CN104332328A - Nickel foam base type preparation method of nickel oxide/ polyaniline supercapacitor electrode material - Google Patents
Nickel foam base type preparation method of nickel oxide/ polyaniline supercapacitor electrode material Download PDFInfo
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- CN104332328A CN104332328A CN201410579087.2A CN201410579087A CN104332328A CN 104332328 A CN104332328 A CN 104332328A CN 201410579087 A CN201410579087 A CN 201410579087A CN 104332328 A CN104332328 A CN 104332328A
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- H01G11/30—Electrodes characterised by their material
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- 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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Abstract
The invention relates to a nickel foam base type preparation method of a nickel oxide/ polyaniline supercapacitor electrode material. The method comprises the following steps: preprocessing porous nickel foam to be used as a current collector of electrodes; getting conductive high-molecular polyaniline as an electrode intermediate layer; performing in-situ growth for a polyaniline nanorod on a nickel foam base; electrochemically depositing a nickel oxide nanosheet activating layer to obtain a super capacitor electrode material with high specific surface area and high activity. The preparation method is simple; polyaniline and nickel oxide are uniformly distributed in the prepared electrode material, and a porous structure is formed; the electromechanical performance is obviously improved by being compared with pure polyaniline and pure nickel oxide, and the specific capacitance reaches 418F/g.
Description
Technical field
The invention belongs to the preparation field of electrode material for super capacitor, particularly a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate.
Background technology
In recent years, ultracapacitor becomes candidate's energy storage device of most potentiality in energy source device of future generation gradually, because it has high power density, fast charge/discharge rates, long life and high operational safety, the required modern electronic equipment of era development and energy resource system can be met.According to charge storage mechanism, ultracapacitor can be roughly divided into two classes, i.e. double electric layer capacitor and fake capacitance capacitor, electrode material for electric double layer capacitor usually uses carbon-based material, and fake capacitance point volume container usually uses the material with redox reaction.
At present, research for fake capacitance ultracapacitor mainly concentrates on the transition metal oxide that development has commercial prospect, because these oxides have high, cheap, the eco-friendly feature of richness, particularly multiple electric charge valence state be can provide for redox electric charge shifts effectively, higher energy density and the theoretical ratio capacitance value of height thus obtained.
Add conducting polymer compound and can increase ratio capacitance, the operation principle of the ultracapacitor of conducting polymer is adopted also to be produce accurate faraday's electric capacity, this electrochemical reaction not only occurs in the surface of material, mainly occur in the 3-D solid structure of material, thus enable the electric charge of conductive polymer electrodes store high-density, produce large accurate faraday's electric capacity.
Summary of the invention
It take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate that technical problem to be solved by this invention is to provide a kind of, preparation method of the present invention is simple, prepared is that in the nickel oxide/polyaniline composite material of substrate, polyaniline and nickel oxide are evenly distributed with nickel foam, form loose structure, chemical property is good, is better than pure polyaniline and pure nickel.
Of the present invention a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, comprising:
(1) at ambient temperature, be that aniline monomer and the dopant of 1:1 ~ 10:1 is mixed in deionized water by mass ratio, under ice-water bath condition, stir, obtain solution A; Initator is dissolved in deionized water, under ice-water bath condition, stirs, obtains solution B;
(2) solution B is added dropwise in solution A, stirs and obtain mixed liquor, then nickel foam is immersed in mixed solution, leave standstill, obtain growing the nickel foam having polyaniline;
(3) prepare NiO precursor solution, have the nickel foam surface electrochemistry deposition NiO of polyaniline by cyclic voltammetry in growth, obtaining take nickel foam as the nickel oxide/polyaniline electrode material for super capacitor of substrate.
In described step (1), dopant is acrylic acid; Initator is ammonium persulfate, and in solution B, the concentration of initator is 0.1 ~ 1g/mL.
In described step (1) under ice-water bath condition, stir 1-2h, obtain solution A; Stir 15-30min, obtain solution B.
In described step (2), the volume ratio of solution A and solution B is 2-5:1; Stir 20-30s and obtain mixed solution.
Nickel foam is pretreated nickel foam in described step (2), and preliminary treatment is specially: first alternately clean with ethanol and deionized water, then uses hydrochloric acid cleaning, ultrasonic, and then use ethanol and deionized water alternately clean again, vacuumize.
