CN105931861B - A kind of preparation method for the electrode of super capacitor for being covered with active electrode film - Google Patents
A kind of preparation method for the electrode of super capacitor for being covered with active electrode film Download PDFInfo
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- CN105931861B CN105931861B CN201610423216.8A CN201610423216A CN105931861B CN 105931861 B CN105931861 B CN 105931861B CN 201610423216 A CN201610423216 A CN 201610423216A CN 105931861 B CN105931861 B CN 105931861B
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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
Abstract
The invention discloses a kind of preparation method for the electrode of super capacitor for being covered with active electrode film, by making oil removing, washing, pickling, water-washing pre-treatment to conductive foil matrix, then conductive foil coating surface ambrose alloy ferrophosphor(us) film after treatment, compound (hydrogen) oxidation film of fabricated in situ is corroded by thermokalite again, the electrode of super capacitor for being covered with active electrode film is made in last cyclic activation.The advantages that electrode of super capacitor of prepared by the present invention be covered with electrode film is conductive, mechanical property, corrosion resistance and heat-resist, and internal resistance is small, and specific capacitance is high, and adhesion is high between electrode film and collector, and electrode film thickness is uniform；The electrode of super capacitor specific capacitance of preparation reaches 1.45F/cm2, capacity retention is up to 98.1% after circulation 3500 times.And preparation method provided by the invention have the characteristics that required equipment investment is few, technological operation is simple and easy to control, it is reproducible, be adapted to industrialization production.
Description
Technical field
The present invention relates to a kind of preparation method of electrode of super capacitor, and in particular to a kind of to be covered with the super of active electrode film
The preparation method of level electrode for capacitors.
Background technology
Ultracapacitor has security and power density high, has extended cycle life, can high current charge-discharge the advantages that, be near
The novel energy storage apparatus that Nian Lai various countries are competitively studied, it is super in fields such as solar wind-energy generating, electric automobile, consumer electronics
The application prospect of capacitor is boundless.
Because electrode is the core component of ultracapacitor, thus new electrode materials turn into ultracapacitor area research
Focus and emphasis.Electrode material for super capacitor mainly includes carbon material, metal (hydrogen) oxide and conducting polymer three major types.
Metal (hydrogen) oxide electrode material heat resistance is better than conductive polymer electrodes material；And when electrode surface area is identical, metal
For the capacitance of (hydrogen) oxide electrode material up to the decades of times of carbon material electric double layer capacitance value, these performance characteristics make metal
The design of (hydrogen) oxide electrode material receives much concern.
Compared with noble metal oxide electrodes material such as ruthenium-oxide, cheap metal (hydrogen) oxide such as (hydrogen) nickel oxide, oxygen
Change manganese etc. because with significant price advantage and being widely applied prospect in civil area and turning into people in recent years and research and develop
Emphasis.
The problem of cheap metal (hydrogen) oxide electrode engineer applied is primarily present includes：
1st, electrode process complexity is prepared, it is more to influence electrode performance factor, causes poor repeatability；
2nd, poorly conductive, it is unfavorable for charge and discharge process electric transmission, causes power density not high；
3rd, mechanical performance is poor, limits in complicated applied force applications；
4th, high is required to current collector material corrosion resistance；
5th, synthesized between electrode material membrane and collector by suppressing, adhesion is poor, membrane thickness unevenness；
6th, internal resistance is larger, and anti-over-charging, which is crossed, to be put poor with short-circuit capability, and security is poor.
The content of the invention
To solve the deficiencies in the prior art, there is good heat resistance and thermostabilization it is an object of the invention to provide a kind of
Property, and preparation technology is simple, it is easy to operate, equipment investment is few, cost is low, be adapted to industrialization production be covered with the super of electrode film
The preparation method of electrode for capacitors.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
A kind of preparation method for the electrode of super capacitor for being covered with active electrode film, comprises the following steps：
S1, substrate pretreated：Using conductive foil as matrix, conductive foil is made to oil removing, washing, pickling, washing process successively；
S2, chemical plating overlay film：Conductive foil after above-mentioned processing is placed in ambrose alloy iron phosphorus chemistry plating solution, on conductive foil surface
Washed after plated nickel copper and iron phosphorus alloy film, collector is made；
S3, thermokalite corrosion fabricated in situ：Above-mentioned collector is immersed in potassium hydroxide solution, taking-up is placed in baking oven hot
Corrosion, in collection liquid surface fabricated in situ hydroxide and/or oxide composite membrane；
S4, cyclic activation：Collector after above-mentioned heat erosion is placed in potassium hydroxide solution after cyclic activation and dried, is made
The electrode of super capacitor of active electrode film must be covered with.
