CN101728085B - Carbon composite metal nitride electrode material and asymmetric electrochemical super capacitor - Google Patents
Carbon composite metal nitride electrode material and asymmetric electrochemical super capacitor Download PDFInfo
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- CN101728085B CN101728085B CN2010101040031A CN201010104003A CN101728085B CN 101728085 B CN101728085 B CN 101728085B CN 2010101040031 A CN2010101040031 A CN 2010101040031A CN 201010104003 A CN201010104003 A CN 201010104003A CN 101728085 B CN101728085 B CN 101728085B
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Abstract
The invention discloses a carbon composite metal nitride electrode material with the chemical formula of MeN/C, wherein Me is one or a mixture of titanium, vanadium, chromium, iron, manganese, magnesium and molybdenum organic compounds; N and C are respectively nitrogen and carbon; the weight ratio of metal to carbon nitride is from 1: 1 to 3: 1. The electrode material is obtained by the method as follows: dissolving the metal organic compound or the mixture of the compounds; adding to mesoporous graphite phase carbon nitride; decompressing for removing air in holes after ultrasonic oscillation; filtering and washing by using ethanol; drying; and treating at high temperature under the protection of inert gas to prepare the electrode material. When the electrode material is used as an electrode of an asymmetric electrochemical super capacitor in electrolyte of an organic system, the working voltage is 4V and the highest specific energy can reach 70.04Wh/kg. The electrode material of the electrochemical super capacitor has excellent performance.
Description
Technical field
The present invention relates to a kind of high-energy-density carbon composite metal nitride electrode material.
The invention still further relates to the application of above-mentioned carbon composite metal nitride electrode material in the asymmetric electric chemical super capacitor of preparation.
Background technology
Along with The development in society and economy, people more and more pay close attention to for green energy resource and biological environment, electric chemical super capacitor is with plurality of advantages such as its high power capacity, high power, long-life, with low cost, safety and environmental protections, become the best novel environment friendly accumulator of market prospects in this century, can be widely used in fields such as information, electronics, the energy, environment, traffic and military projects, in today that energy-conserving and environment-protective become to be the theme day by day, its application more and more causes the attention of countries in the world.
Developed countries is paid much attention to the electric chemical super capacitor research and development, its target is the electrode material of preparation high working voltage, high-energy-density and/or height ratio capacity rate, and then preparation super high power, ultra-high capacity can be used for the large-scale ultracapacitor of power purposes.The carbon back electric chemical super capacitor that with the active carbon is representative has been realized commercialization at home and abroad, but still has monomer operating voltage low (about 1-2.7V), the low shortcomings such as (2-5Wh/kg) of energy density, has limited its application in the high-end field.
In order to improve the ratio electric capacity of raw material of wood-charcoal material, Chinese patent CN101221854A, CN1402272, CN1404082A etc. adopt activated carbon supported MxOy (M represents Ni, Co, Mn, Al, Zn etc.) and Chinese patent CN1482634 load Pb compound, but these materials all are used in the aqueous electrolysis liquid system, and energy density is low.
Summary of the invention
The object of the present invention is to provide a kind of high-energy-density carbon composite metal nitride electrode material.
Another purpose of the present invention is to use above-mentioned carbon composite metal nitride electrode material and prepares asymmetric electric chemical super capacitor.
For achieving the above object, the carbon composite metal nitride electrode material that is used for asymmetric electric chemical super capacitor provided by the invention, chemical general formula is MeN/C, wherein Me is a metallo-organic compound, be one or more mixtures in titanium, vanadium, chromium, iron, manganese, magnesium, the molybdenum organic compound, N, C are respectively nitrogen and carbon, and the weight ratio of metal and carbonitride is 1: 1-3: 1, obtain by following preparation process:
1) one or more metallo-organic compounds is dissolved in the ethanol;
2) add mesoporous carbonitride in step 1 solution, reduced pressure treatment after the vibration makes that air fully discharges in the hole;
3) mixture in the step 2 is carried out suction filtration, drying;
4) mixture that obtains of step 3 is warming up to 600-1000 ℃ and handled 3-10 hour under inert gas shielding, lowers the temperature naturally, obtains the electrode material of carbon composite metal nitride;
Wherein, step 2 is to handle with sonic oscillation.
Wherein, step 4 is to heat up with 1-10 ℃ of/minute clock rate.
