CN108910880A - Porous laminated absorbent charcoal material and preparation method thereof for supercapacitor - Google Patents
Porous laminated absorbent charcoal material and preparation method thereof for supercapacitor Download PDFInfo
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- CN108910880A CN108910880A CN201810800422.5A CN201810800422A CN108910880A CN 108910880 A CN108910880 A CN 108910880A CN 201810800422 A CN201810800422 A CN 201810800422A CN 108910880 A CN108910880 A CN 108910880A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title description 20
- 239000002250 absorbent Substances 0.000 title description 12
- 230000002745 absorbent Effects 0.000 title description 12
- 239000003610 charcoal Substances 0.000 title description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 235000014676 Phragmites communis Nutrition 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 239000007772 electrode material Substances 0.000 claims abstract description 37
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000003763 carbonization Methods 0.000 abstract description 10
- 239000007864 aqueous solution Substances 0.000 abstract description 8
- 239000000243 solution Substances 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 4
- 241000446313 Lamella Species 0.000 abstract description 3
- 239000012190 activator Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 66
- 239000010410 layer Substances 0.000 description 14
- 238000001994 activation Methods 0.000 description 11
- 230000004913 activation Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000003575 carbonaceous material Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002028 Biomass Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005255 carburizing Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- -1 when carbonization Substances 0.000 description 1
Classifications
-
- 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, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The porous laminated active carbon electrode material and preparation method thereof that the invention discloses a kind of for supercapacitor, pretreated reed film is placed in KOH solution and carries out hydro-thermal reaction, it is freeze-dried after filtering, then it is carbonized in nitrogen atmosphere, last cleaned, dry, grinding, obtains the porous laminated active carbon electrode material for supercapacitor.Present invention KOH aqueous solution hydro-thermal process reed film; enter KOH smooth mass transfer in reed film and is evenly distributed on its piece interlayer; when carbonization; KOH, which can not only be used for built-in template, prevents lamella accumulation but also as the uniform opening hole of activator; preparation process of the present invention is simple and environmentally-friendly, easy to operate, is of great significance to the production cost and protection environment that reduce active carbon.
Description
Technical field
The present invention relates to electrode material for super capacitor technical fields, and in particular to a kind of for the porous of supercapacitor
Layer-like active carbon electrode material and preparation method.
Background technique
Efficient energy storage and transformation technology are that the challenge of facing mankind is also opportunity.In all advanced energy storages
In technology, electrochemical storage device, including supercapacitor and rechargeable battery are two kinds of most promising energy storage devices.It is super
Capacitor, power density, longer cycle life and preferable stability with higher, make its portable electronic device,
The fields such as hybrid vehicle and energy resource system have potential application prospect, therefore by the concern of researcher.
Porous carbon material is applied to double because having many advantages, such as biggish specific surface area, preferable electric conductivity and stability
Electric layer capacitor electrode material.But porous carbon material bulk density is smaller, causes volumetric capacitance performance general, limits it
Application.In recent years, since layer structure material active surface abundant and open inter-layer passages enable electrolyte ion
Enough quick insertion/diffusions, meanwhile, the bulk effect of electrode material can be alleviated in charge and discharge process sandwich, significantly mentioned
The charge-discharge performance of high electrode material, thus by strong concern.Although stratified material has many advantages, such as, actually answering
The disadvantages of there are layer heaps to fold in, reunion leads to problems such as its active area reduce, the extension of ion diffusion path, to influence
Its capacitive property.Therefore, the advantages of how making full use of porous structure and layer structure, improves its energy-storage property to greatest extent,
It is the Important Problems studied at present.
Summary of the invention
The object of the present invention is to provide a kind of for the porous laminated active carbon electrode material of supercapacitor and preparation side
Method.