Nickel in above-mentioned steps S2 ambrose alloy ferrophosphor(us) films, copper, the mass percent of iron and phosphorus are respectively 33.74%-
43.02%th, 50.16%-57.58%, 1.94%-5.59% and 3.08%-4.88%.
Nickel in above-mentioned steps S4 electrode films, copper, iron, the mass percent of phosphorus and oxygen be respectively 36.46%-77.97%,
7.47%-51.50%, 4.64%-23.32%, 0.14%-3.01% and 2.93%-7.05%.
Above-mentioned steps S4 electrode films are hydroxide and/or oxide composite membrane with tetrahedron and octahedral structure.
Plating temperature is 81-83 DEG C in above-mentioned steps S2, Plating times 10-60min.
Potassium hydroxide solution concentration is 2-20mol/L in above-mentioned steps S3, soak time 1-5min, and oven temperature is
50-200 DEG C, etching time 1-8h.
Potassium hydroxide solution concentration is 2mol/L in above-mentioned steps S4.
Cyclic activation is 5 weeks in above-mentioned steps S4, and activation voltage is ± 3V, sweep speed 50mV/s.
Conductive foil is the good metal or nonmetallic of electric conductivity in above-mentioned steps S1.
Conductive foil is preferably pure iron foil in above-mentioned steps S1, and size is 20 × 10 × 0.2mm.
The present invention is advantageous in that：With existing ultracapacitor cheap metal (hydrogen) oxide electrode preparation method phase
Than a kind of super capacitor electrode for being covered with active electrode film for corroding fabricated in situ using ambrose alloy iron phosphorus thermokalite provided by the invention
Pole, there is advantages below：
1st, compound (hydrogen) the oxide electrode film that prepared by the present invention is anti-directly in collection liquid surface by situ synthesis techniques
It should generate, there is good adhesion between electrode film and collector；
2nd, the collection liquid surface for preparing of the present invention is coated with ambrose alloy ferrophosphor(us) film, due to ambrose alloy ferrophosphor(us) have it is excellent
Corrosion resistance, thus relatively low is required to the corrosion resistance of collector matrix material；
3rd, electrode of super capacitor prepared by the present invention is because electrode film is directly in collector by situ synthesis techniques
Surface Creation, the good mechanical property of electrode, available for complicated applied force occasion；
4th, collector has good electric conductivity in electrode of super capacitor prepared by the present invention, and electrode film is porous knot
Structure, electrolyte can directly contact with collector, and electrode internal resistance is smaller；
5th, electrode of super capacitor prepared by the present invention has good heat resistance and heat endurance, higher available for temperature
Occasion.
6th, electrode of super capacitor preparation method of the invention have technique is simple to operation, equipment investment is few, cost is low,
The features such as being adapted to industrialization production.
Brief description of the drawings
Fig. 1 is prepared for a kind of embodiment 1 of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
Electrode film surface topography SEM photograph.
Fig. 2 is prepared for a kind of embodiment 1 of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
Electrode of super capacitor use different scanning rates test cyclic voltammetry curve.
Fig. 3 is prepared for a kind of embodiment 1 of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
Electrode of super capacitor circulate the charging and discharging curves of different cycles.
Fig. 4 is prepared for a kind of embodiment 1 of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
Electrode of super capacitor capability retention with circulation cycle relation curve.
Fig. 5 is prepared for a kind of embodiment 2 of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
Electrode film surface topography SEM photograph.
Fig. 6 is a kind of embodiment 2-4 systems of the preparation method for the electrode of super capacitor for being covered with active electrode film of the present invention
The cyclic voltammetry curve of standby electrode of super capacitor.
Embodiment
The detection device and detection method used in the embodiment of the present invention be：
1st, produced using Jeol Ltd., model JSM6360LV SEM is to electrode film table
Face pattern carries out observation analysis.
2nd, using EDAX Co., Ltds of the U.S. production, model GENESIS2000XMS60 energy depressive spectroscopy to ambrose alloy iron
The composition of phosphorus alloy film and electrode film is analyzed.
