CN101882479A - Electrode material of polyaniline-based nitrogen-containing carbon nano-tube super-capacitor, and preparation method thereof - Google Patents
Electrode material of polyaniline-based nitrogen-containing carbon nano-tube super-capacitor, and preparation method thereof Download PDFInfo
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- CN101882479A CN101882479A CN 201010196687 CN201010196687A CN101882479A CN 101882479 A CN101882479 A CN 101882479A CN 201010196687 CN201010196687 CN 201010196687 CN 201010196687 A CN201010196687 A CN 201010196687A CN 101882479 A CN101882479 A CN 101882479A
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- 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
The invention provides an electrode material of a super-capacitor, and a preparation method thereof. The invention adopts a polyaniline nano-tube prepared by a chemical oxidation method as precursor, and leads carbonization to be carried out at 600-1000 DEG C under the nitrogen atmosphere. The obtained polyaniline-based nitrogen-containing carbon nano-tube has a hollow structure with openings at the two ends, and has the length of 0.5-2mu m, the tube parameter of 100-170nm and the nitrogen content of 5-13%. The electrode material has the stable specific electric capacity reaching up to 163F/g under the current density of 0.1A/g; and the capacity retention rate is 83% when the current density is increased to be 1A/g from 0.1A/g. The electrode material has higher discharge specific capacity and good circulating stability.
Description
Technical field
The present invention relates to the electrode material for super capacitor field, particularly a kind of polyaniline-based nitrogen-containing carbon nano-tube electrode material and preparation method thereof.
Background technology
In the modern society of high speed development, along with the aggravation of environmental pollution, the exploitation of novel green energy-storage travelling wave tube is extremely urgent.Ultracapacitor is a kind of novel energy-storing element between traditional capacitor and battery, has up to 1～10Whkg
-1Energy density is bigger 10～100 times than traditional capacitor; Its power density can reach 2kWkg
-1About, be more than 10 times of conventional batteries.And cycle life (more than 100,000 times) [Elzbieta Frackowiak with good cycle efficieny and overlength, Francois Beguin.Carbon materials for the electrochemical storage of energy in capacitor.Carbon.2001,39,937-950.].
Material with carbon element as electrode material for super capacitor mainly contains active carbon, carbon nano-tube and charcoal-aero gel etc. at present.Though active carbon has very high specific area (2860m
2G
-1), but contain in a large number the micropore that can not be soaked into by electrolyte, and effective ratio area only has 22.7%, and specific capacity only is 130Fg
-1Carbon nano-tube has good electrical conductivity, and mesopore is distributed with the formation that is beneficial to electric double layer, and hole link, does not have blind hole, is beneficial to the electrolyte diffusion.But carbon nano-tube is because the smaller (100-400m of specific area
2G
-1), specific discharge capacity only is 40-80Fg
-1, and cost an arm and a leg; The charcoal-aero gel specific capacity is 110Fg
-1About, but manufacturing cycle is very long, and need factor such as supercritical drying to restrict its commercialization development [Elzbieta Frackowiak, Francois Beguin.Carbon materials for the electrochemical storage of energy in capacitors.Carbon, 2001,39:937-950].
Nitrogenous carbon nano-tube is one of focus of research at present as the electrode material of ultracapacitor.By nitrogen-atoms being introduced the graphite flake layer structure, destroy the regularity of material itself, the minimum energy level that occupies track and highest occupied molecular orbital of atom is changed, thereby the orbital energy level between the reduction atom, improve the ability that gives of material electronics, and then reach the effect that improves the material electric property.The researcher is many from carbon nano-tube at present, handle to make by potassium hydroxide activation and ammonification and insert nitrogen-atoms in the material or with carbon nano-tube with contain the material mixing high-temperature process of nitrogenous source, such as, earlier carbon nano-tube is soaked activation with potassium hydroxide solution, again sample high-temperature process under ammonia atmosphere is got final product nitrogenous carbon nano-tube [K.Jurewicz, K.Babel, R.Pietrzak, et al.Capacitance properties of multi-walled carbon nanotubes modified by activation and ammoxidation.Carbon, 2006,44:2368-2375.]; Perhaps melamine, formaldehyde and carbon nano-tube can be got nitrogenous carbon nano-tube [G.Lota through high-temperature process under inert atmosphere, K.Lota, E.Frackowiak.Nanotubes based composites rich in nitrogen for supercapacitor application.Electrochemistry Communication, 2007,9:1828-1832.].But this class methods complex manufacturing, production cost is higher, is unfavorable for realizing suitability for industrialized production.