Realizing the technical solution of the object of the invention is：Porous laminated active carbon electrode material for supercapacitor
And preparation method thereof, the reed film of natural layer structure is placed in KOH aqueous solution and carries out hydro-thermal reaction, is freezed after filtering dry
It is dry, it is then carbonized in nitrogen atmosphere, last cleaned, dry, grinding is obtained for the porous laminated of supercapacitor
Active carbon electrode material, specific step is as follows：
1）The pretreatment of reed film：Reed film surface impurity is cleaned with deionized water, crushed after being dried is stand-by；
2）The potassium hydroxide aqueous solution for configuring 0.2~1.5 mol/L, it is water-soluble to be added to potassium hydroxide for the reed film crushed in right amount
In liquid, moved into hydrothermal reaction kettle after stirring submergence；
3）Reaction kettle is put into baking oven, 5~10 h of hydro-thermal reaction at 120~180 DEG C, naturally cool to filtering after room temperature,
Freeze-drying, obtains mixture；
4）Mixture is placed in crucible, tube furnace is moved under nitrogen atmosphere, is warming up to the heating rate of 1~5 DEG C/min
500~800 DEG C, constant temperature 2~4 h of carbonization obtain carbonized product；
5）Carbonized product obtained first is washed with dilute hydrochloric acid, then being washed with deionized water to filtrate is neutrality, grinds, obtains after dry
The porous laminated active carbon electrode material of supercapacitor.
Further, 15 ~ 20 grams of smashed reed films are put into 1L potassium hydroxide aqueous solution.
Further, hydro-thermal reaction of the present invention, be in 0.2~1.5 mol/LKOH aqueous solution, with 120~
180 DEG C of 5~10 h of target temperature hydro-thermal reaction.It is proved through repetition test, if KOH concentration is lower than 0.2 mol/L, subsequent activation
Pore-creating is ineffective；And when being higher than 1.5 mol/L, between reed film layer, area load KOH reaches saturation, does not have to subsequent activation effect
It is obviously improved.Suitable target temperature and reaction time, be conducive to KOH and be uniformly distributed between reed film layer, while playing just
The purpose of step carbonization presoma, to obtain the better active carbon of performance and higher yield.
When the carbonization, 500~800 DEG C are warming up to the heating rate of 1~5 DEG C/min, carries out 2~4 h of constant temperature carbonization.
If carburizing temperature is lower than 500 DEG C, the carbonization of reed film is not thorough, impurity content is high and pore-creating effect is unobvious；And it is higher than 800 DEG C,
Reed membrane stratiform structure is seriously damaged, and ultimate output and material property can decline, and energy consumption is high.Therefore, suitable to rise
Warm rate and constant temperature time, are conducive to uniform activation, and the original stratiform of reed film can be effectively protected in stable activation process
Structure.
After the present invention uses KOH aqueous solution hydro-thermal reaction, since the amount of reed film absorption KOH is less, filtered filtrate
Still KOH concentration with higher, so can be used as activator recycling.
The product obtained after carbonization is first cleaned with dilute hydrochloric acid, then is washed with deionized water to neutrality, is then dried, most
Grind into powder can be used as electrode active material afterwards.It is cleaned with dilute hydrochloric acid and can remove the carbon being present in activation products hole
The activation products such as sour potassium, potassium oxide keep the hole of active carbon exposed, so that active carbon has flourishing specific surface area, mention
Its high capacitive property.
Compared with prior art, the beneficial effects of the present invention are：
1）Hydro-thermal process reed film is conducive to KOH mass transfer and enters piece interlayer, reduces KOH dosage, improves activation efficiency, and KOH water
Solution is Ke Xunhuanliyong.
2）Less KOH dosage and lower carburizing temperature retain the hetero atoms such as O, N in reed film, are conducive to
Preparation is rich in the active carbon of O, N functional group, and the wetability that can not only improve Carbon Materials can also provide additional fake capacitance, to mention
The capacitive property of high activity Carbon Materials.
3）Reed film is abundance, renewable, environmental-friendly as biomass, passes through simple, green treatment process
It can be prepared by porous laminated absorbent charcoal material, be used as electrode material has preferable capacitive property in supercapacitor.
4）Preparation process of the present invention is simple and environmentally-friendly, easy to operate, has to the production cost and protection environment that reduce active carbon
Significance.
Detailed description of the invention
Fig. 1 is that the SEM of 1 reed film of embodiment schemes.
Fig. 2 is the SEM figure of porous laminated active carbon prepared by embodiment 1.
Fig. 3 is the SEM figure of porous activated carbon prepared by embodiment 2.
Fig. 4 is the DFT graph of pore diameter distribution of the absorbent charcoal material of Examples 1 and 2 preparation.
