene aerogel composite electrode material, and relates to a preparation method of a graphene aerogel composite electrode material. The invention aims to solve the problemsThe graphene aerogel has the technical problems of low strength, small specific surface area and large resistance. The method comprises the following steps: firstly preparing carbonized C60A microstrip; adjusting the pH value of the graphene oxide dispersion liquid, adding ascorbic acid, and then adding carbonized C60Mixing the mixture evenly by a micro-strip, and carrying out hydrothermal reaction to obtain the doped carbonized C60Microstrip graphene hydrogel; dialyzing, freeze-drying to obtain doped C60The microstrip graphene aerogel composite electrode material. The specific capacitance of the material under the current density of 0.5A/g is 150-153F/g, the material has good multiplying power performance, capacity loss is basically avoided after 1000 times of charging/discharging, and the resistance is only 0.38-0.40 omega. Can be used in the field of batteries.
Description
Technical Field
The invention relates to a doped C60A microstrip graphene aerogel composite electrode material and a preparation method thereof.
Background
Graphene has excellent electrical, optical, mechanical and other properties, but the flake graphene directly used as an electrode material has various problems, such as easy agglomeration, inability to prepare large graphene sheets under the influence of natural conditions and the like. These disadvantages severely limit the application of graphene to batteries, and thus reducing the stacking of graphene sheets becomes of great importance. Currently, the preparation of graphene aerogel is an approach for obtaining a porous graphene macrostructure with a large specific surface area. For example, chinese patent application No. 201810033667.X discloses a method for preparing graphene aerogel, which includes freezing graphene slurry or dispersion to obtain ice particles, and then freeze-drying to obtain aerogel powder, wherein the tap density of the aerogel powder is 21-71 mg/mL. The aerogel powder obtained by the method has low strength and small specific surface area. When the graphene aerogel is used for preparing an electrode, the resistance is large, and the specific capacitance of the electrode is small.
Disclosure of Invention
The invention provides a doped carbonized C for solving the technical problems of low strength, small specific surface area and large resistance of the existing graphene aerogel60A preparation method of a microstrip graphene aerogel composite electrode material.
Doped carbonized C of the invention60The preparation method of the microstrip graphene aerogel composite electrode material comprises the following steps:
firstly, preparing carbonized C60Microstrip:
adding isopropanol dropwise to C60CS of2Standing in solution at room temperature in isopropanol and CS2Is two phases of C60Taking out the micro-strip, drying the micro-strip in vacuum, then putting the micro-strip into a tube furnace, heating the micro-strip to 800-1000 ℃ under the protection of nitrogen, and preserving the heat for 2-2.5 hours to obtain carbonized C60A microstrip;
dispersing graphene oxide into deionized water to prepare graphene oxide dispersion liquid with the mass concentration of 2-7 mg/mL, adjusting the pH value of the graphene oxide dispersion liquid to 8-11 by using ammonia water, and adding ascorbic acid as a reducing agent to obtain mixed liquid; carbonizing C60Adding the micro-strips into the mixed solution, uniformly mixing, transferring the mixed solution into a reaction kettle, and carrying out hydrothermal reaction for 10-18 h at the temperature of 150-160 ℃ to obtain the doped carbonized C60Microstrip graphene hydrogel;
thirdly, the doping carbonization C obtained in the second step60Putting the micro-strip graphene hydrogel into 10-30% ethylene glycol aqueous solution for dialysis, and then freeze-drying to obtain doped C60The microstrip graphene aerogel composite electrode material.
The invention utilizes C60Microstrip as raw material, C60The micro-strip has weak conductive capability and is heated to be treated with C60The carbon in the carbon is converted into amorphous carbon, the disorder is increased, the carbon has larger surface area and firm mesoporous framework structure, and the carbon is carbonized60The microstrip is doped into the graphene, so that the accumulation of graphene sheet layers is reduced, the effective surface area of the composite material is increased fundamentally, and the improvement of the specific capacitance of the composite material is facilitated. On the other hand, carbonization of C60After the microstrip and the graphene aerogel are compounded, pi electrons of the composite material are richer, more activation sites are provided, and the electrochemical performance of the composite material is improved. The composite material electrode is used for charging and dischargingThe structure is difficult to change in the electricity process, the capacitance loss is extremely low, and the power characteristic is good, so that the specific capacitance value cycling stability and the multiplying power performance of the electrode material are integrally improved. There was substantially no capacity loss even after 1000 times of charge/discharge. And the equivalent series resistance of the composite electrode is only 0.38-0.40 omega, and the resistance is small.