3rd, using AMETEK companies of the U.S. production, model PARSTAT2273 electrochemical workstation to preparing electrode
Cyclic voltammetry curve is tested.
4th, using Arbin Instruments companies of the U.S. production, model SCTS electrochemical capacitance test system to prepare
The charging and discharging curve and capability retention of electrode are tested.
A kind of preparation method for the electrode of super capacitor for being covered with active electrode film, comprises the following steps：
S1, using 20 × 10 × 0.2mm pure iron foil as matrix, conductive foil is made successively oil removing, washing, pickling, at washing
Reason；
S2, the pure iron foil after processing is placed in plating 10-60min in 82 DEG C of ambrose alloy iron phosphorus chemistry plating solution, in conductive foil
Washed after coating surface ambrose alloy ferrophosphor(us) film, collector is made；
S3, collector is immersed in 1-5min in 2-20mol/L potassium hydroxide solutions, taking-up is placed in 50-200 DEG C of baking oven
Heat erosion 1-8h, in collection liquid surface fabricated in situ hydroxide and/or oxide composite membrane；
S4, the collector after heat erosion is placed in cyclic activation in 2mol/L potassium hydroxide solutions dried after 5 weeks, activation electricity
Press as ± 3V, sweep speed 50mV/s, the obtained electrode of super capacitor for being covered with active electrode film.
Embodiment：
In the present embodiment 1-7, with PARSTAT2273 electrochemical workstations, using Hg/HgO electrodes as reference electrode, platinum electrode
For auxiliary electrode, the electrode of super capacitor for being covered with electrode film prepared by embodiment 1-7 is working electrode, and its bare area is
1.0cm2, using 2mol/L KOH solutions as electrolyte, potential window 0.20-0.70V, when foundation sweep speed is 10mV/s
Cyclic voltammetry curve calculates specific capacitance (F/cm2)。
Energy spectrum analysis shows, embodiment 1, embodiment 5, Plating times 30min, Ni, Cu, Fe in ambrose alloy ferrophosphor(us) film
Mass percent with P is respectively 40.98%, 51.42%, 3.08% and 4.52%.
Energy spectrum analysis shows, embodiment 2, embodiment 3, embodiment 4, Plating times 20min, in ambrose alloy ferrophosphor(us) film
Ni, Cu, Fe and P mass percent are respectively 38.04%, 53.41%, 4.43% and 4.12%.
Energy spectrum analysis shows, embodiment 6, embodiment 7, Plating times 10min, Ni, Cu, Fe in ambrose alloy ferrophosphor(us) film
Mass percent with P is respectively 33.74%, 57.58%, 5.59% and 3.09%.
Energy spectrum analysis shows, in the electrode film of embodiment 1 Ni, Cu, Fe, P and O mass percent be respectively 77.97%,
7.47%th, 7.37%, 0.14% and 7.05%.
Energy spectrum analysis shows, in the electrode film of embodiment 4 Ni, Cu, Fe, P and O mass percent be respectively 76.51%,
10.32%th, 5.95%, 0.31% and 6.91%.
Energy spectrum analysis shows, in the electrode film of embodiment 5 Ni, Cu, Fe, P and O mass percent be respectively 64.77%,
23.51%th, 3.60%, 1.16% and 6.96%.
Energy spectrum analysis shows, in the electrode film of embodiment 6 Ni, Cu, Fe, P and O mass percent be respectively 36.46%,
51.50%th, 6.11%, 3.01% and 2.92%.
Fig. 1 is the SEM photograph for carrying out morphology observation to electrode film surface with SEM, as seen from Figure 1, electrode
Film surface recombination (hydrogen) oxide has tetrahedron and octahedral structure feature.
Fig. 2 is that, using Hg/HgO electrodes as reference electrode, platinum electrode is auxiliary using PARSTAT2273 electrochemical workstations
Electrode, the electrode prepared using embodiment 1 is working electrode, electrode bare area 1.0cm2, 2mol/L KOH solutions are electrolyte,
Potential window is 0.20-0.70V, the cyclic voltammetry curve measured using different scanning rates.From Figure 2 it can be seen that cyclic voltammetric is bent
Redox peaks on line be present, the electrode for showing to prepare is a kind of fake capacitance electrode material.
