CN112079356A - Modified activated carbon material, preparation method and application of modified activated carbon material in super capacitor - Google Patents
Modified activated carbon material, preparation method and application of modified activated carbon material in super capacitor Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- 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
Abstract
A modified activated carbon material, a preparation method and application of a super capacitor thereof. Taking activated carbon with the particle size of 5-200 mu m as a starting raw material, and carrying out mechanical densification treatment under the anaerobic condition to obtain the modified activated carbon material, wherein the blind hole rate is lower than 5 percent, and the tap density is more than 0.6g cm‑3Conductivity greater than 130S m‑1. The modified activated carbon material shows good electrochemical performance when being used as a supercapacitor electrode material: at 1A g‑1The mass specific capacity under the current density can be improved by 35 percent at most, the volume specific capacity can be improved by 330 percent at most, and the multiplying power performance and the cycling stability are excellent. In addition, the time for the self-discharge process to reduce the voltage to half of the initial voltage can be prolonged by 300% at most, and the voltage decay can be reduced by 20% at most after 48 hours.
Description
Technical Field
The invention relates to the field of electrode materials of supercapacitors, in particular to a modified activated carbon material, a preparation method and application of a supercapacitor thereof.
Background
The super capacitor has the advantages of high power density, quick charge and discharge, long service life and the like, plays more and more important roles in the fields of intelligent distributed power grid systems, military equipment, urban traffic track energy storage devices, engineering mechanical power, wind power generation systems and the like in recent years, and can replace the traditional battery to meet the requirements of electric automobiles on high-power discharge during braking and climbing. The key point of the development of the high-performance super capacitor lies in how to improve and enhance the performance of the core component, namely the electrode material, so that the research and the preparation of the high-performance electrode material become urgent.
The active carbon is an electrode material commonly adopted by commercial super capacitors at present, on one hand, the ultrahigh specific surface area and the developed pore structure of the active carbon provide a large number of energy storage sites and are a main source of the electric double layer capacity of the active carbon; on the other hand, large-scale industrial production of activated carbon materials prepared from low-cost raw materials such as coconut shells, coal, coke, etc. is currently achieved, and the low production cost is an important factor for their widespread use in commercial capacitors [ Energy & Environmental Science 2016,9(1):102-106 ]. However, with the rapid development of new application fields such as small-sized mobile devices and wearable devices, miniaturization and light weight become important development trends of supercapacitors in the future, and in this context, activated carbon as an electrode material also exposes many problems:
(1) from the structural point of view, the activated carbon material is usually a block with the particle size of 5-200 μm, the particle size distribution is not uniform, the particles are stacked loosely and have a large number of gaps, the loose organization form of the activated carbon material ensures that the activated carbon material needs to consume a large amount of electrolyte to fill the inner gaps, and the activated carbon material is easy to fall off when a large amount of electrolyte is coated on the surface of a current collector, so that the unit area loading capacity of the current collector is limited, and the consumption of the current collector is large (the prices of commercial carbon-coated aluminum foils, carbon-coated copper foils and foamed nickel current collectors are respectively 35-45, 45-65 and 30-55 ten thousand yuan/ton, and the surface densities are respectively 5-2). The use of a large amount of electrolyte and current collectors not only increases the proportion of inactive components in the device and reduces the overall capacity of the device, but also is not beneficial to the development of low cost and light weight of the device. In addition, the large specific surface area and porous structure of the activated carbon reduce its bulk density (0.3-0.6g cm)-3) Greatly limits the volume performance of the electrode material as a super capacitor, and is not beneficial to the miniaturization and portability of devicesDevelopment [ Energy ]&Environmental Science,2016,9：729-762.]。
(2) Because the activated carbon is mostly subjected to the preparation process of gradually activating the activating agent from outside to inside, the internal pore structure of the activated carbon is in a deep and zigzag branch shape, and a large number of blind holes and closed hole structures exist, so that the problems of incomplete electrolyte infiltration, large ion diffusion resistance and the like are caused, and the specific capacity of the activated carbon in aqueous electrolyte is about 100--1The requirements of practical application are far from being met; the active carbon is in an amorphous carbon structure, and the conductivity is poor, so that the rate capability of the active carbon as a super capacitor electrode material is limited.