The method can rapidly prepare the high-performance composite electrode material with high specific area and high porosity, and has the characteristics of simple operation and easily controlled conditions.
Drawings
FIG. 1 shows doped Carbonisation C prepared in example 160And (3) carrying out cyclic voltammograms on the microstrip graphene aerogel composite electrode material at different scanning speeds.
FIG. 2 shows doped Carbonisation C prepared in example 160The microstrip graphene aerogel composite electrode material has a constant current charge-discharge curve under different current densities.
FIG. 3 shows doped Carbonic C prepared in example 160And (3) a test chart of the cyclicity of the microstrip graphene aerogel composite electrode material under the current density of 10A/g.
FIG. 4 shows doped Carbonic C prepared in example 160And (3) an alternating current impedance spectrogram of the microstrip graphene aerogel composite electrode material.
Detailed Description
The first embodiment is as follows: doped carbon C of the present embodiment60The preparation method of the microstrip graphene aerogel composite electrode material comprises the following steps:
firstly, preparing carbonized C60Microstrip:
adding isopropanol dropwise to C60CS of2Standing in solution at room temperature in isopropanol and CS2Is two phases of C60Taking out the micro-strip, drying the micro-strip in vacuum, then putting the micro-strip into a tube furnace, heating the micro-strip to 800-1000 ℃ under the protection of nitrogen, and preserving the heat for 2-2.5 hours to obtain carbonized C60A microstrip;
secondly, dispersing graphene oxide into deionized water to prepare the oxidized stone with the mass concentration of 2-7 mg/mLAdjusting the pH value of the graphene oxide dispersion liquid to 8-11 by using ammonia water, and adding ascorbic acid as a reducing agent to obtain a mixed liquid; carbonizing C60Adding the micro-strips into the mixed solution, uniformly mixing, transferring the mixed solution into a reaction kettle, and carrying out hydrothermal reaction for 10-18 h at the temperature of 150-160 ℃ to obtain the doped carbonized C60Microstrip graphene hydrogel;
thirdly, the doping carbonization C obtained in the second step60Putting the micro-strip graphene hydrogel into 10-30% ethylene glycol aqueous solution for dialysis, and then freeze-drying to obtain doped C60The microstrip graphene aerogel composite electrode material.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that C is described in the first embodiment60CS of2In solution C60The concentration of (A) is 2-4 mg/ml; the rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment differs from the first or second embodiment in the volume of isopropyl alcohol and C in the first step60The mass ratio of (a) to (b) is 1 ml: (0.6-0.8) mg; the other embodiments are the same as the first or second embodiment.
The fourth concrete implementation mode: the difference between the present embodiment and one of the first to third embodiments is that the temperature of the vacuum drying in the first step is 60 to 65 ℃; the other is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that the preparation method of graphene oxide in step two is as follows: firstly, 1g of graphite powder and 23ml of concentrated sulfuric acid are placed in a beaker, 3g of potassium permanganate is gradually added into a mixed solution, an ice-water bath is used in the process, the reaction temperature is kept below 5 ℃, and dark green viscous liquid is obtained; then placing the mixture in a water bath at 45 ℃ to stir and react for 1h, adding 70ml of deionized water, stirring for 10 min at 95 ℃, and pouring 200ml of deionized water and 2ml of hydrogen peroxide with the mass percentage concentration of 30% to remove unreacted potassium permanganate, wherein the solution is golden yellow or bright yellow; centrifuging the golden yellow or bright yellow solution for 5 minutes at 7000 r/min by using 3mol/L hydrochloric acid to remove metal ions in the reaction, washing the precipitate subjected to acid treatment by using deionized water until the pH of the supernatant is 6, wherein the solution is tan, taking out the obtained tan viscous jelly, and performing vacuum drying at 60 ℃ for 12 hours to obtain solid graphene oxide; the other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: this embodiment is different from the first to fifth embodiments in that C is carbonized in the second step60The mass ratio of the microstrip to the graphene oxide in the graphene oxide dispersion liquid is 1: (10-15); the other is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and the first to the sixth embodiment is that the dialysis time in the third step is 6 to 12 hours; the other is the same as in one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the embodiment and one of the first to seventh embodiments is that the temperature of the freeze drying in the third step is-50 ℃ to-60 ℃, and the drying time is 36-48 hours; the other is the same as one of the first to seventh embodiments.
