CN104201008A - Nickel oxide and nitrogen doped carbon nanotube composite electrode materials for super capacitor and production method thereof - Google Patents
Nickel oxide and nitrogen doped carbon nanotube composite electrode materials for super capacitor and production method thereof Download PDFInfo
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Abstract
The invention discloses nickel oxide and nitrogen doped carbon nanotube composite electrode materials for a super capacitor and a production method thereof. The nickel oxide and nitrogen doped carbon nanotube composite electrode materials comprises a current collector, a nitrogen doped carbon nanotube and nickel oxide; the nitrogen doped carbon nanotube is loaded on the current collector in an in-situ composite mode; nickel oxide wraps the surface of the nitrogen doped carbon nanotube. Compared with the prior art, the performance of the super capacitor is greatly improved, the discharge capacity reaches up to 2800 farads every gram under the 10 amperes every gram of current density and is much higher than that of other similar reported materials, the discharge capacity of the other similar reported materials is 1471 farads every gram under the 10 amperes every gram of current density, the cost is low, the method is simple, the production rate is high, and the nickel oxide and nitrogen doped carbon nanotube composite electrode materials for the super capacitor and the production method thereof are expected to be widely applied to the field of super capacitors.
Description
Technical field
The present invention relates to electrochemical field, particularly nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material and preparation method thereof for a kind of ultracapacitor.
Background technology
The consumption of the variation of weather and fossil fuel (as coal, oil and natural gas etc.) has tremendous influence to All Around The World economy and ecology.Various countries all drop into a large amount of human and material resources and financial resources are researched and developed new forms of energy and renewable and clean energy resource.New forms of energy and renewable and clean energy resource comprise solar energy, wind energy, oceanic energy, Hydrogen Energy, primary cell, secondary cell and ultracapacitor etc.Ultracapacitor, is often called as again electrochemical capacitor, and oneself is no longer circuit element in general sense, but a kind of a kind of Novel energy storage apparatus between traditional electrostatic condenser and rechargeable battery, the commercial applications developing history of existing more than 30 year.According to the difference of energy storage mechanism, ultracapacitor can be divided into double electric layer capacitor and redox capacitors.Because it has the advantages such as the high and overlength service life cycle of large electric current fast charging and discharging, power density, oneself causes numerous research workers' very big interest.Compared with traditional electrostatic condenser, ultracapacitor has more people's energy density; And compared with battery, although its energy density (approximately 5Wh/kg) is lower than battery, but it has higher power density (10Kw/kg), discharge and recharge number of times and can reach more than tens thousand of times, the life-span is long, charging interval is short, can high current charge-discharge.Because ultracapacitor has These characteristics, so be just subject to people's attention once coming out, can be applied to the fields such as consumer electronics product field, data accumulating storage system, intelligent distributed network system field, grid-connected power generation system, electric car power supply and emergent back-up source, particularly on electric automobile, there is very significantly application advantage, belong to the complete series low-carbon economy core product of standard.Ultracapacitor can be divided into two classes according to its energy storage principle: double electric layer capacitor and fake capacitance device.The general principle of double layer capacitor is to utilize the interfacial electric double layer forming between electrode and electrolyte to carry out a kind of electronic component of stored energy.In the time that electrode contacts with electrolyte, due to the effect of Coulomb force, molecular separating force or interatomic force, make solid liquid interface occur double-deck electric charge stable, that symbol is contrary, be called interfacial electric double layer.Fake capacitance is also referred to as pseudo capacitance, at electrode surface or body in the two dimension or accurate two-dimensional space in mutually, electroactive material carries out underpotential deposition, and highly reversible chemisorbed/desorption or oxidation/reduction reaction occurs, and produces the electric capacity relevant with electrode charge current potential.Pseudo capacitance device is divided into: the pseudo capacitance device based on metal oxide and the pseudo capacitance device based on conducting polymer, wherein again with metal oxide with its high power capacity and high stability and receive much concern.
