CN101702379A - Method for preparing non-symmetrical electrochemical supercapacitor and electrode materials - Google Patents

Method for preparing non-symmetrical electrochemical supercapacitor and electrode materials Download PDF

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Publication number
CN101702379A
CN101702379A CN200910226430A CN200910226430A CN101702379A CN 101702379 A CN101702379 A CN 101702379A CN 200910226430 A CN200910226430 A CN 200910226430A CN 200910226430 A CN200910226430 A CN 200910226430A CN 101702379 A CN101702379 A CN 101702379A
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preparation
active carbon
activated carbon
acid
inert gas
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CN101702379B (en
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崔光磊
韩鹏献
王海波
陈骁
刘志宏
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Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
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Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
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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
    • 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
    • H01G11/54—Electrolytes
    • H01G11/58—Liquid electrolytes
    • 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)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The invention relates to a method for preparing a non-symmetrical electrochemical supercapacitor and electrode materials, and the method comprises the steps of crushing petroleum coke, drying, mixing with an activator according to the proportion, heating, activating, cooling, then using hydrochloric acid for washing, and further using deionized water for washing prepared activated carbon till neutral; carrying out high-temperature graphitization on the obtained activated carbon; and adopting the activated carbon and the graphitized activated carbon for producing a positive electrode and a negative electrode respectively, and finally assembling the non-symmetrical electrochemical supercapacitor. The method can improve the working voltage by 1.1V and improve the specific energy by 8.2 times in comparison with the method of assembling an electric double-layer capacitor by adopting the pure activated carbon, and be used for producing the electrochemical supercapacitor with high specific energy, high power and long service life.