The method of utilizing above-mentioned electrode material to prepare asymmetric electric chemical super capacitor provided by the invention, key step is:
1) positive pole of absorbent charcoal material preparation
With commercially available active carbon: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, and it is coated on the aluminium foil, and the oven dry compacting is washed into disk shape pole piece;
2) negative pole of carbon composite metal nitride material preparation
With the carbon composite metal nitride material: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, and is coated on the Copper Foil, and the oven dry compacting is washed into disk shape pole piece;
3) pole piece of step 1 preparation is anodal, and the pole piece of step 2 preparation is a negative pole, and the centre separates with barrier film, injects organic system electrolyte and is assembled into the buckle type electrochemical ultracapacitor.
Wherein, conductive agent is carbon black, graphite or graphitized carbon fibre.
Wherein, binding agent is Kynoar, polytetrafluoroethylene, carboxylic styrene butadiene latex or sodium carboxymethylcellulose.
Wherein, barrier film is single-layer polypropylene, monolayer polyethylene or multilaminar polyethylene/polypropylene, polyethylene composite membrane.
Wherein, in the organic system electrolyte: the electrolyte cation is Li
+Or K
+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.
Carbon composite metal nitride electrode material of the present invention, its composition promptly has good electron conductivity, also show excellent capacitive properties, when being used for the negative pole of asymmetric electric chemical super capacitor, rely on ion to embed storage power, and the anode activated charcoal material is with its high-specific surface area adsorption charge storage power, operating voltage under the common double electric layer capacitor organic system is brought up to 4V from 2.7V, it is low to have overcome common double electric layer capacitor operating voltage, thereby causes the low shortcoming of energy density.
Description of drawings
Fig. 1 is the X-ray diffractogram of carbon composite metal nitride electrode material of the present invention.
Fig. 2 a is the transmission electron microscope figure of the carbon composite metal nitride electrode material of embodiment 1 preparation.
Fig. 2 b is the electron diffraction diagram of the carbon composite metal nitride electrode material of embodiment 1 preparation.
Fig. 2 c is the transmission electron microscope figure of the carbon composite nitride titanium combination electrode material of comparative example 1 preparation.
Fig. 2 d is the electron diffraction diagram of the carbon composite nitride titanium combination electrode material of comparative example 1 preparation.
Embodiment:
Technical scheme of the present invention is that the high-energy-density carbon composite metal nitride electrode material can obtain by following preparation method:
1) one or more metallo-organic compounds is dissolved in the ethanol, is mixed with the solution of certain molar concentration;
2) in step 1 solution, add mesoporous carbonitride (G-C in proportion
3N
4), reduced pressure treatment behind the sonic oscillation 5-30min makes that air fully discharges in the hole;
3) mixture in the step 2 is carried out suction filtration, drip ethanol simultaneously, carry out drying afterwards;
4) with the mix powder that obtains in the step 3, under inert gas shielding, be warming up to 600-1000 ℃ of heat treatment 3-10h with the speed of 1-10 ℃/min, cooling naturally obtains the electrode material of carbon composite metal nitride.
Described high-energy-density carbon composite metal nitride electrode material preparation method, metallo-organic compound can be one or more mixtures in the compound of titanium, vanadium, chromium, iron, manganese, magnesium, molybdenum etc.
The present invention utilizes above-mentioned electrode material to prepare the method for asymmetric electrochemical capacitor, and concrete steps are:
1) positive pole of absorbent charcoal material preparation: with active carbon (commercial goods): conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, it is coated on the aluminium foil, and oven dry, compacting is washed into disk shape pole piece;
2) negative pole of carbon composite metal nitride material preparation: change the absorbent charcoal material in the step 1 into the carbon composite metal nitride material, be coated on the Copper Foil, all the other are identical with step 1;
3) adopt the electrode in step 1 and the step 2 to do positive and negative electrode respectively, separate with barrier film between the both positive and negative polarity, 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 monolayer polyethylene (PE), single-layer polypropylene (PP), three layers of PP/PE/PP composite membrane etc.
In the described organic system electrolyte: the electrolyte cation can be Li
+, K
+Deng, 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.
High-energy-density carbon composite metal nitride electrode material provided by the invention and asymmetric electric chemical super capacitor thereof, cheap and easy to get, the environmental friendliness of material, the monomer operating voltage reaches 4V, specific energy reaches as high as 70.04Wh/kg, it is a kind of electric chemical super capacitor electrode material of excellent performance, 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.
With 228mg Ti (OC
2H
5)
4With 606mg VO (OC
2H
5)
3Be dissolved in the 2g ethanol, to wherein adding the mesoporous carbonitride (G-C of 0.5g
3N
4), this mixture sonic oscillation is handled 10min, the air in the hole is removed in decompression afterwards; Carry out suction filtration then, dropwise drip 2ml ethanol simultaneously and wash; After the drying, be warming up to 800 ℃ with 3 ℃/min under nitrogen protection, lower the temperature naturally behind the heat treatment 3h, obtain the electrode material Ti-V-N/C of carbon composite nitride titanium vanadium, its composition sees Table 1.