The present invention will be described in further detail below with reference to the accompanying drawings by way of experiments, but the present invention is not limited to the following embodiments.
Example 1: doped carbon C of the present example60The preparation method of the microstrip graphene aerogel composite electrode material comprises the following steps:
firstly, preparing carbonized C60Microstrip:
adding 30mL of isopropanol dropwise into 10mL of CS2 solution of C60 with concentration of 2mg/mL, standing at room temperature for 24h, adding isopropanol and CS2Is two phases of C60Taking out the micro-strip, vacuum drying at 60 deg.C for 6h, placing into a tube furnace, heating to 800 deg.C under nitrogen protection, and maintaining for 2h to obtain carbonized C60A microstrip;
secondly, dispersing 120mg of graphene oxide into 40mL of deionized water to prepare graphene oxide dispersion liquid with the mass concentration of 3mg/mL, and then separating the graphene oxideAdjusting the pH of the dispersion to 10 by using ammonia water, and then adding 0.5mL of ascorbic acid as a reducing agent to obtain a mixed solution; 10mg of carbonized C60Adding the mixture into a micro-strip, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction for 10 hours at the temperature of 150 ℃ to obtain the doped carbonized C60Microstrip graphene hydrogel;
thirdly, the doping carbonization C obtained in the second step60Dialyzing the graphene hydrogel with micro strips in 10 mass percent aqueous solution of ethylene glycol for 6 hours, and freeze-drying the graphene hydrogel at the temperature of 60 ℃ below zero for 36 hours to obtain the doped carbonized C60The microstrip graphene aerogel composite electrode material.
The preparation method of the graphene oxide in the second step is as follows: firstly, 1g of graphite powder and 23ml of concentrated sulfuric acid are placed in a beaker, 3g of potassium permanganate is gradually added into a mixed solution, an ice-water bath is used in the process, the reaction temperature is kept below 5 ℃, and dark green viscous liquid is obtained; then placing the mixture in a water bath at 45 ℃ to stir and react for 1h, adding 70ml of deionized water, stirring for 10 min at 95 ℃, and pouring 200ml of deionized water and 2ml of hydrogen peroxide with the mass percentage concentration of 30% to remove unreacted potassium permanganate, wherein the solution is golden yellow or bright yellow; and (3) centrifuging the golden yellow or bright yellow solution for 5 minutes at the rotating speed of 7000 r/min by using 3mol/L hydrochloric acid to remove metal ions in the reaction, washing the precipitate subjected to acid treatment by using deionized water until the pH of the supernatant is 6, wherein the solution is dark brown, taking out the dark brown viscous jelly, and performing vacuum drying at 60 ℃ for 12 hours to obtain solid graphene oxide.
The doped carbon C prepared in this example60The method comprises the steps of mixing a micro-strip graphene aerogel composite electrode material with polyvinylidene fluoride and acetylene black according to a mass ratio of 8:1:1, uniformly coating the mixture on foamed nickel, carrying out vacuum drying for 24 hours at the temperature of 60 ℃, carrying out suction filtration by using an alcohol-water solution of potassium hydroxide with the molar concentration of 6mol/L, and soaking for 24 hours to obtain the electrode slice. The electrode is taken as a working electrode, a platinum electrode is taken as a counter electrode, mercury and mercury oxide are taken as reference electrodes, a three-electrode system is taken, electrolyte is 6mol/L potassium hydroxide, and an electrochemical workstation is utilizedAnd carrying out electrochemical performance test.
Doped Carbonic acid C prepared in example 160The cyclic voltammogram of the microstrip graphene aerogel composite electrode material at different scanning speeds is shown in fig. 1, and it can be seen from fig. 1 that the composite material keeps a good rectangle at a scanning speed of 5mV/s, which indicates that the composite material has good properties of double-layer capacitance, and the rectangle does not have large deviation with the increase of the scanning speed, which indicates that the composite electrode material has good stability.
