CN105047432A - Super capacitor electrode and preparation method thereof - Google Patents
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- CN105047432A CN105047432A CN201510305780.5A CN201510305780A CN105047432A CN 105047432 A CN105047432 A CN 105047432A CN 201510305780 A CN201510305780 A CN 201510305780A CN 105047432 A CN105047432 A CN 105047432A
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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 relates to a super capacitor electrode and a preparation method thereof. The preparation method comprises the following steps: mixing a graphite material with an adhesive and a solvent to prepare a slurry; coating a current collector with the slurry, drying and obtaining a graphite electrode; and taking the graphite electrode as an electrode for placing into an electrolyte, and applying voltage to carry out electrochemical processing so as to obtain the super capacitor electrode, wherein the voltage should be reasonably controlled between electrolytic initial voltage and peeling voltage when the graphite electrode is under certain electrolyte conditions. According to the invention, the method abandons a manufacturing method of taking graphene as a raw material for coating in the prior art and directly takes the routine graphite material as the raw material for manufacturing the graphite electrode, such that the specific capacity of the prepared super capacitor electrode is effectively improved, the method is simple, the cost is low, and industrial application is facilitated.
Description
Technical field
The present invention relates to new energy field, particularly relate to a kind of electrode of super capacitor and preparation method thereof.
Background technology
Increasingly the deterioration of the day by day deficient and environment of traditional fossil energy resource, has impelled the development of the regenerative resource such as solar energy and wind energy.But solar energy, wind energy have fluctuation and intermittence, need effective energy storage device to ensure grid-connected work in electrical network that it can be stable.Meanwhile, the fast development of ev industry also, environmental friendliness, high-power energy management apparatus low in the urgent need to development cost.
Ultracapacitor, also electrochemical capacitor is claimed, it is a kind of electrochemical energy storage device between traditional capacitor and secondary cell, it is the electric double layer capacitance produced based on high surface area carbon electrode/electrolyte interface, or realize the storage of energy based on the redox reaction that surface and the body phase of transition metal oxide or conducting polymer occur, its capacity can reach hundreds of even several thousand farads.As a kind of Novel energy storage apparatus, ultracapacitor has that power output is high, the charging interval is short, long service life, operating temperature range are wide, safety and the advantage such as pollution-free, is expected to become novel green power supply in this century.At present, ultracapacitor is applied on hybrid-power bus, extended-range electric bus, fuel cell car, urban track traffic, pure electric automobile as energy storage component, main and other energy members (engine, storage battery, fuel cell) parallel operation, there is provided the high power of vehicle launch demand, the high power bearing braking energy feedback and big current quick charge impacts.For ultracapacitor, electrode is crucial, at present to requirement normally high-specific surface area, high conductivity and the electrochemical stability of electrode.
Existing electrode of super capacitor is made mainly through applying activated carbon, Graphene etc. on a current collector.Wherein, comparatively Graphene is poor for the electric conductivity of activated carbon, and cause capacitor series resistance comparatively large, Graphene then has excellent conductivity, pliability, mechanical property and very large specific area, and (theoretical monolayer Graphene specific area is 2630m
2/ g), self can be used as the electrode material of double electric layers supercapacitor.But no matter be Graphene, graphene oxide (GO) or redox graphene (RGO), they all easily occur stacking in preparation process, affect grapheme material dispersiveness in the electrolyte and surface wettability, reduce effective ratio area and the conductivity of grapheme material, simultaneously, due to the lamellar structure that Graphene is two dimension, therefore being made into slurry is coated in metal collector, Graphene is parallel to be often attached in metal collector, be unfavorable for transferring charge and ion diffuse, the specific capacity of the electrode of super capacitor therefore prepared is usually lower, resistance is larger.
Summary of the invention
Based on this, be necessary the preparation method that a kind of electrode of super capacitor is provided.
A preparation method for electrode of super capacitor, comprises the steps:
By graphite material and adhesive, solvent, make slurry;
Described slurry is coated collector, dry, obtain graphite electrode;
Using described graphite electrode as electrode, be placed in electrolyte, apply voltage and carry out electrochemical treatments, obtain described electrode of super capacitor, wherein, described voltage is adopted and is determined with the following method:
Using described graphite electrode as electrode, be placed in described electrolyte, carry out voltage linear scanning, correspondingly on current-voltage curve when record current-voltage curve slope absolute value graphite material starting to become on the electrolysis starting voltage of large some correspondence and described graphite electrode starts to peel off peel off voltage, described voltage is in described electrolysis starting voltage and describedly peel off value between voltage.