With commercial goods active carbon and the above-mentioned combination electrode material that obtains respectively with conductive black, PVDF binding agent mixed by 85: 10: 5, be coated in respectively on aluminium foil and the Copper Foil, be washed into pole piece, respectively as anodal, negative pole, adopt 1mol/L LiPF
6/ (EC:DMC) be electrolyte, be assembled into asymmetric electric chemical super capacitor, charging/discharging voltage: 2-4V, current density is that the test result of 74.4mA/g and 22.32A/g sees Table 2.
Embodiment 2
With the Ti (OC among the embodiment 1
2H
5)
4And VO (OC
2H
5)
3Quality change into 85mg and 749mg respectively, all the other are identical with embodiment 1, the composition of combination electrode material and asymmetric electric chemical super capacitor test result thereof see Table 1 and table 2 respectively.
Embodiment 3
With the Ti (OC among the embodiment 1
2H
5)
4And VO (OC
2H
5)
3Quality change into 360mg and 474mg respectively, all the other are identical with embodiment 1, the composition of combination electrode material and asymmetric electric chemical super capacitor test result thereof see Table 1 and table 2 respectively.
Embodiment 4
With the Ti (OC among the embodiment 1
2H
5)
4And VO (OC
2H
5)
3Quality change into 643mg and 191mg respectively, all the other are identical with embodiment 1, the composition of combination electrode material and asymmetric electric chemical super capacitor test result thereof see Table 1 and table 2 respectively.
Figure 1 shows that the X-ray diffractogram of the carbon composite metal nitride electrode material that embodiment 1 to embodiment 4 prepares; Wherein curve a, b, c, d represent embodiment 1,2,3,4 respectively.
Comparative example 1
Ti (OC with 834mg
2H
5)
4Be dissolved in the 2g ethanol, all the other are identical with embodiment 1, prepare carbon composite nitride titanium combination electrode material TiN/C, and the composition of combination electrode material and asymmetric electric chemical super capacitor test result thereof see Table 1 and table 2 respectively.
The electrode material for preparing respectively about embodiment 1 and comparative example 1 can be consulted shown in Figure 2, and Fig. 2 a is the transmission electron microscope figure of the carbon composite metal nitride electrode material of embodiment 1 preparation, and Fig. 2 b is the electron diffraction diagram of embodiment 1; Fig. 2 c is the transmission electron microscope figure of the carbon composite nitride titanium combination electrode material of comparative example 1 preparation, and Fig. 2 d is the electron diffraction diagram of comparative example 1.
Comparative example 2
VO (OC with 834mg
2H
5)
3Be dissolved in the 2g ethanol, all the other are identical with embodiment 1, prepare carbon composite nitride titanium combination electrode material TiN/C, and the composition of combination electrode material and asymmetric electric chemical super capacitor test result thereof see Table 1 and table 2 respectively.
Comparative example 3
Commercially available active carbon is assembled into the double electric layer capacitor that both positive and negative polarity is absorbent charcoal material according to the method for embodiment 1, and electrolyte is Et
4NBF
4/ PC, charging/discharging voltage is: 0-2.7V, test result sees Table 2.
Table 1: the mol ratio of presoma in the composition of carbon composite nitride titanium vanadium electrode material and the original solution
Table 2: embodiment and comparative example test result
| Sequence number | Electrolyte | 74.4mA/g the time based on the ratio electric capacity (F/g) of the two poles of the earth active material | 22.32A/g the time based on the ratio electric capacity (F/g) of the two poles of the earth active material | Specific energy during current density 22.32A/g (Wh/kg) | Specific energy improves multiple (comparing with comparative example 1) |
| |
LiPF 6/ (EC:DMC) | 171.64 | 27.36 | 70.04 | 14.00 |
| Embodiment 2 | The same | 130.46 | 13.53 | 34.65 | 6.93 |
| Embodiment 3 | The same | 181.72 | 15.55 | 39.81 | 7.96 |
| Embodiment 4 | The same | 195.26 | 9.216 | 23.59 | 4.72 |
| Comparative example 1 | The same | 195.84 | 5.76 | 14.74 | 2.95 |
| Comparative example 2 | The same | 129.6 | 6.62 | 16.95 | 3.39 |
| Comparative example 3 | Et 4NBF 4/PC | 30.2 | 26.5 | 5.0 | - |
Claims (8)
1. carbon composite metal nitride electrode material that is used for asymmetric electric chemical super capacitor, chemical general formula is MeN/C, wherein Me is a metallo-organic compound, be one or more mixtures in titanium, vanadium, chromium, iron, manganese, magnesium, the molybdenum organic compound, N, C are respectively nitrogen and carbon, the weight ratio of metallo-organic compound and carbonitride is 1: 1-3: 1, obtain by following preparation process:
1) one or more metallo-organic compounds is dissolved in the ethanol;
2) add mesoporous carbonitride in step 1 solution, reduced pressure treatment after the vibration makes that air fully discharges in the hole;
3) mixture in the step 2 is carried out suction filtration, drying;
4) mixture that obtains of step 3 is warming up to 600-1000 ℃ and handled 3-10 hour under inert gas shielding, lowers the temperature naturally, obtains the electrode material of carbon composite metal nitride.
