CN105679548A - Electrode pad for graphene-based supercapacitor and preparation method of electrode pad - Google Patents
Electrode pad for graphene-based supercapacitor and preparation method of electrode pad Download PDFInfo
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- CN105679548A CN105679548A CN201610011998.4A CN201610011998A CN105679548A CN 105679548 A CN105679548 A CN 105679548A CN 201610011998 A CN201610011998 A CN 201610011998A CN 105679548 A CN105679548 A CN 105679548A
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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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- 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 provides an electrode pad for a graphene-based supercapacitor and a preparation method of the electrode pad. The electrode pad comprises a current collector layer and an active material layer, wherein the current collector layer is a stacked graphene layer; and the active material layer is a porous graphene layer. The preparation method comprises the following steps: (1) preparing mixed slurry containing physically stripped graphene and a carbon nanotube or/and carbon fiber; (2) preparing mixed slurry containing the graphene which is prepared by a chemical oxidation method, a pore-forming agent and the carbon nanotube or/and carbon fiber; and (3) sequentially painting the mixed slurry obtained in the step (1) and the mixed slurry obtained in the step (2) on a substrate, carrying out heating in an inert atmosphere, carrying out pickling and washing in sequence, and drying and rolling the mixed slurry to obtain the electrode pad. The active material layer of the electrode pad is in tight contact with the current collector layer, so that the interface resistance and the internal resistance of a battery can be effectively reduced; and the electrode pad has high electrolyte adsorption and storage capacities and improves the high-rate discharge performance and the energy density of the capacitor.
Description
Technical field
The present invention relates to the electrode plates of a kind of ultracapacitor, be specifically related to a kind of electrode plates for graphene-based ultracapacitor and preparation method thereof.
Background technology
In recent years, along with process of industrialization is constantly accelerated, world today's energy and environment problem increasingly serious, people are continuously increased for the demand of clean and effective and regenerative resource, and the Efficient Conversion of energy is also increasingly subject to storage pay close attention to. Ultracapacitor as important energy storage device have high power density, can fast charging and discharging, million rank long circulation lifes and the characteristic such as safe and reliable. But, current ultracapacitor has the shortcoming that energy density is relatively low, the energy density only 5～7Wh/kg of commercial activated carbon ultracapacitor. In order to meet ever increasing need, develop one of the development trend that ultracapacitor that is light and that have high-energy-density, power density and good circulation stability is new energy field.
At present, in super-capacitor pole piece processing technology, collector generally adopts metal copper foil or aluminium foil, and processing technology is to be coated in a form of slurry in metal collector by active material, and namely active material and collector realize connection between the two by binding agent. This connected mode is often not enough because of the adhesion strength of binding agent, causes that active material and collector gradually disengage in charge and discharge process, makes the internal resistance of cell be continuously increased, and cycle life shortens, the problem that battery there is also safety. Additionally due to metal collector density is relatively big, active material ratio in whole electrode can be reduced, thus limiting the further raising of battery energy density.
Summary of the invention
It is an object of the invention to provide a kind of electrode plates for graphene-based ultracapacitor and preparation method thereof, overcome the deficiencies in the prior art, the electrode plates of graphene-based ultracapacitor is obtained by the compound of Laminated Graphite alkene layer and porous graphene layer, make active material layer and current collector layers close contact, effectively reduce interface resistance and the internal resistance of cell, there is very strong electrolyte absorption and storage capacity simultaneously, improve the high-rate discharge ability of ultracapacitor, also the weight of collector in ultracapacitor is effectively reduced, improve the energy density of ultracapacitor.
To achieve these goals, the present invention takes techniques below scheme:
A kind of electrode plates for graphene-based ultracapacitor, described electrode plates comprises current collector layers and active material layer, and described current collector layers is Laminated Graphite alkene layer, and described active material layer is porous graphene layer.
First optimal technical scheme of described electrode plates, described Laminated Graphite alkene layer includes CNT or/and carbon fiber; Described porous graphene layer includes CNT or/and carbon fiber.
The mass ratio of the second optimal technical scheme of described electrode plates, the Graphene of described Laminated Graphite alkene layer and carbon fiber or CNT is 5～50:1; The mass ratio of the Graphene of described porous graphene layer and carbon fiber or CNT is 5～50:1.
3rd optimal technical scheme of described electrode plates, the Graphene of described Laminated Graphite alkene layer is the graphene film that physics peels off 1～10 layer obtained, and the carbon-to-oxygen ratio of described Graphene is more than 20; The Graphene of described porous graphene layer is the Graphene that chemical oxidization method prepares.