At present, both at home and abroad to the research work of transition metal oxide mainly around the following aspects: (1) is used distinct methods to prepare the RuO of bigger serface: electrode material; (2) finding other cheap materials replaces noble metal to reduce material cost; (3) different materials is compound, to improve the ratio electric capacity of material.In all transition metal oxides, ruthenium-oxide is the most excellent super capacitor material of capacitive property, and RuO2 has high specific capacity, but fancy price has limited its application in ultracapacitor.Therefore, the transition metal oxide of other relative low price is also commonly used for the electrode material of ultracapacitor, as: MnO2, NiO and Co3O4 etc.NiO is as function admirable, and cheap super capacitor material is constantly attracting everybody research interest in recent years.In order further to improve the specific capacity of this material, nanometer technology is constantly applied in the preparation of this material as the effective means of emerging raising energy and material energy storage efficiency, due to the tremendous influence effect of nanometer material structure team performance, the NiO nano material of each middle structure is also produced out simultaneously.Lv etc. (Journal of Alloys and Compounds 603 (2014) 190 – 196) prepare sheet NiO by hydro thermal method on nickel foam surface, be used for as electrode material for super capacitor, recording single electrode is 349F/g than electric capacity; (the J.Power Sources 2014 such as Cao, 264,161-167) prepare and make nanometer column NiO electrode material on nickel foam surface with electrochemical deposition method, and studied the capacitance characteristic of NiO, result shows under the current density of 2A/g, and single electrode is 675F/g than electric capacity.And NiO itself is as transition metal oxide, there is the relatively poor characteristic of conductivity, this time, the compound of NiO and material with carbon element can be promoted to its conductivity, improve its performance as electrode material.To so far, about electrochemical deposition NiO on nitrogen-doped carbon nanometer pipe@nickel foam surface as the research aspect the electrochemistry of electrode of super capacitor, not yet have report, and the material of the three dimensional composite structure of this binder free will inevitably there is huge using value in energy storage and other field.
Summary of the invention
In view of this, the object of the invention is to adopt chemical vapour deposition technique, nitrogen-doped carbon nano material is grown directly upon on the collector of nickel foam, with electrochemical deposition, NiO original position is compounded in to nitrogen-doped carbon nanometer pipe surface again and obtains a kind of composite electrode that can make the performance of ultracapacitor increase substantially, do not need to use any carrier and binding agent, ensureing, under the prerequisite of electrode content, inert matter content in electrode to be dropped to minimum.
Nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for a kind of ultracapacitor of the present invention, described electrode material comprises that nitrogen-doped carbon nanometer pipe on described collector of collector and original position composite load and original position are compounded in the nickel oxide on nitrogen-doped carbon nanometer pipe surface, the common electrode that forms the integrated design with loose structure of nitrogen-doped carbon nanometer pipe and nickel oxide and collector.
Further, described collector is nickel foam, and the nitrogen-doped carbon nanometer pipe of original position composite load on described collector prepared by chemical gaseous phase depositing process, and the nickel oxide that is coated on nitrogen-doped carbon nanometer pipe surface is prepared by electrochemical deposition method;
Further, reaction system is the mixed solution of ethanol and water, and raw material is nickel nitrate and sodium nitrate;
Further, nickel oxide loaded amount is 1-10mg (nickel oxide)/1cm
2(collector);
Further, the volume equivalent diameter of nitrogen-doped carbon nanometer pipe is 20nm-500nm;
Further, described nickel oxide is cotton-shaped, needle-like or sheet.
The present invention also discloses the preparation method of a kind of ultracapacitor nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material, and on collector, original position Compound Negative is loaded with the compound of nitrogen-doped carbon nanometer pipe and NiO, comprises the following steps:
(a) collector preliminary treatment;
(b) nitrogen-doped carbon nanometer pipe is passed through to original position composite load on described collector;
(c) nickel oxide is compounded with on the collector of nitrogen-doped carbon nanometer pipe in original position by original position composite load.
Beneficial effect of the present invention: nitrogen is adulterated to tubular nanometer material with carbon element Direct Uniform growth (or deposition) to the skeleton as NiO nanostructure growth on collector, further on nitrogen doping tubular nanometer material with carbon element, in-situ deposition has the chemically active NiO of good electric again, and set it as the electrode of ultracapacitor, and do not need to use any carrier and binding agent, ensureing, under the prerequisite of electrode material content, inert matter content in air electrode to be dropped to minimum.This novel binder free composite three dimensional structure electrode has obviously promoted the specific capacity of ultracapacitor: when current density is 2A/g up to 769F/g, in the time that bringing up to 50A/g, current density still keeps 577F/g, in the analog material of existing bibliographical information, belong to top standard, the various technical operations that material preparation adopts are simple, are applicable to large-scale production.