The preparation method of electrode of super capacitor of the present invention, abandon the manufacture method of carrying out applying using Graphene as raw material that prior art adopts usually, directly using the graphite material of routine as raw material, first make graphite electrode, under suitable voltage and electrolyte conditions, electrochemical treatments is carried out to graphite electrode again, the layer structure of the graphite material on collector can be made to produce dissociating to a certain degree, but do not come off and still preserve and collector well in electrical contact, specific area is increased.Simultaneously, owing to being dissociate directly carrying out electrochemistry in the solution after the coating on a current collector of graphite material, therefore can define an effective ion transport passage, be convenient to the ion transport in charge and discharge process, and effectively improve the specific capacity of electrode of super capacitor.
Wherein, described voltage is answered conservative control in the electrolysis starting voltage of described graphite electrode under certain electrolyte conditions and is peeled off between voltage, carries out test record especially by voltage linear scanning: described electrolysis starting voltage is tests the magnitude of voltage that the current-voltage curve slope absolute value obtained starts to become large some correspondence; Observe the state of graphite electrode in scanning process, when finding that the graphite material on graphite electrode starts to peel off, the magnitude of voltage on corresponding current-voltage curve, peels off voltage described in being.
In addition, the mode that the present invention dissociates owing to adopting original position, namely first fixes common graphite material on a current collector, and then dissociates, effectively prevent the stack-up issue in the past directly using Graphene smear.
Wherein in an embodiment, described electrolyte is H
2sO
4solution, oxalic acid solution, ionic liquid solution, Na
2sO
4solution, LiPF
6one or more in/carbonic allyl ester solution.Above-mentioned electrolyte is chosen as any concentration value, can obtain corresponding magnitude of voltage, carry out electrochemical treatments with this to graphite electrode, can prepare electrode of super capacitor of the present invention according to the defining method of voltage of the present invention.
Wherein in an embodiment, described graphite material is one or more in native graphite, pyrolytic graphite, graphitized intermediate-phase carbon microballoon, expanded graphite.
Wherein in an embodiment, the material of described collector is aluminium, nickel, carbon fiber or carbon nano-tube.Specifically can be aluminium foil, aluminium net, nickel sheet, nickel foam, nickel screen, carbon fiber paper and Buckie paper, the material of preferred described collector is aluminium, thus while electrochemical treatments is carried out to described graphite electrode, the collector region surface oxidative deactivation that also can not apply at slurry becomes the alumina layer of one deck densification, effectively can ensure larger work potential window, avoid collector by corrosion such as electrolyte simultaneously.
Wherein in an embodiment, also comprise the steps: by depositing metal oxide or conducting polymer on the graphite electrode of electrochemical method after described electrochemical treatments, and suppress.
Graphite electrode after above-mentioned electrochemical treatments, can also further by electrochemical method depositing metal oxide or conducting polymer isoreactivity material, improve its conductivity, and then carry out pressurization compacting, the existence of the active material of deposition can be played a supporting role to the graphite material of dissociation, avoids it to occur when suppressing stacking, ensure the unimpeded of ion channel, meanwhile, the resistance of the electrode after compacting obviously reduces, and further increases the specific capacity of electrode.
Wherein in an embodiment, described metal oxide is MnO
2, NiO, Co
3o
4, SnO
2, V
2o
5or RuO
2; Described conducting polymer is polypyrrole, polyaniline or polythiophene.
Wherein in an embodiment, the pressure of described compacting is 1-3MPa.
Wherein in an embodiment, described adhesive is one or more in PTFE, PVDF, PVA, CMC, SBR, polyurethane, polyacrylate; Described solvent is one or more in water, NMP, DMF, oxolane, alcohol, acetone.
Electrochemical treatments of the present invention adopt voltage mode to can be one in constant voltage, step, pulse.
The present invention also provides the preparation method of described electrode of super capacitor the electrode of super capacitor prepared.