4th optimal technical scheme of described electrode plates, the graphene film that described physics is peeled off is monolayer, and in order to make to be formed between Laminated Graphite alkene good overlap joint, its lateral dimension is 1～100 μm, it is preferable that be of a size of 10 μm.
5th optimal technical scheme of described electrode plates, the thickness of described Laminated Graphite alkene layer is 0.5～50 μm, and the thickness of described porous graphene layer is 10～100 μm.
6th optimal technical scheme of described electrode plates, the thickness of described Laminated Graphite alkene layer is 20 μm, and the thickness of described porous graphene layer is 20 μm.
A kind of preparation method of described electrode plates, described preparation method comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: prepared solid content is the slurry of 1%～10% to the Graphene peeled off by physics or/and carbon fiber is scattered in water with CNT;
2) porous graphene slurry is prepared: the Graphene and the pore creating material that are prepared by chemical oxidization method according to the mass ratio of 1:1～5 are scattered in water, and add CNT or/and it is the slurry of 1%～10% that carbon fiber forms solid content;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, at 400～1200 DEG C of temperature, pickling and washing successively after heating 0.5～12h, after drying, roll-in obtains electrode plates.
First optimal technical scheme of described preparation method, step 1) described in slurry solid content be 2%～5%.
Second optimal technical scheme of described preparation method, step 2) described in pore creating material be the combination of one or more in potassium hydroxide, potassium oxide, potassium carbonate, sodium carbonate, sodium oxide, sodium hydroxide, metallic nickel granule, iron granule and metallic cobalt granule; The mass ratio of the Graphene that described pore creating material is prepared with chemical oxidization method is 2:1.
Step 3) described heating-up temperature preferably 800～1100 DEG C, it is most preferred that 1000 DEG C; Described heat time heating time preferably 2～4h. Heating rate during heating is 3～8 DEG C/min, it is preferable that 4～6 DEG C/min, it is most preferred that 5 DEG C/min.
Product after heating carries out pickling and filtration, to remove the metallic catalyst or activator wherein remained. The acid solution of described pickling is one or both in hydrochloric acid, sulphuric acid and nitric acid, and the dip time of described pickling is 0.5～8h, it is preferable that 1～7h, more preferably 2～6h.
Product drying after pickling and washing is preferably dried, and the temperature of described drying is 100～150 DEG C, it is preferable that 90～140 DEG C, more preferably 100～120 DEG C, and the time of described drying is 8～12h, it is preferable that 10h.
Described electrode plates is for preparing the application of graphene-based ultracapacitor.
With immediate prior art ratio, there is advantages that
1) electrode plates of the present invention, active material layer and current collector layers close contact, can effectively reduce interface resistance and the internal resistance of cell, there is very strong electrolyte absorption and storage capacity simultaneously, improve the high-rate discharge ability of ultracapacitor, also effectively reduce the weight of collector in ultracapacitor, improve the energy density of ultracapacitor;
2) the preparation method is that with metal aluminum foil, Copper Foil, pottery, glass etc. for matrix, prepare Laminated Graphite alkene and porous graphene slurry that the method utilizing layered coatings prepares electrode plates;
3) the Laminated Graphite alkene of current collector layers of the present invention is the Graphene that physics peels off prepared by graphite, and this Graphene has perfect sp2 structure, and when high-temperature process, this perfect lattice structure can not be etched by pore creating material; The porous graphene of active material layer of the present invention is the graphene oxide utilizing the method for chemical oxidation graphite to prepare, this Graphene has substantial amounts of defect, can react with pore creating material under the high temperature conditions, produce substantial amounts of gas, forming loose structure, original position etching reaction also can form substantial amounts of micropore and mesoporous simultaneously.
Accompanying drawing explanation
Fig. 1: the photo of the embodiment of the present invention 1 Laminated Graphite alkene layer;
Fig. 2: the photo of the embodiment of the present invention 1 porous graphene layer;
Fig. 3: the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 Laminated Graphite alkene layer;
Fig. 4: the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 porous graphene layer;
Fig. 5: the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 electrode plates;
Fig. 6: the ratio capacitance map of the embodiment of the present invention 1 and comparative example 1 electrode plates;
Fig. 7: the ratio resistance view of the embodiment of the present invention 1 and comparative example 1 electrode plates;
Fig. 8: the embodiment of the present invention 1 and comparative example 1 electrode plates energy density figure when 2.7V;
Fig. 9: the cycle performance figure of the embodiment of the present invention 1 and comparative example 1 electrode plates.
Detailed description of the invention
In order to be illustrated more clearly that technical scheme and technique effect, below with reference to drawings and Examples, the invention will be further described.