Described concentration of hydrochloric acid is 1 ~ 6mol/L, and ultrasonic time is 1 ~ 8h; Vacuumize temperature is 40-70 DEG C, and drying time is 4-8h.
In described step (2), time of repose is 12-48h.
In described step (3), NiO precursor solution is nickel nitrate solution, and concentration is 0.1M-1M.
In described step (3), the design parameter of cyclic voltammetry is: make of platinum electrode and do reference electrode to electrode, Ag/AgCl electrode, sweep speed is 1 ~ 50mV/s, and cycle-index is 10 ~ 100 times.
Preparation method of the present invention, uses the foam nickel base of porous to considerably increase specific area as collector.Adopt the polyaniline intermediate layer of even compact that acrylic acid obtains as initator as dopant, ammonium persulfate, good conductivity and be conducive to the lifting of ratio capacitance.With cyclic voltammetry electrochemical precipitation process NiO as active layer, form loose structure with polyaniline, the electrode obtained chemical property obtains remarkable lifting.
Preparation method of the present invention: (1) carries out preliminary treatment to the nickel foam of porous, as the collector of electrode; (2) use conductive polymer polyanilinc as electrode intermediate layer, growth in situ polyaniline nano-rod in foam nickel base; (3) electrochemical deposition nickel oxide nano sheet active layer on the basis of (2), obtains one and has high-specific surface area, highly active electrode material for super capacitor
beneficial effect
(1) preparation method of the present invention is simple, requires low to production equipment;
(2) the nickel oxide/polyaniline composite electrode prepared by has large specific area and loose structure, and chemical property is good, and ratio capacitance reaches 418F/g, is better than pure polyaniline and pure nickel.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph that embodiment 1 synthesizes nickel oxide/polyaniline composite material, and wherein (a) is 10000 times of SEM photos amplified, and (b) is 20000 times of SEM photos amplified;
Fig. 2 is the cyclic voltammetry curve that embodiment 1 synthesizes nickel oxide/polyaniline composite electrode;
Fig. 3 is the charging and discharging curve that embodiment 1 synthesizes nickel oxide/polyaniline composite electrode;
Fig. 4 is the ratio capacitance curve that embodiment 1 synthesizes nickel oxide/polyaniline composite electrode and pure nickel electrode.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Nickel foam is cut out the thin slice of the wide 1cm of growth 4cm, ethanol and deionized water is used to replace flushing 3 times, take out after putting into the ultrasonic 2h of hydrochloric acid solution of 6mol/L, then after replacing flushing three times with ethanol and deionized water, put into vacuum drying oven dry 4h at the temperature of 60 DEG C.
Be scattered in the deionized water of 150mL by 2g polyaniline and 1.5g acrylic acid, ice-water bath stirs 2h, obtains A liquid.Be dissolved in the deionized water of 50mL by 6.5g ammonium persulfate, ice-water bath stirs 30min, obtains B liquid.B liquid is slowly added drop-wise in A liquid, stirs 30s and obtain mixed liquor.To immerse in mixed liquor through pretreated nickel foam thin slice and leave standstill 24h, obtain the polyaniline of in-situ polymerization.
The nickel nitrate taking 5.82g is dissolved in 200mL deionized water, prepares the precursor solution of nickel nitrate solution as NiO of 0.1M.Adopt cyclic voltammetry, using platinum electrode as to electrode, Ag/AgCl electrode as reference electrode, arranging voltage range is 0 ~-1.2V, and sweep speed is 50mV/s, circulates in electrochemical deposition NiO in nickel foam that growth has a polyaniline through 40.Obtaining take nickel foam as the nickel oxide/polyaniline electrode material for super capacitor of substrate.Surface sweeping electron microscopic observation shows: polyaniline and nickel oxide are evenly distributed, and forms loose structure.Cyclic voltammetry curve shows: the ratio capacitance of this composite electrode is higher than the ratio capacitance of pure NiO electrode.Calculated by charging and discharging curve: the ratio capacitance of this composite electrode is issued to 418F/g in the sweep speed of 1mV/s.
Embodiment 2
Nickel foam is cut out the thin slice of the wide 1cm of growth 4cm, ethanol and deionized water is used to replace flushing 3 times, take out after putting into the ultrasonic 3h of hydrochloric acid solution of 5mol/L, then after replacing flushing three times with ethanol and deionized water, put into vacuum drying oven dry 5h at the temperature of 60 DEG C.