Fig. 5 is the XPS analysis N 1s electron spectrum fitted figure of porous laminated active carbon prepared by embodiment 1.
Fig. 6 is the XPS analysis O 1s electron spectrum fitted figure of porous laminated active carbon prepared by embodiment 1.
Fig. 7 is the cyclic voltammetry curve figure of porous laminated active carbon electrode material prepared by embodiment 1.
Fig. 8 is the cycle charge-discharge curve graph of porous laminated active carbon electrode material prepared by embodiment 1.
Fig. 9 is the specific capacitance of the activated carbon electrodes of Examples 1 and 2 preparation with the variation diagram of current density.
Figure 10 is the specific capacitance of the activated carbon electrodes of Examples 1 and 2 preparation with the variation diagram of cycle-index.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments to the present invention
It is described in detail.
Present invention KOH aqueous solution hydro-thermal process reed film, makes the smooth mass transfer of KOH enter in reed film and be evenly distributed on
Its piece interlayer, when carbonization, KOH, which can not only be used for built-in template, prevents lamella accumulation but also as the uniform opening hole of activator.Use with
High specific surface area porous layer-like active Carbon Materials are made as presoma in the reed film of natural layer structure.Reed film belongs to can
Renewable biomass realizes reed film high-efficiency resource recycling.KOH aqueous solution can be recycled in preparation process, is carbonized and lives
Change process is combined into step progress, and the preparation process that low temperature lacks alkali is small to equipment corrosion, has environment friendly.Therefore, to raising
Performance of the supercapacitor and reduction Activated Carbon Production cost are of great significance.
（One）Preparation process：
Embodiment 1：
1）The pretreatment of reed film：Reed film surface impurity is cleaned with deionized water, crushed after being dried is stand-by.By Fig. 1 as it can be seen that reed
Apparent lamellar structure is presented in reed film and surface is more coarse.
2）It weighs 0.78g potassium hydroxide and is dissolved in the lye for forming 0.2 mol/L in 70 ml deionized waters.Weigh 1g crushing
Reed film be added in lye, stirring submergence after move into 100ml hydrothermal reaction kettle in.
3）Reaction kettle is put into baking oven, 5 h of hydro-thermal reaction at 130 DEG C, it is dry to naturally cool to filtering after room temperature, freezing
It is dry, obtain mixture.
4）Mixture is placed in nickel crucible, moves into tube furnace under nitrogen atmosphere, is heated up with the heating rate of 2 DEG C/min
To 650 DEG C, constant temperature carbonization 2h obtains activation products.
5）Activation products obtained first are washed with 0.1mol/L dilute hydrochloric acid, then being washed with deionized water to the pH value of filtrate is 6
~7, it is ground after dry, obtains supercapacitor with porous laminated active carbon electrode material.
The SEM figure of the above porous laminated absorbent charcoal material is as shown in figure 3, reed film after hydro-thermal-carbonization treatment, forms hole
The porous active Carbon Materials that road is interconnected, lamella is accumulated.
Fig. 5 is the electron spectrum fitted figure of the XPS analysis N1s of porous laminated absorbent charcoal material prepared by embodiment 1.By scheming
5 is visible：N 1s spectral peak is divided into four peaks, illustrates absorbent charcoal material surface nitrogen-containing functional group rich in, their surface
Activity can provide fake capacitance abundant, to enhance the capacitive property of absorbent charcoal material.
Fig. 6 is the electron spectrum fitted figure of the XPS analysis O1s of porous active Carbon Materials prepared by embodiment 1.It can by Fig. 6
See：O 1s spectral peak is divided into three peaks, illustrates absorbent charcoal material surface oxygen-containing functional group rich in, can effectively enhance
The wetability of material is to improve capacitive property.
Embodiment 2：
1）The pretreatment of reed film：Reed film surface impurity is cleaned with deionized water, crushed after being dried is stand-by.
2）The reed film for weighing 1g crushing is added in 70ml deionized water, moves into 100ml hydro-thermal reaction after stirring submergence
In kettle.