Embodiment 1
A kind of preparation method for the electrode plates of graphene-based ultracapacitor comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: 2.5g Graphene and 0.5g CNT that physics is peeled off preparation are scattered in 50ml water and form slurry;
2) porous graphene slurry is prepared: the 25g Graphene prepared by chemical oxidization method, 5g CNT, 50g potassium hydroxide are scattered in 100ml water formation slurry;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, 2h is heated at 800 DEG C of temperature, the soak with hydrochloric acid 2h of gained sample 1M is carried out, clean with water again, 100 DEG C of dry 10h, namely obtain electrode plates by direct for dried sample roll-in.
Fig. 1 show Laminated Graphite alkene layer (current collector layers), it can be seen that Laminated Graphite alkene layer Dispersion on surface is uniform, it does not have big defect. Porous graphene layer (active material layer) shown in Fig. 2 shows that the dispersibility of porous graphene is also better, and mechanical strength is high. The current collector layers that the present embodiment is obtained has carried out scanning electron microscope detection (SEM), as it is shown on figure 3, graphene sheet layer consistent size, is uniformly dispersed; Fig. 4 show the SEM figure of porous graphene layer, it can be seen that porous graphene layer has obvious loose structure, and this loose structure is conducive to diffusion and the transmission of electrolyte ion.Fig. 5 show the profile scanning figure of electrode plates, it can be seen that Laminated Graphite alkene layer and porous graphene layer compact siro spinning technology, it does not have depart from, and the thickness of Laminated Graphite alkene layer is approximately 20 microns simultaneously, and the thickness of porous graphene layer is also 20 microns.
Electrode plates is carried out capacity measurement,
Cs=4Ccell
As shown in Figure 6, under 1mV/s sweeps speed, the ratio electric capacity 31.2F/g (these data are the ratio electric capacity of button cell, and the ratio electric capacity of material is 124.8F/g) of ultracapacitor, to sweep speed from 1mV/s and sweep speed to 200mV/s, capability retention is 55%. Further to the test of its electrochemical impedance as it is shown in fig. 7, the resistance of electrode plates semicircle (capacitance resistance) and straight line (diffusion resistance) two parts can be included from figure. Through contrast, it will be seen that the capacitance resistance of electrode plates and diffusion resistance are due to the close contact of the satisfactory electrical conductivity of Graphene and porous graphene layer with Laminated Graphite alkene current collector layers so that internal resistance substantially reduces. Through calculating, the energy density of electrode plates is as shown in Figure 8, it is 6.8Wh/kg when 2.7V, the energy density of the electrode plates of the present embodiment energy density (5.2Wh/kg) apparently higher than the electrode plates of comparative example 1 is can be seen that from figure, main cause is probably the quality quality significantly lower than aluminium foil of Graphene, making Unit Weight, the ratio of active material is improved, so that energy density is obviously improved. Further to its loop test as it is shown in figure 9, after circulating at 10000 times, the capability retention of electrode plates is 91%, it is shown that the cycle performance that electrode plates is excellent.
Embodiment 2
A kind of preparation method for the electrode plates of graphene-based ultracapacitor comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: 5g Graphene and 0.5g CNT that physics is peeled off preparation are scattered in 80ml water and form slurry;
2) porous graphene slurry is prepared: the 30g Graphene prepared by chemical oxidization method, 5g CNT, 70g sodium hydroxide are scattered in 200ml water formation slurry;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, 1h is heated at 1000 DEG C of temperature, the soak with hydrochloric acid 2h of obtained sample 1M is carried out, clean with water again, 100 DEG C of dry 10h, namely obtain electrode plates by direct for dried sample roll-in.
Embodiment 3
A kind of preparation method for the electrode plates of graphene-based ultracapacitor comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: 5g Graphene and 0.5g CNT that physics is peeled off preparation are scattered in 90ml water and form slurry;
2) porous graphene slurry is prepared: the 100g Graphene prepared by chemical oxidization method, 5g CNT, 400g cobalt granule are scattered in 900ml water formation slurry;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, 8h is heated at 500 DEG C of temperature, the soak with hydrochloric acid 2h of gained sample 1M is carried out, clean with water again, 100 DEG C of dry 10h, namely obtain electrode plates by direct for dried sample roll-in.
Embodiment 4
A kind of preparation method for the electrode plates of graphene-based ultracapacitor comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: 5g Graphene and 0.3g carbon fiber that physics is peeled off preparation are scattered in 150ml water and form slurry;
2) porous graphene slurry is prepared: the 50g Graphene prepared by chemical oxidization method, 20g CNT, 150g nickel Granular composite form slurry in 260ml water;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, 6h is heated at 700 DEG C of temperature, the soak with hydrochloric acid 2h of obtained sample 1M is carried out, clean with water again, 100 DEG C of dry 10h, namely obtain electrode plates by direct for dried sample roll-in.