Compared with prior art, the present invention has following beneficial effect:
The preparation method of electrode of super capacitor of the present invention, abandon the manufacture method of carrying out applying using Graphene as raw material that prior art adopts usually, directly make graphite electrode using the graphite material of routine as raw material, electrochemical treatments is carried out under suitable voltage and electrolyte conditions, make the electrode of super capacitor specific capacity for preparing high, resistance is low, and preparation method is easy simultaneously, cost is low, is convenient to commercial Application.
Graphite electrode after electrochemical treatments, can also carry out electrochemical deposition active material and pressing step, reduces the resistance of described electrode of super capacitor thus further, improves capacitance.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of graphite electrode described in embodiment 1;
Fig. 2 is the electron scanning micrograph of electrode of super capacitor described in embodiment 1;
Fig. 3 is the charging and discharging curve of electrode of super capacitor described in embodiment 1;
Fig. 4 is the charging and discharging curve of electrode of super capacitor described in comparative example 1;
Fig. 5 is the electron scanning micrograph of electrode of super capacitor described in embodiment 2;
Fig. 6 is the charging and discharging curve of electrode of super capacitor described in embodiment 2;
Fig. 7 is the electron scanning micrograph of electrode of super capacitor described in comparative example 2;
Fig. 8 is another electron scanning micrograph of electrode of super capacitor described in comparative example 2;
Fig. 9 is that embodiment 2 contrasts with the charging and discharging curve of electrode of super capacitor described in comparative example 2, wherein, the electrode charge and discharge curve (1A/g) of electrode of super capacitor described in 1-comparative example 2, the electrode charge and discharge curve (1A/g) of electrode of super capacitor described in 2-embodiment 2;
Figure 10 is the discharge and recharge correlation curve before and after electrode of super capacitor compacting described in embodiment 2, wherein, and the electrode charge and discharge curve (2A/g) of the electrode of super capacitor before 1-compacting, the electrode of super capacitor (2A/g) after 2-compacting;
Figure 11 is the charging and discharging curve of electrode of super capacitor described in embodiment 3;
Figure 12 is the charging and discharging curve of electrode of super capacitor described in embodiment 4.
Embodiment
Below in conjunction with specific embodiment, electrode of super capacitor of the present invention and preparation method thereof is described in further detail.
Embodiment 1
The preparation method of a kind of electrode of super capacitor of the present embodiment, comprises the steps:
Make graphite electrode: natural flake graphite, PVDF are mixed with 9:1 ratio, add NMP fully to stir and evenly mix and make graphite slurry, adopt coating machine, graphite slurry is spread evenly across on aluminium foil, 120 DEG C of dryings, obtain graphite electrode (electron scanning micrograph is shown in Fig. 1);
Electrochemical treatments: H put into by the graphite electrode made
2sO
4the aqueous solution (concentration is 0.5mol/L) in, under normal temperature condition, apply positive voltage 2.2V, after 5min, cleaning, namely obtain described electrode of super capacitor, its electron scanning micrograph is shown in Fig. 2.
Above-mentioned positive voltage value obtains by the following method:
Using described graphite electrode as electrode, be placed in H
2sO
4the aqueous solution in, carry out voltage linear scanning, the electrolysis starting voltage that record current-voltage curve slope absolute value starts to become large some correspondence is+1.3V, the voltage that peels off corresponding on current-voltage curve when graphite material on described graphite electrode starts to peel off is+2.5V, therefore described voltage span is positive voltage 1.3 ~ 2.5V.
At 1mol/LLi
2sO
4adopt three electrode modes (reference electrode is Ag/AgCl electrode) to carry out electrode charge and discharge test to described electrode of super capacitor in solution, find that ratio capacitance reaches 30F/g, potential windows is 1.6V, as shown in Figure 3.
Comparative example 1
By preparation method with embodiment 1, the electrode of super capacitor not carrying out described electrochemical treatments carries out electrode charge and discharge test under same condition, finds that its ratio capacitance is only 0.18F/g, and potential windows is 1.6V, as shown in Figure 4.
Contrast finds, relative to the electrode of super capacitor of comparative example 1, described in embodiment 1, the specific capacity of electrode of super capacitor adds 166 times.