(3) When the supercapacitor is disconnected from the charging circuit or load, a phenomenon of voltage decay, i.e., a self-discharge phenomenon, often occurs. Compared with a battery, the super capacitor has the advantages that the voltage attenuation is caused in the standby state of application equipment due to the rapid self-discharge rate, the reliability of energy and capacity parameters is reduced, and the service life is greatly shortened. The generation mechanisms of the self-discharge phenomenon include a faraday reaction mechanism, ohmic leakage, and a charge redistribution mechanism. [ Physical Chemistry Chemical Physics,2016,18: 661-. The charge redistribution mechanism mainly exists in a super capacitor taking porous carbon as an electrode material, the bent deep hole has diffusion resistance to electrolyte ions, and when the bent deep hole is used as the electrode material, the outer surface of the material has a higher charging speed than that in the hole. After charging, when the system is in an open circuit state, the electrode material may have electric potential distributed inwards along the pores, the redundant electric charge at the tips of the pores migrates to the depths of the pores, the electric potential of the electrode rapidly drops, and a very rapid self-discharge process of the device is initiated. [ Journal of Physical Chemistry C,2010,114:12030- & Journal of Power Sources,2014,245:822- & 829 ] so for activated carbon, the deeper pore and wider pore size distribution are not good for the uniform distribution of electrolyte ions, and self-discharge phenomenon caused by charge redistribution mechanism is very easy to occur.
In summary, on the premise of ensuring that the capacity and high power characteristics of the super capacitor are not lost, the ineffective specific surface area and the pore volume in the activated carbon are reduced to improve the density and the volume performance of the activated carbon, and the size and the distribution uniformity of the pore channels are regulated to relieve the self-discharge phenomenon, so that the method becomes an important direction for modifying the activated carbon material. In recent years, researchers prepare activated carbon with special morphology such as activated carbon nanospheres and activated carbon fibers by regulating and controlling preparation conditions of the activated carbon, and prepare composite gel by using graphene loaded activated carbon (Advanced Science,2019: 1802355) to achieve a densification effect, but the methods are complex in process, consume a lot of resources and are only limited to laboratory research. In addition, the research on the self-discharge phenomenon generated by the activated carbon electrode is mostly focused on the mechanism research, and the research on the effect of inhibiting the self-discharge through the modification of the electrode material is focused on the novel carbon material such as graphene and carbon nanotubes [ Nano Energy,2017, 31: 183- & Nano Energy,2014,4:14-22 ], and few studies on modification of activated carbon have been made. Therefore, an active carbon material modification mode which is simple in process, convenient to operate and easy to realize industrialization is urgently needed to be found, and the purposes of densification and self-discharge alleviation are achieved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention modifies the commercial activated carbon material by using a simple mechanical method on the premise of comprehensively considering commercial value and process means. The characteristics and the modification method of the active carbon are as follows:
the modified activated carbon material obtained by the invention has a blind hole rate not higher than 5%.
The further preferable scheme of the invention is as follows: the blind hole rate is not higher than 3%.
The further preferable scheme of the invention is as follows: the tap density of the modified activated carbon material is more than 0.6 g-cm-3。
The further preferable scheme of the invention is as follows: the modified activated carbon material has a conductivity greater than 130 S.m-1。
The method for modifying the activated carbon material comprises the following steps: taking active carbon with the grain diameter of 5-200 mu m as a starting material to carry out mechanical densification treatment under the oxygen-free condition.
The further preferable scheme of the invention is as follows: the activated carbon material is selected from commercial activated carbon, coal-based activated carbon and bamboo charcoal-based activated carbon.
The further preferable scheme of the invention is as follows: the mechanical densification treatment mode is one or more of ball milling, crushing and grinding.
The further preferable scheme of the invention is as follows: the processing rotating speed of the mechanical densification treatment is 200-.