Description

The preparation method of a kind of asymmetric electric chemical super capacitor and electrode material
Technical field
The invention belongs to material science and electrochemical techniques scientific domain, be specifically related to a kind of preparation method of electrode material of asymmetric electric chemical super capacitor.
The invention still further relates to the method for preparing asymmetric electric chemical super capacitor with above-mentioned electrode material.
Background technology
Electrochemical capacitor is a kind of novel, efficient, practical electrochemical energy storage device, have high power density, high-energy-density, have extended cycle life, advantage such as pollution-free, be widely used in modern high-tech field such as electric/hybrid vehicle, mobile energy storage device, industrial power management and hybrid power system.
Electric chemical super capacitor can be divided into according to energy storage mechanism difference:
(1) double electric layer capacitor, the generation of its electric capacity are mainly based on separation of charge produced on electrode, the electrolyte electric double layer capacitance;
(2) electric chemical super capacitor, it is made up of noble metal and metal oxide containing precious metals electrode, the generation of its electric capacity is based on electroactive ion at precious metal surface generation underpotential deposition, or the redox reaction that takes place in mutually at metal oxide containing precious metals electrode surface and body and the adsorption capacitance that produces, but, limited its commercial application because the noble metal price is extremely expensive.
It is electrode material that traditional double electric layer capacitor both positive and negative polarity all adopts active carbon, and in organic electrolyte system, voltage limit is about 1-2.7V, and stored charge is limited in one's ability, as patent CN1646423A, CN1810637A etc.
Summary of the invention
The object of the present invention is to provide a kind of electrode material preparation method who is used for asymmetric electric chemical super capacitor.
Another purpose of the present invention is to provide a kind of method of using the asymmetric electric chemical super capacitor of electrode material preparation.
For achieving the above object, the electrode preparation method of asymmetric electric chemical super capacitor provided by the invention, key step is:
1) with petroleum coke fragmentation (be preferably and be crushed to 100 orders), oven dry;
2) activator is soluble in water, obtain petroleum coke particles 1-5 by weight with step 1: 1 mixed, dipping;
3) with the macerate of step 2 under inert gas shielding, be warming up to 600-1000 ℃ by the heating rate of 1-10 ℃/min and activate, the cooling back is washed with water to neutrality with watery hydrochloric acid (5wt%) washing, drying, ball milling makes active carbon;
4) active carbon of step 3 is placed under 1600-3000 ℃ in high temperature graphitization stove, the inert gas shielding carry out graphitization, obtain graphited active carbon electrode material.
Among the described preparation method, activator is one or more mixtures in potassium hydroxide, NaOH, zinc chloride, calcium chloride, potash, phosphoric acid, potassium dihydrogen phosphate, potassium sulfide, sulfuric acid, the boric acid.
Among the described preparation method, the inert gas in the step 3 is nitrogen or argon gas, and the inert gas in the step 4 is an argon gas.
Among the described preparation method, the water in step 2 and the step 3 is meant deionized water.
The method of utilizing above-mentioned electrode material to prepare asymmetric electric chemical super capacitor provided by the invention, key step is:
A) positive pole of absorbent charcoal material preparation:
Active carbon with claim 1 step 3: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, be coated on the aluminium foil, and oven dry, anode pole piece is made in compacting;
B) negative pole of graphited absorbent charcoal material preparation:
Graphited absorbent charcoal material with claim 1 step 4: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, be coated on the Copper Foil, and oven dry, cathode pole piece is made in compacting;
C) separate with barrier film in the middle of the cathode pole piece among the anode pole piece of steps A and the step B, inject organic system electrolyte and be assembled into the buckle type electrochemical ultracapacitor.
Described conductive agent can be carbon black, graphite, graphitized carbon fibre etc.; Binding agent can be Kynoar PVDF, polytetrafluoroethylene PTFE, carboxylic styrene butadiene latex SBR, sodium carboxymethylcellulose CMC etc.
Described barrier film can be individual layer PE (polyethylene), individual layer PP (polypropylene), three layers of PP/PE/PP composite membrane etc.
In the described organic system electrolyte, the electrolyte cation can be tetraethyl ammonium root (C 2H 5) 4N 4 +, TBuA root (C 4H 9) 4N +, Li +, anion can be hexafluoro-phosphate radical PF 6 -, tetrafluoroborate BF 4 -, trifluoromethanesulfonic acid root CF 3SO 3 -, perchlorate ClO 4 -Deng, organic solvent can be dimethyl carbonate (DMC), diethyl carbonate (DEC), ethylene carbonate (EC), propene carbonate (PC), methyl ethyl carbonate alkene ester (CMC), carbonic acid first propyl ester (MPC), 1,2-dimethoxy-ethane (DME), 1,4-butyrolactone (GBL) etc.
Asymmetric electric chemical super capacitor of the present invention, because graphited active carbon electrode material has the crystallinity height, shows well-behaved characteristics, the active carbon of asymmetric electric chemical super capacitor positive pole relies on the adsorption charge storage power, and the graphited active carbon of negative pole relies on ion to embed storage power, operating voltage under the common double electric layer capacitor organic system is improved 3.8V from 2.7V, it is low to have overcome common double electric layer capacitor operating voltage, thereby causes the low shortcoming of energy density.
Embodiment
One of technical solution provided by the invention is, the preparation method of described graphited active carbon electrode material, and concrete steps are:
1) with the petroleum coke fragmentation, 100 mesh sieves are crossed in the oven dry back;
2) activator is dissolved in the deionized water, obtain petroleum coke particles 1-5 by weight with step 1: 1 ratio is evenly mixed, and floods 8-24 hour (h);
3) mixture in the step 2 is placed the charing boat, be placed in the activation furnace, under inert gas shielding, being warming up to 600-1000 ℃ by the heating rate of 1-10 ℃/min activates, after the cooling active carbon that obtains is used the salt acid elution of 5wt% earlier, extremely neutral with deionized water wash afterwards, drying, ball milling 5-24h;
4) active carbon that step 3 is obtained places under 1600-3000 ℃ in high temperature graphitization stove, the inert gas shielding and carries out graphitization, obtains graphited active carbon electrode material.
Activator of the present invention can be for potassium hydroxide, NaOH, zinc chloride, calcium chloride, potash, phosphoric acid, potassium dihydrogen phosphate, potassium sulfide, sulfuric acid, boric acid is a kind of or two or more mixtures wherein.
The inert gas of charing of the present invention can be nitrogen, argon gas etc., and graphited inert gas is an argon gas.
The manufacture method of asymmetric electrochemical capacitor of the present invention, concrete steps are:
A) positive pole of absorbent charcoal material preparation:
With the resulting active carbon of step 3: conductive agent: binding agent is by weight 100: the mixed of 5-10: 5-10 is even, it is coated on the aluminium foil, and oven dry, compacting is washed into disk shape pole piece;
B) negative pole of graphited absorbent charcoal material preparation:
With the resulting graphited absorbent charcoal material of step 4: conductive agent: binding agent is by weight 100: the mixed of 5-10: 5-10 is even, it is coated on the Copper Foil, and oven dry, compacting is washed into disk shape pole piece;
C) electrode with steps A is anodal, and the electrode among the step B is a negative pole, and the centre separates with barrier film, injects organic system electrolyte and is assembled into asymmetric capacitor.
Conductive agent of the present invention can be carbon black, graphite, graphitized carbon fibre etc.; Binding agent can be Kynoar PVDF, polytetrafluoroethylene PTFE, carboxylic styrene butadiene latex SBR, sodium carboxymethylcellulose CMC etc.
The barrier film that the present invention adopts can be individual layer PE, individual layer PP, three layers of PP/PE/PP composite membrane etc.
In the organic system electrolyte of the present invention: the electrolyte cation can be tetraethyl ammonium root (C 2H 5) 4N 4 +, TBuA root (C 4H 9) 4N +, Li +, anion can be hexafluoro-phosphate radical PF 6 -, tetrafluoroborate BF 4 -, trifluoromethanesulfonic acid root CF 3SO 3 -, perchlorate ClO 4 -Deng, organic solvent can be dimethyl carbonate (DMC), diethyl carbonate (DEC), ethylene carbonate (EC), propene carbonate (PC), methyl ethyl carbonate alkene ester (CMC), carbonic acid first propyl ester (MPC), 1,2-dimethoxy-ethane (DME), 1,4-butyrolactone (GBL) etc.
Graphited active carbon electrode material provided by the invention and asymmetric electrochemical capacitor thereof, cheap and easy to get, the environmental friendliness of material, its operating voltage has improved 1.1V than common double electric layer capacitor, the specific energy height, its 8.2 times more than especially, but and adopting the electrochemical capacitor long service life fast charging and discharging of this material preparation, security performance is good.
Further set forth the present invention with embodiment below, but the present invention is not so limited.
Embodiment 1
With commercially available petroleum coke fragmentation, 100 mesh sieves are crossed in the oven dry back; With 20g activator NaOH deionized water dissolving, join and contain in the 5g petroleum coke powder stainless steel activation boat, mix, behind the dipping 24h, place the tubular type activation furnace, under nitrogen protection, with the heating rate of 5 ℃/min, be warming up to 800 ℃ of heat treatment 3h, reduce to room temperature afterwards naturally; The active carbon that obtains is used 5wt% salt acid elution earlier, use the deionized water cyclic washing again to neutral.Get the above-mentioned active carbon 2g that obtains in graphite crucible, be placed on the following 2000 ℃ of constant temperature 2h of argon shield in the graphitizing furnace, reduce to room temperature then and get material.
With the above-mentioned active carbon that obtains and graphited active carbon respectively with conductive black, PVDF binding agent mixed by weight 85: 10: 5, be coated in respectively on aluminium foil and the Copper Foil, be washed into pole piece, the aluminium foil that is coated with active carbon is as positive pole, the Copper Foil that scribbles graphited active carbon is as negative pole, separate with the barrier film polyethylene between the positive and negative electrode pole piece, inject 1mol/L LiPF 6/ (EC: DMC) electrolyte is assembled into asymmetric electric chemical super capacitor, charging/discharging voltage: 2-3.8V, current density is: 0.5A/g.Test result sees Table 1.
Embodiment 2
Make the graphitization temperature among the embodiment 1 into 1800 ℃, other conditions are identical with embodiment 1, and test result sees Table 1.
Embodiment 3
Make the graphitization temperature among the embodiment 1 into 2800 ℃, other conditions are identical with embodiment 1, and test result sees Table 1.
Comparative example 1
According to the method for embodiment 1, be that active carbon is coated on the aluminium foil with obtaining among the embodiment 1, electrolyte adopts 1mol/L LiPF 6/ PC is assembled into the symmetric form double electric layer capacitor, charging/discharging voltage: 0-2.7V, and other conditions are identical with embodiment 1, and test result sees Table 1.
Table 1: embodiment and comparative example
Embodiment Electrolyte Charging/discharging voltage (V) Than electric capacity (F/g) Specific energy (Wh/kg) Specific energy improves multiple (comparing with comparative example 1)
?1 ??LiPF 6/EC∶DMC) ??2～3.8 ??78.2 ??42.58 ??8.2
?2 The same ??2～3.8 ??70.5 ??38.37 ??7.4
?3 The same ??2～3.8 ??54.7 ??29.78 ??5.7
Comparative example 1 ??Et 4NBF 4/PC ??0～2.7 ??86 ??5.2 ??-