Embodiment 2
Make graphite electrode: the emulsion (60%) of natural flake graphite, PTFE mixes with 9:1 (dry weight) ratio, stir and make graphite slurry, adopt coating machine, graphite slurry is spread evenly across on aluminium foil, 120 DEG C of dryings;
Electrochemical treatments: the graphite pole piece made puts into H
2sO
4the aqueous solution (concentration is 0.3mol/L) in, under normal temperature condition, apply positive voltage 3.8V (magnitude of voltage preparation method is with embodiment 1), after 5min, cleaning, namely obtains the graphite pole piece after electrochemical treatments;
Position activity material: the MnSO graphite pole piece after electrochemical treatments being inserted 0.25mol/L
4in solution, add positive voltage, deposition MnO
2, clean up, dry, obtain described electrode of super capacitor.
Electron scanning micrograph as shown in Figure 5, as can be seen from the figure MnO
2deposit on electrode uniformly.
At 1mol/LLi
2sO
4adopt three electrode modes (reference electrode is Ag/AgCl electrode) to carry out electrode charge and discharge test (1A/g) to described electrode of super capacitor in solution, find that ratio capacitance reaches 330F/g, potential windows is 1.0V, as shown in Figure 6.
Comparative example 2
Preparation method, with embodiment 2, does not carry out the electron scanning micrograph of the electrode of super capacitor of described electrochemical treatments as shown in Figure 7,8.MnO as can be seen from Figure
2deposit on graphite pole piece, but due to stress reason generation crack.Under same condition, carry out electrode charge and discharge test, discovery ratio capacitance is 45F/g, as shown in Figure 9, is only 1/7 of electrode for capacitors ratio capacitance described in embodiment 2, and equivalent series resistance is 2 times of electrode of super capacitor described in embodiment 2.
Further pressurization experiment: electrode of super capacitor described in embodiment 2 is suppressed under 2MPa, charge-discharge test (2A/g, 1mol/LLi are carried out to the pole piece before and after pressurization
2sO
4three electrode modes are adopted in solution), after finding pressurization, the equivalent series resistance of electrode of super capacitor reduces 5 times (see Figure 10).
Embodiment 3
The preparation method of a kind of electrode of super capacitor of the present embodiment, comprises the steps:
Make graphite electrode: graphitized intermediate-phase carbon microballoon, SBR emulsion are mixed with 9:1 ratio, add alcohol and fully stir and evenly mix and make graphite slurry, adopt coating machine, graphite slurry is spread evenly across on aluminium foil, 120 DEG C of dryings;
Electrochemical treatments: LiPF put into by the graphite electrode made
6in/carbonic allyl ester solution (concentration is 1mol/L), be lithium metal to electrode, under normal temperature condition, apply positive voltage 0.6V (relative to Li
+/ Li), after 5min, cleaning, namely obtains described electrode of super capacitor.
Above-mentioned positive voltage value obtains by the following method:
Using described graphite electrode as electrode, be placed in described LiPF
6in/carbonic allyl ester solution, carry out voltage linear scanning, the electrolysis starting voltage that record current-voltage curve slope absolute value starts to become large some correspondence is 0.8V, the voltage that peels off corresponding on current-voltage curve when graphite material on described graphite electrode starts to peel off is 0.4V, and described voltage span is 0.4-0.8V.
At 1mol/LLi
2sO
4adopt three electrode modes (reference electrode is Ag/AgCl electrode) to carry out electrode charge and discharge test to described electrode of super capacitor in solution, find that ratio capacitance reaches 105F/g, potential windows is 1.0V, as shown in figure 11.
Embodiment 4
The preparation method of a kind of electrode of super capacitor of the present embodiment, comprises the steps:
Make graphite electrode: expanded graphite, CMC are mixed with 9:1 ratio, add water and fully stir and evenly mix and make graphite slurry, adopt coating machine, graphite slurry is spread evenly across on aluminium foil, 120 DEG C of dryings;
Electrochemical treatments: ionic liquid solution (volumetric concentration is 50%) put into by the graphite electrode made, under normal temperature condition, after applying voltage-0.7,5min, cleaning, namely obtains described electrode of super capacitor.
Above-mentioned positive voltage value obtains by the following method:
Using described graphite electrode as electrode, be placed in described ionic liquid solution, carry out voltage linear scanning, the electrolysis starting voltage that record current-voltage curve slope absolute value starts to become large some correspondence is 0.5V, the voltage that peels off corresponding on current-voltage curve when graphite material on described graphite electrode starts to peel off is-0.8V, and described voltage value is voltage-0.8 ~ 0.5V.