Brief description of the drawings
Below in conjunction with the drawings and specific embodiments to further instruction of the present invention.
Fig. 1 is the nickel oxide that obtains of embodiment 4 and the nitrogen-doped carbon nanometer pipe catalyst stereoscan photograph in the online deposition of collector Ni.
Fig. 2 is the XRD analysis collection of illustrative plates of the composite electrode of gained in embodiment 4.
Fig. 3 is the specific capacity that the composite electrode of gained in embodiment 4 has superelevation during for ultracapacitor, under the current density test condition increasing successively, there is good stability, in the time that current density is 2A/g up to 769F/g, when 5A/g, be 686F/g, when 10A/g, be 668F/g, when 20A/g, be 622F/g, in the time that current density is brought up to 50A/g, still keep 577F/g.
Embodiment
Nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for the ultracapacitor of the present embodiment, described electrode material comprises that nitrogen-doped carbon nanometer pipe on described collector of collector and original position composite load and original position are compounded in the nickel oxide on nitrogen-doped carbon nanometer pipe surface, the common electrode that forms the integrated design with loose structure of nitrogen-doped carbon nanometer pipe and nickel oxide and collector.
In the present embodiment, described collector is nickel foam, and the nitrogen-doped carbon nanometer pipe of original position composite load on described collector prepared by chemical gaseous phase depositing process, and the nickel oxide that is coated on nitrogen-doped carbon nanometer pipe surface is prepared by electrochemical deposition method.
In the present embodiment, reaction system is the mixed solution of ethanol and water, and raw material is nickel nitrate and sodium nitrate.
In the present embodiment, nickel oxide loaded amount is 1-10mg (nickel oxide)/1cm
2(collector);
In the present embodiment, the volume equivalent diameter of nitrogen-doped carbon nanometer pipe is 20nm-500nm;
In the present embodiment, described nickel oxide is cotton-shaped, needle-like or sheet.
The present invention also discloses the preparation method of a kind of ultracapacitor nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material, and on collector, original position Compound Negative is loaded with the compound of nitrogen-doped carbon nanometer pipe and NiO, comprises the following steps:
(a) collector preliminary treatment;
(b) nitrogen-doped carbon nanometer pipe is passed through to original position composite load on described collector;
(c) nickel oxide is compounded with on the collector of nitrogen-doped carbon nanometer pipe in original position by original position composite load.
Ultracapacitor composite electrode of the present invention, on collector, original position Compound Negative is loaded with the compound of nitrogen-doped carbon nanometer pipe and NiO; Be preferably, NiO is cotton-shaped, needle-like or sheet.Nitrogen-doped carbon nanometer pipe, NiO and collector three person form loose structure jointly.Described " original position is compound " refers at collection liquid surface reaction in-situ and generates and while load nitrogen-doped carbon nanometer pipe and NiO, be known for those skilled in the art, adopt the compound structure of original position to make collector and carbon nanomaterial and NiO jointly form the electrode of integrated design.In preparation method, time prepared by nitrogen-doped carbon nanometer pipe, required presoma is selected from following organic substance: (I) nitrogenous source: urea, pyridine, melamine, imidazoles, ethylenediamine, dimethyl amide or its combination; (II) carbon source: toluene, dimethylbenzene, acetylene, ethane, ethene, ethanol or its combination; Can adopt graphite acr method, laser evaporation method, catalystic pyrolysis, chemical vapour deposition technique, template, hydro thermal method or condensed phase electrolysis method of formation to carry out original position compound; Time prepared by nickel oxide, required presoma is the soluble-salt that comprises nickel ion, comprises nitrate, carbonate, phosphate etc.; Can adopt electrochemical deposition method, hydro thermal method etc.
Below by specific embodiment, the present invention is further elaborated.
Embodiment mono-
1. really take ferrocene 300mg (analyzing pure) and melamine 500mg (analyzing pure), after being mixed, in mortar, be fully ground to and mix.2. to be placed in acetone ultrasonic for foam Ni, with distilled water washing, and then ultrasonic with ethanol, washs with distilled water.2. foam Ni after treatment is placed in objective table, puts into reaction warehouse flat-temperature zone.Temperature-rise period leads to Ar (60cm
3/ min) as protection gas, ethene is as carbon source.Reach after design temperature, will 1. slowly add reaction warehouse, obtain the composite construction of nitrogen-doped carbon nanometer pipe@foam Ni net.3. 2g nickel nitrate and 2g sodium nitrate are put into and the deionized water of 100ml is housed and the blend solution of ethanol 1:1 (volume ratio) stirs as electroplate liquid, 2. middle gained composite construction is work electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, galvanostatic deposition method is carried out electrochemical deposition (size of current is 32mA, and sedimentation time is 1800S).4. above-mentioned gained composite construction 100 degree under inert atmosphere are annealed 2 hours, obtain nickel oxide original position and be compounded in the composite construction that nitrogen-doped carbon nanometer pipe@foam Ni nets.