The further preferable scheme of the invention is as follows: the treatment rotating speed is 500-6000 r/min, and the treatment time is 8-24 hours.
In addition, the invention also provides application of the modified activated carbon material as an electrode material of a super capacitor.
The regulation and control of physicochemical properties such as particle size, pore structure, composition and the like of the activated carbon material can be realized by utilizing the action effects such as friction, extrusion, impact and the like generated in the mechanical process. The modified activated carbon material is an irregular block assembled by particles with widened particle size distribution and reduced porosity compared with the raw material, microscopic pores of the material are exposed or damaged, the density is obviously improved, and the modified activated carbon material can be fully infiltrated by electrolyte when used as a super capacitor electrode material. The specific change process of the material in the mechanical treatment process is as follows: (1) after being crushed by mechanical force, the active carbon particles are firstly crushed, the average particle size is reduced, and meanwhile, a large number of branch-shaped pore channels, blind holes, closed holes and other structures in the active carbon are exposed, so that the pore volume and the specific surface area of the material are increased; in addition, the reduction of the particle size also greatly reduces the stacking gaps among the particles, and the density of the activated carbon is improved to a certain degree; (2) along with the extension of the mechanical densification treatment time, a part of crushed activated carbon particles are reassembled due to the increase of the surface energy, and are aggregated and accumulated to form a part of larger blocks, so that the particle size distribution of the material is widened, meanwhile, a part of pore channels are damaged or buried, and the pore volume and the specific surface area are reduced; the widening of the particle size distribution can enable smaller particles to be filled in the stacking gaps of larger particles, the contact among the particles is tighter, and the density is further improved.
The activated carbon after mechanical modification can be used as a high-density electrode material of a super capacitor. The acting forces such as compaction, friction and the like in the mechanical densification treatment process are reducedThe void and blind hole rate among the activated carbon particles is regulated, the physical and chemical properties such as the specific surface area, the pore volume and the like are regulated, the effective void utilization rate is improved, the mass specific capacity is improved, the density of the activated carbon material is obviously improved, and the volume performance is improved; the order degree of the carbon layer can be improved under high-energy mechanical force and high-temperature environment in the action process, and a graphite microcrystalline structure is introduced into the amorphous carbon through a micro-region graphitization effect, so that the conductivity of the activated carbon material is greatly improved, the multiplying power performance of the activated carbon material is improved, the electric double layer capacitance of the activated carbon material is increased, and the mass specific capacity of the material is effectively improved; the pore channel structure is recombined by utilizing mechanical force, the tortuosity of the pore channel structure is reduced, a charge transmission path is shortened, the electrolyte infiltration is effectively promoted, and meanwhile, electrolyte ions can be uniformly distributed in an electrode material body phase, so that the self-discharge phenomenon is greatly inhibited. Tests show that when the activated carbon is used as a supercapacitor electrode material, the activated carbon subjected to mechanical dense modification is 1A g-1The mass specific capacity under the current density can be improved by 35 percent at most, the volume specific capacity can be improved by 330 percent at most, and the multiplying power performance and the cycling stability are excellent. In addition, the time for the self-discharge process to reduce the voltage to half of the initial voltage can be prolonged by 300% at most, and the voltage decay can be reduced by 20% at most after 48 hours. Therefore, the invention also provides application of the modified activated carbon prepared by the method as an electrode material of a super capacitor.
The invention utilizes the high-energy mechanical force generated in the processes of ball milling, crushing, grinding and the like to modify and prepare the high-density active carbon electrode material. The mechanical processes have low process cost, simple operation and no subsequent treatment steps, can effectively improve the material preparation efficiency, and the prepared material has stable performance and is easy to realize large-scale industrial production.
Drawings
FIG. 1 is a graph showing the particle size distribution of S1 and the change in density of S1 over different milling times.
FIG. 2 is a plot of the mass and volume specific capacity rates of S1 and S1-12.
FIG. 3 is a self-discharge curve of S1 and S1-12.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, but the present invention is not limited to the following examples.