3）Reaction kettle is put into baking oven, 5 h of hydro-thermal reaction at 130 DEG C, it is dry to naturally cool to filtering after room temperature, freezing
It is dry, obtained product is uniformly mixed with 2g potassium hydroxide.
4）Mixture is placed in nickel crucible, moves into tube furnace under nitrogen atmosphere, is heated up with the heating rate of 2 DEG C/min
To 650 DEG C, constant temperature activates 2h, obtains activation products.
5）Activation products obtained first are washed with 0.1mol/L dilute hydrochloric acid, then being washed with deionized water to the pH value of filtrate is 6
~7, it is ground after dry, obtains porous active carbon electrode material.
The SEM of the above porous active carbon electrode material schemes as shown in figure 3, reed film forms a large amount of hole after KOH is activated,
But whole irregularly bulk, the lamellar structure of presenting is seriously damaged.
Fig. 4 is the DFT graph of pore diameter distribution of porous carbon material prepared by embodiment 1 and 2.As seen from Figure 4：Embodiment 1 is made
The central hole structure that the porous laminated absorbent charcoal material obtained can not only have micropore abundant also flourishing, and it is more made from embodiment 2
Porous materials are mainly based on micropore.
（Two）Using：
Above two porous active carbon electrode materials obtained are taken to carry out parallel test respectively：
Porous active carbon electrode material, conductive agent and binder are prepared by mixing into electrode slice with 85: 10: 5 mass ratio,
Three-electrode system electrochemical property test is carried out in 6mol/L KOH electrolyte.
Fig. 7 is the cyclic voltammetry curve figure of porous laminated active carbon electrode material prepared by embodiment 1.
As seen from Figure 7：The cyclic voltammetry curve of institute's sample shows class rectangle, illustrates the capacitor of sample mainly by double electricity
Layer capacitance provides.Significantly deforming does not occur in cyclic voltammetry curve in the case where sweeping speed greatly, and illustrates that electrode material has preferable electricity
Capacitive can be with rapid electric charge memory mechanism.
Fig. 8 is the constant current charge-discharge curve graph of porous laminated active carbon electrode material prepared by embodiment 1.
As seen from Figure 8：The constant current charge-discharge curve of institute's sample shows slight deformation under different current densities
Isosceles triangle, illustrate electrode material have good electric double layer capacitance characteristic, because of the redox reaction of surface functional group
Slight deformation is generated, illustrates that obtained active carbon has preferable capacitive property and high rate performance.
Fig. 9 is the specific capacitance of the active carbon electrode material of Examples 1 and 2 preparation with the variation diagram of current density.
As seen from Figure 9：The specific capacitance of electrode material prepared by embodiment 1 is apparently higher than the specific capacitance value of embodiment 2, and works as
When current density increases to 10 A/g from 0.5 A/g, the capacity retention of embodiment 1 is also higher, illustrates layer structure to capacitor
The promotion effect of performance is obvious.
Figure 10 is the specific capacitance of the active carbon electrode material of Examples 1 and 2 preparation with the variation diagram of cycle-index.
As seen from Figure 10：Embodiment 1 prepare electrode material it is more stable in cyclic process and circulation 5000 times after still have
Higher capacity retention illustrates it with outstanding cyclical stability.
The electrode slice formed with porous laminated active carbon electrode material made from 1 method of example follows under speed in sweeping for 100 mV/s
Ring volt-ampere curve still shows preferable rectangular configuration, and when current density is 0.5 A/g, specific capacitance reaches 353 F/g；Electric current
When density is 2 A/g, capacity retention ratio reaches 96.4% after 5000 charge and discharge cycles.
The electrode slice formed with porous active carbon electrode material made from 2 method of example specific capacitance in current density 0.5A/g
Reach 269 F/g；When current density is 2 A/g, capacity retention ratio reaches 91.0% after 5000 charge and discharge cycles.