Fig. 3 is the electrode of the charging and discharging curve with SCTS electrochemical capacitance test system and tests, graphite electrode and the preparation of embodiment 1
Form two electrode systems, 2mol/L KOH solutions are electrolyte, current density 0.5mA/cm2, charge and discharge potential window is
0.00-0.70V, electrode exposed surface area are 1.0cm2, as seen from Figure 3, charging and discharging curve is in linear approximate relationship, and symmetry
It is good, there is typical capacitor electrode material charging and discharging curve feature.
Fig. 4 is the electrode of the cyclical stability with SCTS electrochemical capacitance test system and tests, graphite electrode and the preparation of embodiment 1
Form two electrode systems, 2mol/L KOH solutions are electrolyte, current density 0.5mA/cm2, charge and discharge potential window is
0.00-0.70V, electrode exposed surface area are 1.0cm2, after 3500 circulations, capacity retention still up to 98.1%, is shown
Go out excellent cyclical stability.
Fig. 5 is the SEM photograph that the electrode film surface prepared with SEM to embodiment 4 carries out morphology observation,
As seen from Figure 5, electrode film surface recombination (hydrogen) oxide is mainly tetrahedral structure, a length of submicron order of tetrahedron seamed edge.
Fig. 6 is the cyclic voltammetry curve of the electrode prepared with embodiment 2-4 heat erosion different time.Using
PARSTAT2273 electrochemical workstations, using Hg/HgO electrodes as reference electrode, platinum electrode is auxiliary electrode, with embodiment 2-4 systems
Standby electrode is working electrode, its bare area 1.0cm2, 2mol/L KOH solutions are electrolyte, sweep speed 10mV/s,
Potential window is 0.20-0.70V.As seen from Figure 6, redox peaks on cyclic voltammetry curve be present, illustrate prepared electricity
Pole film is a kind of fake capacitance electrode material.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way for above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical scheme, all fall within protection scope of the present invention.
Claims (8)
1. a kind of preparation method for the electrode of super capacitor for being covered with active electrode film, it is characterised in that comprise the following steps：
S1, substrate pretreated：Using conductive foil as matrix, conductive foil is made to oil removing, washing, pickling, washing process successively；
S2, chemical plating overlay film：Conductive foil after above-mentioned processing is placed in ambrose alloy iron phosphorus chemistry plating solution, in conductive foil coating surface
Washed after ambrose alloy ferrophosphor(us) film, collector is made；
S3, thermokalite corrosion fabricated in situ：Above-mentioned collector is immersed in potassium hydroxide solution, it is rotten that taking-up is placed in heat in baking oven
Erosion, in collection liquid surface fabricated in situ hydroxide and/or oxide composite membrane；
S4, cyclic activation：Collector after above-mentioned heat erosion is placed in potassium hydroxide solution after cyclic activation and dried, is made and covers
The electrode of super capacitor of active electrode film；
Nickel in above-mentioned steps S2 ambrose alloy ferrophosphor(us) films, copper, the mass percent of iron and phosphorus be respectively 33.74%-43.02%,
50.16%-57.58%, 1.94%-5.59% and 3.08%-4.88%；
Nickel in above-mentioned steps S4 electrode films, copper, iron, the mass percent of phosphorus and oxygen be respectively 36.46%-77.97%,
7.47%-51.50%, 4.64%-23.32%, 0.14%-3.01% and 2.93%-7.05%.
2. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, the step S4 electrode films are hydroxide and/or oxide composite membrane with tetrahedron and octahedral structure.
3. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, plating temperature is 81-83 DEG C in the step S2, Plating times 10-60min.
4. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, potassium hydroxide solution concentration is 2-20mol/L, soak time 1-5min, oven temperature 50- in the step S3
200 DEG C, etching time 1-8h.
5. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, potassium hydroxide solution concentration is 2mol/L in the step S4.
6. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, cyclic activation is 5 weeks in the step S4, and activation voltage is ± 3V, sweep speed 50mV/s.
7. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, conductive foil is the good metal or nonmetallic of electric conductivity in the step S1.
8. a kind of preparation method of electrode of super capacitor for being covered with active electrode film according to claim 1, its feature
It is, conductive foil is pure iron foil in the step S1, and size is 20 × 10 × 0.2mm.
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