Summary of the invention
At the problems referred to above, the purpose of this invention is to provide a kind of new electrode material for super capacitor---polyaniline-based nitrogen-containing carbon nano-tube.
For reaching the purpose that a kind of new electrode material for super capacitor is provided, the technical solution used in the present invention is: a kind of polyaniline-based nitrogen-containing carbon nano-tube, and it has the hollow structure of both ends open, length 0.5～2 μ m, caliber 100～170nm, nitrogen content 5～13%.
Another object of the present invention provides a kind of preparation method of polyaniline-based nitrogen-containing carbon nano-tube, makes by following method:
Step 1: prepared isopyknic aniline solution and ammonium persulfate solution in 1: 5～5: 5 by the mole concentration ratio, then two solution are mixed, react 12～36h under the room temperature, suction filtration afterwards, and be neutral with absolute ethyl alcohol and washed with de-ionized water to filtrate pH value with product, 50 ℃ of oven dry of vacuum obtain the polyaniline nano pipe;
Step 2: get step 1 gained polyaniline nano pipe, under nitrogen atmosphere, progressively be heated to 600～1000 ℃, be incubated 2～5 hours, obtain polyaniline-based nitrogen-containing carbon nano-tube.
The further preferred version of the present invention is: described aniline solution and ammonium persulfate solution are selected from a kind of in hydrochloric acid, sulfuric acid, phosphoric acid or the deionized water solution of 1mol/L.
Another purpose of the present invention provides a kind of electrode material for super capacitor of polyaniline-based nitrogen-containing carbon nano-tube preparation, is made up of by mass percentage following component: polyaniline-based nitrogen-containing carbon nano-tube 80%, acetylene black 10%, binding agent 10%.
The present invention adopts nitrogenous carbon nano-tube as electrode material for super capacitor.Inner hole link of nitrogenous carbon nano-tube and both ends open structure are beneficial to the diffusion and the infiltration of electrolyte, thereby improve its effective ratio area.Nitrogen-atoms is introduced in the regular carbon structure, can be introduced the redox fake capacitance on the basis of material with carbon element electric double layer capacitance, the double action of two kinds of electric capacity can effectively improve the ratio electric capacity of electrode material.Therefore nitrogenous carbon nano-tube is the electrode material of the good ultracapacitor of a kind of chemical property.
The present invention prepares the polyaniline nano pipe, just can obtain polyaniline-based nitrogen-containing carbon nano-tube through carbonization process again by chemical oxidization method.Technology is simple, the material preparation cost is low, easily realizes large-scale production.
The ultracapacitor specific discharge capacity that uses the polyaniline-based nitrogen-containing carbon nano-tube electrode material is at 133-167Fg
-1Between, far above the specific capacity (40-80Fg of carbon nano-tube
-1), when current density increased to 1A/g gradually from 0.1A/g, capability retention was 82%.Good power-performance and cycle performance have been showed.
Description of drawings
Accompanying drawing 1 is the sem photograph of gained polyaniline-based nitrogen-containing carbon nano-tube under 700 ℃ of carburizing temperatures.
Accompanying drawing 2 is the transmission electron microscope picture of gained polyaniline-based nitrogen-containing carbon nano-tube under 700 ℃ of carburizing temperatures.
Accompanying drawing 3 is respectively the nitrogen element content variation diagram of 600,700,850 ℃ and 1000 ℃ following gained polyaniline-based nitrogen-containing carbon nano-tubes for carburizing temperature.