Example 1
A commercial activated carbon S1 was placed in a ball mill and ball milled for 12 hours at a constant rotation speed of 500 rpm under an argon atmosphere to obtain a high-density activated carbon material (S1-12).
As shown in the particle size distribution diagram of figure 1, the average particle size after ball milling is reduced from 16.9 μm to 11.5 μm; the tap density of the active carbon is measured to be 0.37g cm-3Increased to 0.73g cm-3The yield is improved by 97%; the nitrogen adsorption and desorption test result shows that the specific surface area and the pore volume are 1673m2g-1And 0.8cm3g-1Down to 302m2g-1And 0.3cm3g-1. The blind hole rate is reduced from 15.6% to 3.7%. Conductivity of 57S m-1Is improved to 138S m-1。
As shown in the electrochemical performance test result of the super capacitor in the attached figure 2, the electrochemical performance test result is shown at 1A g-1Under the current density, the mass specific capacity and the volume specific capacity of S1 are 179F g respectively-1And 66F cm-3The specific mass capacity and the specific volume capacity of S1-12 are 187F g respectively-1And 137F cm-3. The mass specific capacity is improved by 108 percent while the volume specific capacity is improved; at 10A g-1The specific mass capacities of S1 and S1-12 at current density were 171F g-1And 177F g-1The volume specific capacity is 63F cm-3And 129F cm-3The improvement is 104%.
As shown in the self-discharge test result of the super capacitor in the attached figure 3, the initial voltage is 3.5V, and the time for reducing the voltage of S1 and S1-12 to half of the initial voltage in the open circuit state is 5.4 hours and 22.4 hours respectively, which is prolonged by 310%; after 48 hours of standing the voltage decayed to 1.18 and 1.42V, respectively, with a 20% reduction.
Example 2
A commercial activated carbon S2 was placed in a ball mill and ball milled for 8 hours at a constant rotation speed of 500 rpm under a nitrogen atmosphere to obtain a high-density activated carbon material (S2-8).
The tap density is measured to be 0.41g cm-3Increased to 0.81g cm-3And the yield is improved by 98 percent. The specific surface area is 1294m2g-1Is reduced to 582m2g-1. The blind hole rate is reduced from 18.9% to 4.2%. The conductivity is 87S m-1Is improved to 164S m-1. The electrochemical test results showed that the electrochemical test was at 1A g-1Under the current density, the S2-8 specific mass capacity is improved by 12 percent compared with the S2, and meanwhile, the specific volume capacity is improved by 238 percent; at 10A g-1Under the current density, the volume specific capacity is improved by 204 percent.
The self-discharge test result of the super capacitor shows that the initial voltage is 3.5V, and the time for reducing the voltage of S2 and S2-8 to half of the initial voltage is 6.5 hours and 13 hours respectively under the open circuit state, so that the voltage is prolonged by 100 percent; after 48 hours of standing the voltage decayed to 1.21 and 1.32V, respectively, with a 9% reduction.
Example 3
A commercial activated carbon S2 was put into a pulverizer and pulverized at a constant rotation speed of 2800 rpm for 16 hours under a vacuum atmosphere to obtain a high-density activated carbon material (S2-16).
The tap density of S2-16 was measured to be 1.02g cm-3The specific surface area is 822m2g-1. The blind porosity was 3.2%. Conductivity of 57S m-1Is improved to 280S m-1. The electrochemical test results showed that the electrochemical test was at 1A g-1Under the current density, the mass specific capacity of S2-16 is improved by 15% compared with that of S2, and meanwhile, the volume specific capacity is improved by 248%; at 10A g-1Under the current density, the volume specific capacity is improved by 243%. The self-discharge test result shows that the time for reducing the S2-16 voltage to half of the initial voltage is respectively 13 hours, and the time is prolonged by 140 percent; after standing for 48 hours, the voltage decayed to 1.44V, which decreased by 20%.
Example 4
A commercial activated carbon S2 was put into a grinder and ground for 10 hours at a constant rotation speed of 3000 rpm under an argon atmosphere to obtain a high-density activated carbon material (S2-10).