Be scattered in the deionized water of 150mL by 2g polyaniline and 2g acrylic acid, ice-water bath stirs 2h, obtains A liquid.Be dissolved in the deionized water of 50mL by 5g ammonium persulfate, ice-water bath stirs 30min, obtains B liquid.B liquid is slowly added drop-wise in A liquid, stirs 30s and obtain mixed liquor.To immerse in mixed liquor through pretreated nickel foam thin slice and leave standstill 24h, obtain the polyaniline intermediate layer of in-situ polymerization.
The nickel nitrate taking 8.72g is dissolved in 200mL deionized water, prepares the precursor solution of nickel nitrate solution as NiO of 0.15M.Adopt cyclic voltammetry, using platinum electrode as to electrode, Ag/AgCl electrode as reference electrode, arranging voltage range is 0 ~-1.2V, and sweep speed is 20mV/s, circulates in electrochemical deposition NiO in nickel foam that growth has a polyaniline through 30.Obtaining take nickel foam as the nickel oxide/polyaniline electrode material for super capacitor of substrate.Surface sweeping electron microscopic observation shows: polyaniline and nickel oxide are evenly distributed, and forms loose structure.Cyclic voltammetry curve shows: the ratio capacitance of this composite electrode is higher than the ratio capacitance of pure NiO electrode.Calculated by charging and discharging curve: the ratio capacitance of this composite electrode is issued to 398F/g in the sweep speed of 1mV/s.
Embodiment 3
Nickel foam is cut out the thin slice of the wide 1cm of growth 4cm, ethanol and deionized water is used to replace flushing 3 times, take out after putting into the ultrasonic 4h of hydrochloric acid solution of 4mol/L, then after replacing flushing three times with ethanol and deionized water, put into vacuum drying oven dry 6h at the temperature of 60 DEG C.
Be scattered in the deionized water of 150mL by 2g polyaniline and 1g acrylic acid, ice-water bath stirs 2h, obtains A liquid.Be dissolved in the deionized water of 50mL by 8g ammonium persulfate, ice-water bath stirs 30min, obtains B liquid.B liquid is slowly added drop-wise in A liquid, stirs 30s and obtain mixed liquor.To immerse in mixed liquor through pretreated nickel foam thin slice and leave standstill 24h, obtain the polyaniline intermediate layer of in-situ polymerization.
The nickel nitrate taking 11.63g is dissolved in 200mL deionized water, prepares the precursor solution of nickel nitrate solution as NiO of 0.2M.Adopt cyclic voltammetry, using platinum electrode as to electrode, Ag/AgCl electrode as reference electrode, arranging voltage range is 0 ~-1.2V, and sweep speed is 10mV/s, circulates in electrochemical deposition NiO in nickel foam that growth has a polyaniline through 20.Obtaining take nickel foam as the nickel oxide/polyaniline electrode material for super capacitor of substrate.Surface sweeping electron microscopic observation shows: polyaniline and nickel oxide are evenly distributed, and forms loose structure.Cyclic voltammetry curve shows: the ratio capacitance of this composite electrode is higher than the ratio capacitance of pure NiO electrode.Calculated by charging and discharging curve: the ratio capacitance of this composite electrode is issued to 409F/g in the sweep speed of 1mV/s.
Claims (9)
1. be a preparation method for the nickel oxide/polyaniline electrode material for super capacitor of substrate with nickel foam, comprise:
(1) at ambient temperature, be that aniline monomer and the dopant of 1:1 ~ 10:1 is mixed in deionized water by mass ratio, under ice-water bath condition, stir, obtain solution A; Initator is dissolved in deionized water, under ice-water bath condition, stirs, obtains solution B;
(2) solution B is added dropwise in solution A, stirs and obtain mixed liquor, then nickel foam is immersed in mixed solution, leave standstill, obtain growing the nickel foam having polyaniline;
(3) prepare NiO precursor solution, have the nickel foam surface electrochemistry deposition NiO of polyaniline by cyclic voltammetry in growth, obtaining take nickel foam as the nickel oxide/polyaniline electrode material for super capacitor of substrate.
2. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (1), dopant is acrylic acid; Initator is ammonium persulfate, and in solution B, the concentration of initator is 0.1 ~ 1g/mL.
3. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (1) under ice-water bath condition, stir 1-2h, obtain solution A; Stir 15-30min, obtain solution B.
4. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (2), the volume ratio of solution A and solution B is 2-5:1; Stir 20-30s and obtain mixed solution.
5. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (2), nickel foam is pretreated nickel foam, preliminary treatment is specially: first alternately clean with ethanol and deionized water, use hydrochloric acid cleaning, ultrasonic again, then again alternately clean with ethanol and deionized water, vacuumize.
6. according to claim 5 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: described concentration of hydrochloric acid is 1 ~ 6mol/L, ultrasonic time is 1 ~ 8h; Vacuumize temperature is 40-70 DEG C, and drying time is 4-8h.
7. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (2), time of repose is 12-48h.
8. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (3), NiO precursor solution is nickel nitrate solution, and concentration is 0.1M-1M.
9. according to claim 1 a kind of take nickel foam as the preparation method of the nickel oxide/polyaniline electrode material for super capacitor of substrate, it is characterized in that: in described step (3), the design parameter of cyclic voltammetry is: make of platinum electrode and do reference electrode to electrode, Ag/AgCl electrode, sweep speed is 1 ~ 50mV/s, and cycle-index is 10 ~ 100 times.
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Cited By (8)
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| CN106158394A (en) * | 2016-06-29 | 2016-11-23 | 西北师范大学 | A kind of preparation method of nickel foam based super capacitor electrode material |
| CN106449175A (en) * | 2016-11-14 | 2017-02-22 | 江苏大学 | Method for preparing nickel tungstate/polyaniline super-capacitor electrode material by taking foamed nickel as substrate |
| CN106750284A (en) * | 2017-01-19 | 2017-05-31 | 北京工商大学 | A kind of foam metal doped polyaniline electromagnetic shielding material and preparation method thereof |
| CN108010727A (en) * | 2017-11-17 | 2018-05-08 | 合肥师范学院 | Core shell structure nickel oxide/polyaniline electrode material for super capacitor and preparation method |
| CN108648923A (en) * | 2018-05-03 | 2018-10-12 | 河北工业大学 | A kind of MnO2The preparation method of-PANI/ titanium foam combination electrodes |
| CN111825127A (en) * | 2020-07-07 | 2020-10-27 | 江苏大学 | Preparation method and application of metal nickel-based nano material |
| CN113223871A (en) * | 2021-04-15 | 2021-08-06 | 山东科技大学 | Preparation and application of NiO/C composite electrode material with foam nickel sheet as substrate |
| CN113394030A (en) * | 2021-06-26 | 2021-09-14 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106158394A (en) * | 2016-06-29 | 2016-11-23 | 西北师范大学 | A kind of preparation method of nickel foam based super capacitor electrode material |
| CN106158394B (en) * | 2016-06-29 | 2018-04-13 | 西北师范大学 | A kind of preparation method of nickel foam based super capacitor electrode material |
| CN106449175A (en) * | 2016-11-14 | 2017-02-22 | 江苏大学 | Method for preparing nickel tungstate/polyaniline super-capacitor electrode material by taking foamed nickel as substrate |
| CN106750284A (en) * | 2017-01-19 | 2017-05-31 | 北京工商大学 | A kind of foam metal doped polyaniline electromagnetic shielding material and preparation method thereof |
| CN108010727B (en) * | 2017-11-17 | 2019-09-27 | 合肥师范学院 | Core-shell structure nickel oxide/polyaniline electrode material for super capacitor and preparation method |
| CN108010727A (en) * | 2017-11-17 | 2018-05-08 | 合肥师范学院 | Core shell structure nickel oxide/polyaniline electrode material for super capacitor and preparation method |
| CN108648923A (en) * | 2018-05-03 | 2018-10-12 | 河北工业大学 | A kind of MnO2The preparation method of-PANI/ titanium foam combination electrodes |
| CN108648923B (en) * | 2018-05-03 | 2020-01-21 | 河北工业大学 | MnO (MnO)2Preparation method of-PANI/foam titanium composite electrode |
| CN111825127A (en) * | 2020-07-07 | 2020-10-27 | 江苏大学 | Preparation method and application of metal nickel-based nano material |
| CN111825127B (en) * | 2020-07-07 | 2023-06-16 | 江苏大学 | Preparation method and application of metallic nickel-based nanomaterial |
| CN113223871A (en) * | 2021-04-15 | 2021-08-06 | 山东科技大学 | Preparation and application of NiO/C composite electrode material with foam nickel sheet as substrate |
| CN113394030A (en) * | 2021-06-26 | 2021-09-14 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
| CN113394030B (en) * | 2021-06-26 | 2022-09-09 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
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