Doped Carbonic acid C prepared in example 160The constant current charge-discharge curve graph of the microstrip graphene aerogel composite electrode material under different current densities is shown in fig. 2, and it can be seen from fig. 2 that the charge-discharge curve keeps an isosceles triangle shape in the constant current charge-discharge process, and it can be seen that the composite material has a very stable double electric layer property, the specific capacitance of the composite material is 153F/g under the current density of 0.5A/g, and the isosceles triangle shape still keeps very good with the increase of the current density, and it can be seen that the composite material has a very good multiplying power performance.
Doped Carbonic acid C prepared in example 160The test chart of the cyclicity of the microstrip graphene aerogel composite electrode material under the current density of 10A/g is shown in fig. 3, and as can be seen from fig. 3, the cyclicity of the electrode is good, the specific capacitance is hardly attenuated after 1000 times of charging/discharging, and the capacitance retention rate is still 96%, which indicates that the composite material has good cyclicity.
Doped Carbonic acid C prepared in example 160An alternating-current impedance spectrogram of the microstrip graphene aerogel composite electrode material is shown in fig. 4, and as can be seen from fig. 4, the electrode has relatively low resistance, and the equivalent series resistance of the electrode is 0.39 Ω, so that the electrode has good application in the aspect of electrodes.
Example 2: doped carbon C of the present example60The preparation method of the microstrip graphene aerogel composite electrode material comprises the following steps:
firstly, preparing carbonized C60Microstrip:
30mL of isopropanol were added dropwise to a concentration of 10mL of 2mg/ml of C60In CS2 solution, standing at room temperature for 24h, adding into isopropanol and CS2Is two phases of C60Taking out the micro-strip, vacuum drying at 60 deg.C for 6h, placing into a tube furnace, heating to 800 deg.C under nitrogen protection, and maintaining for 2h to obtain carbonized C60A microstrip;
dispersing 200mg of graphene oxide into 40mL of deionized water, ultrasonically dispersing for 2h, mechanically stirring until a uniformly dispersed and stable graphene oxide dispersion liquid with the mass concentration of 5mg/mL is formed, adjusting the pH value of the graphene oxide dispersion liquid to 11 by using ammonia water, and adding 0.7mL of ascorbic acid as a reducing agent to obtain a mixed solution; 15mg of carbonized C60Adding the mixture into a micro-strip, uniformly mixing, transferring into a reaction kettle, and carrying out hydrothermal reaction for 8 hours at the temperature of 170 ℃ to obtain the doped carbonized C60Microstrip graphene hydrogel;
thirdly, the doping carbonization C obtained in the second step60Dialyzing the graphene hydrogel with micro strips in 10 mass percent aqueous solution of ethylene glycol for 6 hours, and freeze-drying the graphene hydrogel at the temperature of 60 ℃ below zero for 36 hours to obtain the doped carbonized C60The microstrip graphene aerogel composite electrode material.
And the preparation method of the graphene oxide in the second step is the same as that of the embodiment 1.
The doped carbon C prepared in example 2 was subjected to the same process as in example 160And carrying out electrochemical performance test on the microstrip graphene aerogel composite electrode material.
Doped Carbonic acid C prepared in example 160The charging and discharging curve of the microstrip graphene aerogel composite electrode material keeps an isosceles triangle shape in the constant current charging and discharging process, the microstrip graphene aerogel composite electrode material has a very stable double electric layer property, the specific capacitance of the composite material is 150F/g under the current density of 0.5A/g, the isosceles triangle shape still keeps good along with the increase of the current density, and the composite material has good rate capability. Meanwhile, the electrode prepared by the composite electrode material has good cycle stability, the specific capacitance is hardly attenuated after 1000 times of charging/discharging, the capacitance retention rate is still 95 percent,the composite material has good cycle stability.
Claims (7)
1. Doping carbonization C60The preparation method of the microstrip graphene aerogel composite electrode material is characterized by comprising the following steps of:
firstly, preparing carbonized C60Microstrip:
adding isopropanol dropwise to C60CS of2Standing in solution at room temperature in isopropanol and CS2Is two phases of C60Taking out the micro-strip, drying the micro-strip in vacuum, then putting the micro-strip into a tube furnace, heating the micro-strip to 800-1000 ℃ under the protection of nitrogen, and preserving the heat for 2-2.5 hours to obtain carbonized C60A microstrip;
dispersing graphene oxide into deionized water to prepare graphene oxide dispersion liquid with the mass concentration of 2-7 mg/mL, adjusting the pH value of the graphene oxide dispersion liquid to 8-11 by using ammonia water, and adding ascorbic acid as a reducing agent to obtain mixed liquid; carbonizing C60Adding the micro-strips into the mixed solution, uniformly mixing, transferring the mixed solution into a reaction kettle, and carrying out hydrothermal reaction for 10-18 h at the temperature of 150-160 ℃ to obtain the doped carbonized C60Microstrip graphene hydrogel; wherein is carbonized C60The mass ratio of the microstrip to the graphene oxide in the graphene oxide dispersion liquid is 1: (10-15);
thirdly, the doping carbonization C obtained in the second step60Putting the micro-strip graphene hydrogel into 10-30% ethylene glycol aqueous solution for dialysis, and then freeze-drying to obtain doped C60The microstrip graphene aerogel composite electrode material.