The pore structure analysis result of the resulting porous active carbon electrode material of both examples above is listed in the following table.
| Embodiment sample | BET specific surface area (m2·g-1) | Micropore specific area (m2·g-1) | Middle pore specific surface area (m2·g-1) | Total hole volume (cm3·g-1) | Micropore volume （cm3·g-1） | Middle pore volume （cm3·g-1） | Average pore size （nm） |
| Example 1 | 1289 | 790 | 473 | 1.02 | 0.82 | 0.20 | 1.41 |
| Example 2 | 1067 | 823 | 231 | 0.64 | 0.59 | 0.05 | 1.08 |
As seen from the above table：Although the less KOH of example 1, obtained absorbent charcoal material ratio still with higher
Surface area, reasonable pore-size distribution can increase the contact area between electrode and electrolyte liquor as electrode material, promote electrolyte
Ion quickly transmits, to improve the capacitive property of material.
Porous laminated absorbent charcoal material can be prepared using natural layer biomass as presoma, this material have both it is porous and
The problem of the advantages of layer structure, very good solution porous material density is small and stratified material stacks, reunites, will be outstanding
Electrode material for electric double layer capacitor.Use reed film for the porous laminated carbon resistance rod of the high-performance of precursor preparation supercapacitor
Material can make full use of reed film, and reed film belongs to renewable biomass, and economic benefit and social benefit are very huge
Greatly.
Claims (9)
1. the preparation method of porous laminated active carbon electrode material, which is characterized in that it is molten that pretreated reed film is placed in KOH
Carry out hydro-thermal reaction in liquid, be freeze-dried after filtering, be then carbonized in nitrogen atmosphere, it is last it is cleaned, dry, grind
Mill, obtains the porous laminated active carbon electrode material for supercapacitor.
2. preparation method as described in claim 1, which is characterized in that the pretreatment of reed film includes that cleaning reed film surface is miscellaneous
Matter, crushed after being dried step.
3. preparation method as described in claim 1, which is characterized in that the concentration of KOH solution is 0.2~1.5 mol/L.
4. preparation method as described in claim 1, which is characterized in that be put into 1LKOH solution 15 ~ 20 grams it is pretreated
Reed film.
5. preparation method as described in claim 1, which is characterized in that hydrothermal temperature is 120~180 DEG C, hydro-thermal reaction
Time is 5~10 h.
6. preparation method as described in claim 1, which is characterized in that be warming up to 500~800 DEG C of constant temperature carbon in nitrogen atmosphere
Change 2~4 h.
7. preparation method as described in claim 1, which is characterized in that when being carbonized in nitrogen atmosphere, heating rate 1
~5 DEG C/min.
8. the porous laminated active carbon electrode material of method preparation as claimed in claim 1.
9. the porous laminated active carbon electrode material of method preparation as claimed in claim 1 is in supercapacitor
Using.
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| CN201810800422.5A CN108910880A (en) | 2018-07-20 | 2018-07-20 | Porous laminated absorbent charcoal material and preparation method thereof for supercapacitor |
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| CN201810800422.5A Pending CN108910880A (en) | 2018-07-20 | 2018-07-20 | Porous laminated absorbent charcoal material and preparation method thereof for supercapacitor |
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| CN110060881A (en) * | 2019-04-28 | 2019-07-26 | 常州大学 | A kind of preparation method of water system high capacity electrode material for super capacitor |
| CN110803699A (en) * | 2019-11-08 | 2020-02-18 | 江苏科技大学 | Composite carbon material for seawater desalination and preparation method thereof |
| CN111137886A (en) * | 2019-11-19 | 2020-05-12 | 南京工程学院 | Method for preparing electrode material by aquatic plant |
| CN112886026A (en) * | 2021-01-11 | 2021-06-01 | 扬州工业职业技术学院 | Reed flower biochar-based electrode material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110060881A (en) * | 2019-04-28 | 2019-07-26 | 常州大学 | A kind of preparation method of water system high capacity electrode material for super capacitor |
| CN110803699A (en) * | 2019-11-08 | 2020-02-18 | 江苏科技大学 | Composite carbon material for seawater desalination and preparation method thereof |
| CN111137886A (en) * | 2019-11-19 | 2020-05-12 | 南京工程学院 | Method for preparing electrode material by aquatic plant |
| CN112886026A (en) * | 2021-01-11 | 2021-06-01 | 扬州工业职业技术学院 | Reed flower biochar-based electrode material and preparation method thereof |
| CN112886026B (en) * | 2021-01-11 | 2022-03-25 | 扬州工业职业技术学院 | Reed flower biochar-based electrode material and preparation method thereof |
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