Embodiment bis-
1. really take ferrocene 300mg (analyzing pure) and melamine 500mg (analyzing pure), after being mixed, in mortar, be fully ground to and mix.2. to be placed in acetone ultrasonic for foam Ni, with distilled water washing, and then ultrasonic with ethanol, washs with distilled water.2. foam Ni after treatment is placed in objective table, puts into reaction warehouse flat-temperature zone.Temperature-rise period leads to Ar (60cm
3/ min) as protection gas, ethene is as carbon source.Reach after design temperature, will 1. slowly add reaction warehouse, obtain the composite construction of nitrogen-doped carbon nanometer pipe@foam Ni net.3. 2g nickel nitrate and 2g sodium nitrate are put into and the deionized water of 100ml is housed and the blend solution of ethanol 1:1 (volume ratio) stirs as electroplate liquid, 2. middle gained composite construction is work electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, galvanostatic deposition method is carried out electrochemical deposition (size of current is 16mA, and sedimentation time is 1800S).4. above-mentioned gained composite construction 100 degree under inert atmosphere are annealed 2 hours, obtain nickel oxide original position and be compounded in the composite construction that nitrogen-doped carbon nanometer pipe@foam Ni nets.
Embodiment tri-
1. really take ferrocene 300mg (analyzing pure) and melamine 500mg (analyzing pure), after being mixed, in mortar, be fully ground to and mix.2. to be placed in acetone ultrasonic for foam Ni, with distilled water washing, and then ultrasonic with ethanol, washs with distilled water.2. foam Ni after treatment is placed in objective table, puts into reaction warehouse flat-temperature zone.Temperature-rise period leads to Ar (60cm
3/ min) as protection gas, ethene is as carbon source.Reach after design temperature, will 1. slowly add reaction warehouse, obtain the composite construction of nitrogen-doped carbon nanometer pipe@foam Ni net.3. 2g nickel nitrate and 2g sodium nitrate are put into and the deionized water of 100ml is housed and the blend solution of ethanol 1:1 (volume ratio) stirs as electroplate liquid, 2. middle gained composite construction is work electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, galvanostatic deposition method is carried out electrochemical deposition (size of current is 8mA, and sedimentation time is 1800S).4. above-mentioned gained composite construction 100 degree under inert atmosphere are annealed 2 hours, obtain nickel oxide original position and be compounded in the composite construction that nitrogen-doped carbon nanometer pipe@foam Ni nets.
Embodiment tetra-
1. really take ferrocene 300mg (analyzing pure) and melamine 500mg (analyzing pure), after being mixed, in mortar, be fully ground to and mix.2. to be placed in acetone ultrasonic for foam Ni, with distilled water washing, and then ultrasonic with ethanol, washs with distilled water.2. foam Ni after treatment is placed in objective table, puts into reaction warehouse flat-temperature zone.Temperature-rise period leads to Ar (60cm
3/ min) as protection gas, ethene is as carbon source.Reach after design temperature, will 1. slowly add reaction warehouse, obtain the composite construction of nitrogen-doped carbon nanometer pipe@foam Ni net.3. 2g nickel nitrate and 2g sodium nitrate are put into and the deionized water of 100ml is housed and the blend solution of ethanol 1:1 (volume ratio) stirs as electroplate liquid, 2. middle gained composite construction is work electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, galvanostatic deposition method is carried out electrochemical deposition (size of current is 4mA, and sedimentation time is 1800S).4. above-mentioned gained composite construction 100 degree under inert atmosphere are annealed 2 hours, obtain nickel oxide original position and be compounded in the composite construction that nitrogen-doped carbon nanometer pipe@foam Ni nets.