At 1mol/LLi
2sO
4adopt three electrode modes (reference electrode is Ag/AgCl electrode) to carry out electrode charge and discharge test to described electrode of super capacitor in solution, find that ratio capacitance reaches 162F/g, potential windows is 1V, as shown in figure 12.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification is recorded.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for electrode of super capacitor, is characterized in that, comprises the steps:
By graphite material and adhesive, solvent, make slurry;
Described slurry is coated collector, dry, obtain graphite electrode;
Using described graphite electrode as electrode, be placed in electrolyte, apply voltage and carry out electrochemical treatments, obtain described electrode of super capacitor, wherein, described voltage is adopted and is determined with the following method:
Using described graphite electrode as electrode, be placed in described electrolyte, carry out voltage linear scanning, correspondingly on current-voltage curve when record current-voltage curve slope absolute value graphite material starting to become on the electrolysis starting voltage of large some correspondence and described graphite electrode starts to peel off peel off voltage, described voltage is in described electrolysis starting voltage and describedly peel off value between voltage.
2. the preparation method of electrode of super capacitor according to claim 1, is characterized in that, described electrolyte is H
2sO
4solution, oxalic acid solution, ionic liquid solution, Na
2sO
4solution, LiPF
6one or more in/carbonic allyl ester solution.
3. the preparation method of electrode of super capacitor according to claim 1, is characterized in that, described graphite material is one or more in native graphite, pyrolytic graphite, graphitized intermediate-phase carbon microballoon, expanded graphite.
4. the preparation method of electrode of super capacitor according to claim 1, is characterized in that, the material of described collector is aluminium, nickel, carbon fiber or carbon nano-tube.
5. the preparation method of electrode of super capacitor according to claim 1, is characterized in that, also comprises the steps: by depositing metal oxide or conducting polymer on the graphite electrode of electrochemical method after described electrochemical treatments, and suppresses.
6. the preparation method of electrode of super capacitor according to claim 5, is characterized in that, described metal oxide is MnO
2, NiO, Co
3o
4, SnO
2, V
2o
5or RuO
2; Described conducting polymer is polypyrrole, polyaniline or polythiophene.
7. the preparation method of electrode of super capacitor according to claim 5, is characterized in that, the pressure of described compacting is 1-3MPa.
8. the preparation method of the electrode of super capacitor according to any one of claim 1-7, is characterized in that, described adhesive is one or more in PTFE, PVDF, PVA, CMC, SBR, polyurethane, polyacrylate; Described solvent is one or more in water, NMP, DMF, oxolane, alcohol, acetone.
9. the electrode of super capacitor that the preparation method of the electrode of super capacitor described in any one of claim 1-8 prepares.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105702477A (en) * | 2016-04-26 | 2016-06-22 | 中国科学院微电子研究所 | Method for preparing super-capacitor electrode material based on graphene |
| CN106277221A (en) * | 2016-08-25 | 2017-01-04 | 北京理工大学 | A kind of high capacity carbon content active electrode preparation method |
| CN108573817A (en) * | 2017-03-09 | 2018-09-25 | 香港中文大学 | Tri compound flexible electrode, flexible super capacitor and their preparation method and device |
| CN109216648A (en) * | 2018-08-21 | 2019-01-15 | 中国科学院金属研究所 | Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105702477A (en) * | 2016-04-26 | 2016-06-22 | 中国科学院微电子研究所 | Method for preparing super-capacitor electrode material based on graphene |
| CN105702477B (en) * | 2016-04-26 | 2018-06-29 | 中国科学院微电子研究所 | The preparation method of super capacitance electrode material based on graphene |
| CN106277221A (en) * | 2016-08-25 | 2017-01-04 | 北京理工大学 | A kind of high capacity carbon content active electrode preparation method |
| CN108573817A (en) * | 2017-03-09 | 2018-09-25 | 香港中文大学 | Tri compound flexible electrode, flexible super capacitor and their preparation method and device |
| CN109216648A (en) * | 2018-08-21 | 2019-01-15 | 中国科学院金属研究所 | Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance |
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