Claims (9)

1. electrode material preparation method who is used for asymmetric electric chemical super capacitor, key step is:
1) with the petroleum coke fragmentation, oven dry;
2) activator is soluble in water, obtain petroleum coke particles 1-5 by weight with step 1: 1 mixed, dipping;
3) with the macerate of step 2 under inert gas shielding, be warming up to 600-1000 ℃ by the heating rate of 1-10 ℃/min and activate, the cooling back is washed with water to neutrality with the watery hydrochloric acid washing, drying, ball milling makes active carbon;
4) active carbon of step 3 is placed under 1600-3000 ℃ in high temperature graphitization stove, the inert gas shielding carry out graphitization, obtain graphited active carbon electrode material.
2. preparation method according to claim 1, wherein, the activator in the step 2 is one or more mixtures in potassium hydroxide, NaOH, zinc chloride, calcium chloride, potash, phosphoric acid, potassium dihydrogen phosphate, potassium sulfide, sulfuric acid, the boric acid.
3. preparation method according to claim 1, wherein, the inert gas in the step 3 is nitrogen or argon gas, the inert gas in the step 4 is an argon gas.
4. preparation method according to claim 1, wherein, the watery hydrochloric acid in the step 3 is the aqueous hydrochloric acid solution of 5wt%.
5. preparation method according to claim 1, wherein, the water in step 2 and the step 3 is meant deionized water.
6. method of utilizing the described electrode material of claim 1 to prepare asymmetric electric chemical super capacitor, key step is:
A) positive pole of absorbent charcoal material preparation:
With claim 1 step 3 preparation active carbon: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, be coated on the aluminium foil, oven dry, anode pole piece is made in compacting;
B) negative pole of graphited absorbent charcoal material preparation:
Graphited absorbent charcoal material with the preparation of claim 1 step 4: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, be coated on the Copper Foil, and oven dry, cathode pole piece is made in compacting;
C) separate with barrier film in the middle of the cathode pole piece among the anode pole piece of steps A and the step B, inject organic system electrolyte and be assembled into the buckle type electrochemical ultracapacitor.
7. preparation method according to claim 6, wherein, the conductive agent among steps A and the step B is carbon black, graphite or graphitized carbon fibre; Binding agent is Kynoar, polytetrafluoroethylene, carboxylic styrene butadiene latex or sodium carboxymethylcellulose.
8. preparation method according to claim 6, wherein, the barrier film among the step C is monolayer polyethylene, single-layer polypropylene or three-layer polypropylene/polyethylene/polypropylene composite membrane.
9. preparation method according to claim 6, wherein, in the organic system electrolyte among the step C, the electrolyte cation is tetraethyl ammonium root, TBuA root or Li +Anion is hexafluoro-phosphate radical, tetrafluoroborate, trifluoromethanesulfonic acid root or perchlorate; Organic solvent is dimethyl carbonate, diethyl carbonate, ethylene carbonate, propene carbonate, methyl ethyl carbonate alkene ester, carbonic acid first propyl ester, 1,2-dimethoxy-ethane or 1,4-butyrolactone.
CN200910226430A 2009-11-20 2009-11-20 Method for preparing non-symmetrical electrochemical supercapacitor and electrode materials Active CN101702379B (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
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CN102013336A (en) * 2010-09-16 2011-04-13 南京双登科技发展研究院有限公司 Asymmetrical super capacitor
CN102627279A (en) * 2012-03-29 2012-08-08 南京正森环保科技有限公司 Method for preparing smoke mercury-removing activated carbon
CN103280334A (en) * 2013-04-03 2013-09-04 王子齐 General power high energy storage multi-medium capacitor-battery container
CN103882559A (en) * 2014-03-13 2014-06-25 中国科学院化学研究所 High-specific surface porous carbon fiber, preparation method and application of carbon fiber
US8848339B2 (en) 2011-12-15 2014-09-30 Industrial Technology Research Institute Capacitor and manufacturing method thereof
CN104715934A (en) * 2013-12-16 2015-06-17 中国科学院兰州化学物理研究所 Hybrid super capacitor and manufacturing method thereof
CN105016337A (en) * 2014-04-17 2015-11-04 中国科学院上海硅酸盐研究所 Active carbon material used for supercapacitor electrodes and preparation method thereof
US9611392B2 (en) 2011-12-15 2017-04-04 Industrial Technology Research Institute Self-assembly coating material, heat sink and method of forming heat sink
CN106744945A (en) * 2016-11-16 2017-05-31 北京方大炭素科技有限公司 A kind of method for improving electric conductivity with activated carbon based on purifying petroleum coke based super capacitor
CN111977653A (en) * 2020-08-24 2020-11-24 中国林业科学研究院林产化学工业研究所 Modified activated carbon for super capacitor and preparation method thereof
US11961668B2 (en) 2022-04-13 2024-04-16 Imam Abdulrahman Bin Faisal University Vanadium doped cobalt nickel spinel ferrite-based nanocomposite electrodes