Accompanying drawing 4 is respectively the specific discharge capacity of 600,700,850 and 1000 ℃ of following gained polyaniline-based nitrogen-containing carbon nano-tubes and the graph of relation of current density for carburizing temperature.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
Embodiment 1
Take by weighing 1.11g aniline and 3.4g ammonium persulfate and be dissolved in respectively in the 60ml deionized water, the preparation molar concentration rate is 4: 5 aniline solution and an ammonium persulfate solution, then ammonium persulfate solution is poured in the aniline solution into room temperature reaction 24h rapidly.It is neutral that the suction filtration products therefrom is cleaned to filtrate pH value with deionized water and ethanolic solution respectively, and 50 ℃ of oven dry of vacuum get the polyaniline nano pipe.
The polyaniline nano pipe as the precursor alumina crucible of packing into, is put into horizontal retort then, heat under nitrogen atmosphere, heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 700 ℃, be incubated 4 hours, and get polyaniline-based nitrogen-containing carbon nano-tube.
Take by weighing the 0.008g polyaniline-based nitrogen-containing carbon nano-tube at 8: 1: 1 by mass ratio, 0.001g acetylene black, 0.001g binding agent.Make electrode material after mixing.
Polyaniline-based nitrogen-containing carbon nano-tube length is 0.5～2 μ m shown in accompanying drawing 1 ESEM (SEM), caliber 100～170nm; The analysis showed that as accompanying drawing 2 transmission electron microscopes (TEM) polyaniline-based nitrogen-containing carbon nano-tube has the hollow open structure; The nitrogen content of the polyaniline-based nitrogen-containing carbon nano-tube that obtains of 700 ℃ of carbonization treatment is 10.88% as shown in Figure 3; 4 electrochemical property test results show that this electrode material is at 0.1Ag as accompanying drawing
-1Specific discharge capacity under the current density can reach 163Fg
-1At 1Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 133Fg
-1
Embodiment 2
The preparation method of polyaniline nano pipe is with embodiment 1, and different is to heat under the nitrogen atmosphere in retort, and heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 600 ℃, be incubated 5 hours, and get polyaniline-based nitrogen-containing carbon nano-tube.
The nitrogen content of the polyaniline-based nitrogen-containing carbon nano-tube that obtains of 600 ℃ of carbonization treatment is 13% as shown in Figure 3; 4 electrochemical property test results show that this electrode material is at 0.1Ag as accompanying drawing
-1Specific discharge capacity under the current density can reach 112Fg
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 52Fg
-1
Embodiment 3
The preparation method of polyaniline nano pipe is with embodiment 1, and different is to heat under the nitrogen atmosphere in retort, and heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 850 ℃, be incubated 3 hours, and obtain polyaniline-based nitrogen-containing carbon nano-tube.
The nitrogen content of the polyaniline-based nitrogen-containing carbon nano-tube that obtains of 850 ℃ of processing is 7.95% as shown in Figure 3; 4 electrochemical property test results show that the electrode material that utilizes this material preparation is at 0.1Ag as accompanying drawing
-1Specific discharge capacity under the current density can reach 110Fg
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 99.5Fg
-1
Embodiment 4
The preparation method of polyaniline nano pipe is with embodiment 1, and different is to heat under the nitrogen atmosphere in retort, and heating rate is 0.5 ℃ of min
-1, insulation 2h continues to be heated to 1000 ℃ in the time of 400 ℃, is incubated 2 hours, obtains polyaniline-based nitrogen-containing carbon nano-tube.
The nitrogen content of the polyaniline-based nitrogen-containing carbon nano-tube that obtains of 1000 ℃ of processing is 5% as shown in Figure 3; 4 electrochemical property test results show that this electrode material is at 0.1Ag as accompanying drawing
-1Specific discharge capacity under the current density can reach 89Fg
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 82.1Fg
-1
Embodiment 5
Take by weighing 0.28g aniline and 3.4g ammonium persulfate and be dissolved in the 1molL of 60ml respectively
-1In the hydrochloric acid solution, the preparation molar concentration rate is 1: 5 aniline solution and ammonium persulfate solution, at room temperature reacts 12h after mixing; It is neutral that the suction filtration products therefrom is cleaned to filtrate pH value with deionized water and ethanolic solution respectively, and 50 ℃ of oven dry of vacuum are ground, and obtain the polyaniline nano pipe.