2. the carbon composite metal nitride electrode material that is used for asymmetric electric chemical super capacitor according to claim 1, wherein, step 2 is to handle with sonic oscillation.
3. the carbon composite metal nitride electrode material that is used for asymmetric electric chemical super capacitor according to claim 1, wherein, step 4 is to heat up with 1-10 ℃ of/minute clock rate.
4. method of utilizing the described electrode material of claim 1 to prepare asymmetric electric chemical super capacitor, key step is:
1) positive pole of absorbent charcoal material preparation
With active carbon: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, and it is coated on the aluminium foil, and the oven dry compacting is washed into disk shape pole piece;
2) negative pole of carbon composite metal nitride material preparation
With the carbon composite metal nitride material: conductive agent: binding agent is by weight 100: 5-10: 5-10 mixes, and is coated on the Copper Foil, and the oven dry compacting is washed into disk shape pole piece;
3) pole piece of step 1 preparation is anodal, and the pole piece of step 2 preparation is a negative pole, and the centre separates with barrier film, injects organic system electrolyte and is assembled into the buckle type electrochemical ultracapacitor.
5. method according to claim 4, wherein, conductive agent is carbon black, graphite or graphitized carbon fibre.
6. method according to claim 4, wherein, binding agent is Kynoar, polytetrafluoroethylene, carboxylic styrene butadiene latex or sodium carboxymethylcellulose.
7. method according to claim 4, wherein, barrier film is single-layer polypropylene, monolayer polyethylene or polyethylene/polypropylene/poly composite membrane.
8. method according to claim 4, wherein, in the organic system electrolyte: the electrolyte cation is Li+ or K+; 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.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102646839A (en) * | 2012-03-30 | 2012-08-22 | 中国科学院青岛生物能源与过程研究所 | Carbon material and carbon composite material used for air electrode of lithium air battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021662B (en) * | 2012-12-11 | 2015-06-24 | 常州大学 | Nanometer multilayer mesoporous metal nitride/graphene composite materials for super capacitor and preparation method thereof |
| CN103908977A (en) * | 2013-01-04 | 2014-07-09 | 安徽大学 | Preparation method and application of magnetic composite photocatalysis material based on graphite-phase carbon nitride |
| CN110060884A (en) * | 2019-03-30 | 2019-07-26 | 南京理工大学 | A kind of preparation method of the high-performance flexible carbon film electrodes material based on biological fiber fabric |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1402272A (en) * | 2002-08-19 | 2003-03-12 | 中国科学院山西煤炭化学研究所 | Method for increasing specific capacitance of active carbon electrode by carrying transition metal |
| CN1404082A (en) * | 2002-04-18 | 2003-03-19 | 江苏隆源双登电源有限公司 | Treatment process of active carbon for super capacitor |
| CN1482634A (en) * | 2002-09-11 | 2004-03-17 | 江苏隆源双登电源有限公司 | Modification method for cathode activated charcoal of ultracapacitor |
| CN101221854A (en) * | 2007-12-13 | 2008-07-16 | 同济大学 | Production method for active carbon electrode material of load transition metal and application thereof |
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2010
- 2010-01-26 CN CN2010101040031A patent/CN101728085B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1404082A (en) * | 2002-04-18 | 2003-03-19 | 江苏隆源双登电源有限公司 | Treatment process of active carbon for super capacitor |
| CN1402272A (en) * | 2002-08-19 | 2003-03-12 | 中国科学院山西煤炭化学研究所 | Method for increasing specific capacitance of active carbon electrode by carrying transition metal |
| CN1482634A (en) * | 2002-09-11 | 2004-03-17 | 江苏隆源双登电源有限公司 | Modification method for cathode activated charcoal of ultracapacitor |
| CN101221854A (en) * | 2007-12-13 | 2008-07-16 | 同济大学 | Production method for active carbon electrode material of load transition metal and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102646839A (en) * | 2012-03-30 | 2012-08-22 | 中国科学院青岛生物能源与过程研究所 | Carbon material and carbon composite material used for air electrode of lithium air battery |
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