The tap density of S2-10 was measured to be 0.92g cm-3Specific surface area of 860m2g-1. The blind porosity was 2.7%. Conductivity of 57S m-1Is improved to 206S m-1. Electrochemical testingThe results showed 1A g-1Under the current density, the mass specific capacity of S2-10 is improved by 13% compared with that of S2, and the volume specific capacity is improved by 192%; at 10A g-1Under the current density, the volume specific capacity is improved by 201 percent. The self-discharge test result shows that the time for reducing the voltage to half of the initial voltage is prolonged by 170 percent; after 48 hours of standing the voltage decay decreased by 17%.
Example 5
The activated carbon S3 prepared by laboratory activation is put into a wall breaking machine and treated for 5 hours at the constant rotating speed of 20000 revolutions per minute under the nitrogen atmosphere, and the high-density activated carbon material (S3-5) is obtained.
The tap density of S3 before and after treatment is measured to be 0.38g cm-3Increased to 0.62g cm-3Specific surface area is 1072m2g-1Increased to 1550m2g-1. The blind hole rate is reduced from 21.6% to 4.7%. Conductivity number 62S m-1Is raised to 126S m-1. The electrochemical test results showed that the electrochemical test was at 1A g-1Under the current density, the mass specific capacity of S3-1 is improved by 13% compared with that of S3, and meanwhile, the volume specific capacity is improved by 112%; at 10A g-1Under the current density, the volume specific capacity is improved by 118 percent. The self-discharge test result shows that the time for reducing the voltage to half of the initial voltage is prolonged by 30 percent; after 48 hours of standing the voltage decay decreased by 2%.
Example 6
The activated carbon S3 prepared by laboratory activation is put into a ball mill to be ball-milled for 48 hours under the nitrogen atmosphere at a constant rotating speed of 200 r/min, and a high-density activated carbon material (S3-48) is obtained.
The tap density of S3-48 was measured to be 0.71g cm-3. The blind porosity was 2.3%. The conductivity was 216S m-1. The electrochemical test result shows that the silver-ion-doped silver-ion alloy is 1Ag-1Under the current density, the mass specific capacity of S3-48 is improved by 23% compared with that of S3, and the volume specific capacity is improved by 330%; at 10A g-1Under the current density, the volume specific capacity is improved by 328 percent. The self-discharge test result shows that the time for reducing the voltage to half of the initial voltage is prolonged by 230 percent; after 48 hours of standing the voltage decay decreased by 18%.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A modified activated carbon material characterized by having a blind via rate of not greater than 5%.
2. The modified activated carbon material of claim 1, wherein the blind porosity is not greater than 3%.
3. The modified activated carbon material of claim 1, wherein the modified activated carbon material has a tap density greater than 0.6 g-cm-3。
4. A modified activated carbon material of claim 1, wherein the modified activated carbon material has an electrical conductivity greater than 130S-m-1。
5. A method of preparing a modified activated carbon material according to any one of claims 1 to 4, characterized in that: taking active carbon with the grain diameter of 5-200 mu m as a starting material to carry out mechanical densification treatment under the oxygen-free condition.
6. A method of preparing the modified activated carbon material of claim 5, wherein the activated carbon material is selected from the group consisting of commercial activated carbon, coal-based activated carbon and bamboo charcoal-based activated carbon.
7. The method for preparing a modified activated carbon material according to claim 5, wherein the mechanical densification treatment is selected from one or more of ball milling, pulverizing and grinding.
8. The method for preparing modified activated carbon material according to claim 5, wherein the treatment rotation speed of the mechanical densification treatment is 200-.
9. The method for preparing modified activated carbon material as claimed in claim 8, wherein the processing rotation speed is 500-6000 rpm, and the processing time is 8-24 hours.
10. Use of a modified activated carbon material according to any one of claims 1 to 4 for the preparation of electrodes and supercapacitors thereof.
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| CN113402905A (en) * | 2021-06-28 | 2021-09-17 | 青岛黑猫新材料研究院有限公司 | High-porosity carbon black, preparation method and preparation device thereof |
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