With this polyaniline nano pipe, put into heating under the horizontal retort nitrogen atmosphere behind the crucible of packing into, heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 700 ℃, be incubated 4 hours, and get polyaniline-based nitrogen-containing carbon nano-tube.Obtain polyaniline-based nitrogen-containing carbon nano-tube.
Electrochemical property test is the result show, this electrode material shows good electrochemical, at 0.1Ag
-1Current density under specific discharge capacity can reach 109Fg
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 89.1Fg
-1
Take by weighing 0.83g aniline and 3.4g ammonium persulfate and be dissolved in the 1molL of 60ml respectively
-1In the sulfuric acid solution, the preparation molar concentration rate is 3: 5 aniline solutions and ammonium persulfate solution, at room temperature reacts 24h after mixing; It is neutral that the suction filtration products therefrom is cleaned to filtrate pH value with deionized water and ethanolic solution respectively, and 50 ℃ of oven dry of vacuum are ground, and obtain the polyaniline nano pipe.
With this polyaniline nano pipe, put into heating under the horizontal retort nitrogen atmosphere behind the crucible of packing into, heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 850 ℃, be incubated 3 hours, and get polyaniline-based nitrogen-containing carbon nano-tube.Obtain polyaniline-based nitrogen-containing carbon nano-tube.
Electrochemical property test is the result show, this electrode material shows good electrochemical, at 0.1Ag
-1Current density under specific discharge capacity can reach 120Fg
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 105Fg
-1
Embodiment 7
Take by weighing 1.388g aniline and 3.4g ammonium persulfate and be dissolved in the 1molL of 60ml respectively
-1In the phosphoric acid solution, the preparation molar concentration rate is 5: 5 aniline solutions and ammonium persulfate solution, mixes room temperature reaction 36h; It is neutral that the suction filtration products therefrom is cleaned to filtrate pH value with deionized water and ethanolic solution respectively, and 50 ℃ of oven dry of vacuum are ground, and obtain the polyaniline nano pipe.
With this polyaniline nano pipe, put into heating under the horizontal retort nitrogen atmosphere behind the crucible of packing into, heating rate is 0.5 ℃ of min
-1, when being warming up to 400 ℃, room temperature is incubated 2h, continue to be heated to 600 ℃, be incubated 5 hours, and get polyaniline-based nitrogen-containing carbon nano-tube.
Electrochemical property test is the result show, this electrode material is at 0.1Ag
-1Specific discharge capacity can reach 130Fg under the current density
-11Ag
-1Under the current density circulation 100 times after, specific discharge capacity can keep 112Fg
-1
Below preferred embodiment of the present invention is specified, but the present invention is not limited to described embodiment, those of ordinary skill in the art also can make all modification that is equal to or replacement under the prerequisite of spirit of the present invention, modification that these are equal to or replacement all are included in the application's claim institute restricted portion.
Claims (4)
1. a polyaniline-based nitrogen-containing carbon nano-tube is characterized in that described polyaniline-based nitrogen-containing carbon nano-tube has the hollow structure of both ends open, length 0.5～2 μ m, caliber 100～170nm, nitrogen content 5～13%.
2. method for preparing the described polyaniline-based nitrogen-containing carbon nano-tube of claim 1 is characterized in that making by following method:
Step 1: prepared isopyknic aniline solution and ammonium persulfate solution in 1: 5～5: 5 by the mole concentration ratio, then two solution are mixed, react 12～36h under the room temperature, suction filtration afterwards, and be neutral with absolute ethyl alcohol and washed with de-ionized water to filtrate pH value with product, 50 ℃ of oven dry of vacuum obtain the polyaniline nano pipe;
Step 2: get step 1 gained polyaniline nano pipe, under nitrogen atmosphere, progressively be heated to 600～1000 ℃, be incubated 2～5 hours, obtain polyaniline-based nitrogen-containing carbon nano-tube.
3. as preparing the method for polyaniline-based nitrogen-containing carbon nano-tube as described in the claim 2, it is characterized in that: described aniline solution and ammonium persulfate solution are selected from a kind of in hydrochloric acid, sulfuric acid, phosphoric acid or the deionized water solution of 1mol/L.