2. A doped carbonated C as claimed in claim 160The preparation method of the microstrip graphene aerogel composite electrode material is characterized in that the step C in the step one60CS of2In solution C60The concentration of (b) is 2-4 mg/ml.
3. A blend according to claim 1 or 2Heterocarbon C60The preparation method of the microstrip graphene aerogel composite electrode material is characterized in that the volume of isopropanol and C in the step one60The mass ratio of (a) to (b) is 1 ml: (0.6-0.8) mg.
4. A doped carbonated C according to claim 1 or 260The preparation method of the microstrip graphene aerogel composite electrode material is characterized in that the temperature of vacuum drying in the step one is 60-65 ℃.
5. A doped carbonated C according to claim 1 or 260The preparation method of the microstrip graphene aerogel composite electrode material is characterized in that the preparation method of the graphene oxide in the second step is as follows: firstly, 1g of graphite powder and 23ml of concentrated sulfuric acid are placed in a beaker, 3g of potassium permanganate is gradually added into a mixed solution, an ice-water bath is used in the process, the reaction temperature is kept below 5 ℃, and dark green viscous liquid is obtained; then placing the mixture in a water bath at 45 ℃ to stir and react for 1h, adding 70ml of deionized water, stirring for 10 min at 95 ℃, and pouring 200ml of deionized water and 2ml of hydrogen peroxide with the mass percentage concentration of 30% to remove unreacted potassium permanganate, wherein the solution is golden yellow or bright yellow; and (3) centrifuging the golden yellow or bright yellow solution for 5 minutes at the rotating speed of 7000 r/min by using 3mol/L hydrochloric acid to remove metal ions in the reaction, washing the precipitate subjected to acid treatment by using deionized water until the pH of the supernatant is 6, wherein the solution is dark brown, taking out the dark brown viscous jelly, and performing vacuum drying at 60 ℃ for 12 hours to obtain solid graphene oxide.
6. A doped carbonated C according to claim 1 or 260The preparation method of the microstrip graphene aerogel composite electrode material is characterized in that the dialysis time in the third step is 6-12 hours.
7. A doped carbonated C according to claim 1 or 260Preparation of microstrip graphene aerogel composite electrode materialThe preparation method is characterized in that the freeze drying temperature in the third step is-50 ℃ to-60 ℃, and the drying time is 36-48 hours.
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| CA2866650A1 (en) * | 2012-03-09 | 2013-09-12 | Basf Se | Aerogel based on doped graphene |
| CN103496695A (en) * | 2013-09-30 | 2014-01-08 | 东南大学 | Preparation method of nitrogen-doped reducing graphene oxide aerogel |
| US10633255B2 (en) * | 2016-09-08 | 2020-04-28 | Lawrence Livermore National Security, Llc | Graphene macro-assembly-fullerene composite for electrical energy storage |
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| CN106698410B (en) * | 2016-12-05 | 2019-11-26 | 四川大学 | The preparation method of nitrogen atom doping carbon nanomaterial |
| CN106904606A (en) * | 2017-03-20 | 2017-06-30 | 中国石油大学(北京) | A kind of preparation method and its obtained doping carbon material of the carbon material that adulterates |
| CN108128769A (en) * | 2018-02-05 | 2018-06-08 | 山东佳星环保科技有限公司 | A kind of preparation method of the graphene aerogel electrode material of low-cost and high-performance |
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Inventor after: Ji Guancheng Inventor after: Zhang Lei Inventor after: Li Ji Inventor after: Liu Guoqiang Inventor before: Ji Guancheng Inventor before: Zhang Lei Inventor before: Li Ji |