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CN101239718A (en) * 2002-07-30 2008-08-13 可乐丽化学株式会社 Activated carbon, method for production thereof, polarized electrode and electrical double layer capacitor
KR101149966B1 (en) * 2004-12-27 2012-06-01 파나소닉 주식회사 Polarizable electrode member, process for producing the same, and electrochemical capacitor utilizing the member
JP4989114B2 (en) * 2006-06-02 2012-08-01 日本カーボン株式会社 Negative electrode and negative electrode active material for lithium secondary battery

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102013336A (en) * 2010-09-16 2011-04-13 南京双登科技发展研究院有限公司 Asymmetrical super capacitor
US9611392B2 (en) 2011-12-15 2017-04-04 Industrial Technology Research Institute Self-assembly coating material, heat sink and method of forming heat sink
US8848339B2 (en) 2011-12-15 2014-09-30 Industrial Technology Research Institute Capacitor and manufacturing method thereof
CN102627279A (en) * 2012-03-29 2012-08-08 南京正森环保科技有限公司 Method for preparing smoke mercury-removing activated carbon
CN103280334A (en) * 2013-04-03 2013-09-04 王子齐 General power high energy storage multi-medium capacitor-battery container
CN103280334B (en) * 2013-04-03 2016-08-24 王子齐 General power high energy storage multi-medium capacitor-battery container
CN104715934A (en) * 2013-12-16 2015-06-17 中国科学院兰州化学物理研究所 Hybrid super capacitor and manufacturing method thereof
CN103882559A (en) * 2014-03-13 2014-06-25 中国科学院化学研究所 High-specific surface porous carbon fiber, preparation method and application of carbon fiber
CN105016337A (en) * 2014-04-17 2015-11-04 中国科学院上海硅酸盐研究所 Active carbon material used for supercapacitor electrodes and preparation method thereof
CN105016337B (en) * 2014-04-17 2018-10-02 中国科学院上海硅酸盐研究所 A kind of absorbent charcoal material and preparation method thereof can be used for electrode of super capacitor
CN106744945A (en) * 2016-11-16 2017-05-31 北京方大炭素科技有限公司 A kind of method for improving electric conductivity with activated carbon based on purifying petroleum coke based super capacitor
CN111977653A (en) * 2020-08-24 2020-11-24 中国林业科学研究院林产化学工业研究所 Modified activated carbon for super capacitor and preparation method thereof
CN111977653B (en) * 2020-08-24 2023-06-02 中国林业科学研究院林产化学工业研究所 Modified activated carbon for super capacitor and preparation method thereof
US11961668B2 (en) 2022-04-13 2024-04-16 Imam Abdulrahman Bin Faisal University Vanadium doped cobalt nickel spinel ferrite-based nanocomposite electrodes

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