Experimental technique in above-described embodiment, conventionally according to normal condition, or the condition of advising according to manufacturer.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (7)
1. a nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor, it is characterized in that: described electrode material comprises that nitrogen-doped carbon nanometer pipe on described collector of collector and original position composite load and original position are compounded in the nickel oxide on nitrogen-doped carbon nanometer pipe surface the common electrode that forms the integrated design with loose structure of nitrogen-doped carbon nanometer pipe and nickel oxide and collector.
2. nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 1, it is characterized in that: described collector is nickel foam, the nitrogen-doped carbon nanometer pipe of original position composite load on described collector prepared by chemical gaseous phase depositing process, and the nickel oxide that is coated on nitrogen-doped carbon nanometer pipe surface is prepared by electrochemical deposition method.
3. nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 2, is characterized in that: reaction system is the mixed solution of ethanol and water, and raw material is nickel nitrate and sodium nitrate.
4. nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 3, is characterized in that: nickel oxide loaded amount is 1-10mg (nickel oxide)/1cm
2(collector).
5. nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 4, is characterized in that: the volume equivalent diameter of nitrogen-doped carbon nanometer pipe is 20nm-500nm.
6. nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 5, is characterized in that: described nickel oxide is cotton-shaped, needle-like or sheet.
7. the preparation method of nickel oxide nitrogen-doped carbon nanometer pipe combination electrode material for ultracapacitor according to claim 1, is characterized in that: on collector, original position Compound Negative is loaded with the compound of nitrogen-doped carbon nanometer pipe and Co3O4, comprises the following steps:
(a) collector preliminary treatment;
(b) nitrogen-doped carbon nanometer pipe is passed through to original position composite load on described collector;
(c) nickel oxide is compounded with on the collector of nitrogen-doped carbon nanometer pipe in original position by original position composite load.
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Cited By (6)
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| CN104681810A (en) * | 2015-01-11 | 2015-06-03 | 北京工业大学 | Cobaltosic oxide nitrogen-doped carbon nanotube three-dimensional composite electrode material for lithium ion battery and manufacturing method of electrode material |
| CN104966625A (en) * | 2015-07-31 | 2015-10-07 | 西安科技大学 | N-doped porous carbon/NiO composite material and preparation method therefor |
| CN105244188A (en) * | 2015-10-22 | 2016-01-13 | 东莞市鸿愃实业有限公司 | Preparation method of carbon nano tube yarn flexible super capacitor composite electrode material |
| CN110379640A (en) * | 2019-07-16 | 2019-10-25 | 苏州科技大学 | Multilayered structure composite material and preparation method and application |
| CN110853938A (en) * | 2019-11-22 | 2020-02-28 | 吉林建筑大学 | Symmetrical super capacitor |
| CN114974938A (en) * | 2022-07-08 | 2022-08-30 | 曲靖师范学院 | Preparation of Mn-Ni double-monoatomic modulation CN graded carbon tube electrode material |
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| CN104681810A (en) * | 2015-01-11 | 2015-06-03 | 北京工业大学 | Cobaltosic oxide nitrogen-doped carbon nanotube three-dimensional composite electrode material for lithium ion battery and manufacturing method of electrode material |
| CN104966625A (en) * | 2015-07-31 | 2015-10-07 | 西安科技大学 | N-doped porous carbon/NiO composite material and preparation method therefor |
| CN104966625B (en) * | 2015-07-31 | 2017-07-28 | 西安科技大学 | One kind mixes N porous carbons/NiO composites and preparation method thereof |
| CN105244188A (en) * | 2015-10-22 | 2016-01-13 | 东莞市鸿愃实业有限公司 | Preparation method of carbon nano tube yarn flexible super capacitor composite electrode material |
| CN110379640A (en) * | 2019-07-16 | 2019-10-25 | 苏州科技大学 | Multilayered structure composite material and preparation method and application |
| CN110853938A (en) * | 2019-11-22 | 2020-02-28 | 吉林建筑大学 | Symmetrical super capacitor |
| CN110853938B (en) * | 2019-11-22 | 2021-07-23 | 吉林建筑大学 | Symmetrical super capacitor |
| CN114974938A (en) * | 2022-07-08 | 2022-08-30 | 曲靖师范学院 | Preparation of Mn-Ni double-monoatomic modulation CN graded carbon tube electrode material |
| CN114974938B (en) * | 2022-07-08 | 2023-07-14 | 曲靖师范学院 | Preparation of Mn-Ni double single-atom modulation CN graded carbon tube electrode material |
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