4. an electrode material for super capacitor that uses the described polyaniline-based nitrogen-containing carbon nano-tube preparation of claim 1 is characterized in that: be made up of by mass percentage following component: polyaniline-based nitrogen-containing carbon nano-tube 80%, acetylene black 10%, binding agent 10%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708436A (en) * | 2013-12-17 | 2014-04-09 | 北京化工大学 | Nitrogen-containing carbon nanotube with high heat resistance and preparation method of carbon nanotube |
| CN104743543A (en) * | 2015-03-04 | 2015-07-01 | 同济大学 | Method for preparing polyaniline/phenolic aldehyde based carbon material |
| CN105314614A (en) * | 2014-06-04 | 2016-02-10 | 北京化工大学 | Nitrogen-doped porous carbon nanotube material and its preparation method and use in super capacitor electrode |
| CN105355934A (en) * | 2015-10-31 | 2016-02-24 | 哈尔滨工业大学 | Preparation method of nitrogen-doped carbon nanotubes |
| CN105460917A (en) * | 2015-12-08 | 2016-04-06 | 武汉理工大学 | Nitrogen-doped carbon nanotube adopting hierarchical structure and preparation method |
| CN107055511A (en) * | 2017-04-13 | 2017-08-18 | 常州纳欧新材料科技有限公司 | A kind of three-dimensional cross-linked CNT and preparation method thereof |
| CN109110744A (en) * | 2018-08-30 | 2019-01-01 | 浙江工业大学 | A kind of preparation method of hollow tubular polyaniline carbon material |
| CN111606405A (en) * | 2020-06-03 | 2020-09-01 | 北京林业大学 | Method for degrading organic pollutants in water by activating peracetic acid through nitrogen-doped carbon material |
| CN113186565A (en) * | 2021-04-14 | 2021-07-30 | 天津大学 | Preparation method of novel nitrogen-doped carbon material for electrocatalytic reduction of carbon dioxide |
-
2010
- 2010-06-10 CN CN 201010196687 patent/CN101882479A/en active Pending
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708436A (en) * | 2013-12-17 | 2014-04-09 | 北京化工大学 | Nitrogen-containing carbon nanotube with high heat resistance and preparation method of carbon nanotube |
| CN103708436B (en) * | 2013-12-17 | 2015-10-28 | 北京化工大学 | Nitrogenous carbon nanotube of a kind of high heat resistance and preparation method thereof |
| CN105314614A (en) * | 2014-06-04 | 2016-02-10 | 北京化工大学 | Nitrogen-doped porous carbon nanotube material and its preparation method and use in super capacitor electrode |
| CN104743543A (en) * | 2015-03-04 | 2015-07-01 | 同济大学 | Method for preparing polyaniline/phenolic aldehyde based carbon material |
| CN105355934A (en) * | 2015-10-31 | 2016-02-24 | 哈尔滨工业大学 | Preparation method of nitrogen-doped carbon nanotubes |
| CN105460917A (en) * | 2015-12-08 | 2016-04-06 | 武汉理工大学 | Nitrogen-doped carbon nanotube adopting hierarchical structure and preparation method |
| CN105460917B (en) * | 2015-12-08 | 2017-12-29 | 武汉理工大学 | A kind of nitrogen-doped carbon nanometer pipe and preparation method with hierarchy |
| CN107055511A (en) * | 2017-04-13 | 2017-08-18 | 常州纳欧新材料科技有限公司 | A kind of three-dimensional cross-linked CNT and preparation method thereof |
| CN107055511B (en) * | 2017-04-13 | 2019-04-16 | 常州纳欧新材料科技有限公司 | A kind of three-dimensional cross-linked carbon nanotube and preparation method thereof |
| CN109110744A (en) * | 2018-08-30 | 2019-01-01 | 浙江工业大学 | A kind of preparation method of hollow tubular polyaniline carbon material |
| CN111606405A (en) * | 2020-06-03 | 2020-09-01 | 北京林业大学 | Method for degrading organic pollutants in water by activating peracetic acid through nitrogen-doped carbon material |
| CN113186565A (en) * | 2021-04-14 | 2021-07-30 | 天津大学 | Preparation method of novel nitrogen-doped carbon material for electrocatalytic reduction of carbon dioxide |
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