Embodiment 5
A kind of preparation method for the electrode plates of graphene-based ultracapacitor comprises the following steps:
1) Laminated Graphite alkene slurry is prepared: 5g Graphene and 0.8g carbon fiber that physics is peeled off preparation are scattered in 60ml water and form slurry;
2) porous graphene slurry is prepared: the 200g Graphene prepared by chemical oxidization method, 5g CNT, 250g sodium carbonate are scattered in 1200ml water formation slurry;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, 5h is heated at 1100 DEG C of temperature, the soak with hydrochloric acid 2h of obtained sample 1M is carried out, clean with water again, 100 DEG C of dry 10h, by direct for dried sample roll-in and electrode plates.
Comparative example 1
The 25g Graphene prepared by chemical oxidization method, 5g CNT, 50g potassium hydroxide are scattered in 100ml water formation mixed slurry; By obtained mixed slurry brushing in foil substrate, in an inert atmosphere, at 800 DEG C of temperature, heating 2h, is carried out the soak with hydrochloric acid 2h of obtained sample 1M, then cleans with water, 100 DEG C of dry 10h, namely obtain electrode plates by direct for dried sample roll-in.
Utilize the performance of electro-chemical test electrode plates, as shown in Figure 6, under 1mV/s sweeps speed, the ratio electric capacity 27F/g of ultracapacitor, sweep speed from 1mV/s and sweep speed to 200mV/s, capability retention is 51%, analyzes the capacitive property electrode plates significantly lower than embodiment 1 of the electrode plates showing this comparative example, and high rate performance is also below the electrode plates of embodiment 1. Further electrochemical impedance is tested as shown in Figure 7, the capacitance resistance of this comparative example electrode plates and diffusion resistance are all higher than embodiment 1 electrode plates as seen from the figure, main cause be probably active material contact with the interface of aluminum foil current collector substantially not as in embodiment 1 electrode slice active material layer contact with current collector layers. Through calculating, the energy density of this comparative example electrode plates as shown in Figure 8, when 2.7V, only has 5.2Wh/kg, lower than the energy density (6.8Wh/kg) of embodiment 1 electrode plates. Cycle performance be have also been made test, as it is shown in figure 9, after circulating at 10000 times, capability retention is 84%, lower than being embodiment 1 electrode plates (91%) simultaneously.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention. It should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention carries out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention. The multiple amendment of these embodiments be will be apparent from for those skilled in the art, and generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments. Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (10)
1., for an electrode plates for graphene-based ultracapacitor, described electrode plates comprises current collector layers and active material layer, it is characterised in that described current collector layers is Laminated Graphite alkene layer, and described active material layer is porous graphene layer.
2. electrode plates according to claim 1, it is characterised in that described Laminated Graphite alkene layer includes CNT or/and carbon fiber; Described porous graphene layer includes CNT or/and carbon fiber.
3. electrode plates according to claim 2, it is characterised in that the mass ratio of the Graphene of described Laminated Graphite alkene layer and carbon fiber or CNT is 5～50:1; The mass ratio of the Graphene of described porous graphene layer and carbon fiber or CNT is 5～50:1.
4. electrode plates according to claim 1, it is characterised in that the Graphene of described Laminated Graphite alkene layer is the graphene film that physics peels off 1～10 layer obtained; The Graphene of described porous graphene layer is the Graphene that chemical oxidization method prepares.
5. electrode plates according to claim 4, it is characterised in that the graphene film that described physics is peeled off is monolayer, and its lateral dimension is 1～100 μm.
6. electrode plates according to claim 1, it is characterised in that the thickness of described Laminated Graphite alkene layer is 0.5～50 μm, and the thickness of described porous graphene layer is 10～100 μm.
7. electrode plates according to claim 6, it is characterised in that the thickness of described Laminated Graphite alkene layer is 20 μm, and the thickness of described porous graphene layer is 20 μm.
8. the preparation method of electrode plates described in a claim 1, it is characterised in that said method comprising the steps of:
1) Laminated Graphite alkene slurry is prepared: prepared solid content is the slurry of 1%～10% to the Graphene peeled off by physics or/and carbon fiber is scattered in water with CNT;
2) porous graphene slurry is prepared: the Graphene and the pore creating material that are prepared by chemical oxidization method according to the mass ratio of 1:1～5 are scattered in water, and add CNT or/and it is the slurry of 1%～10% that carbon fiber forms solid content;
3) electrode plates is prepared: by step 1) and 2) gained mixed slurry is painted on matrix in succession, in an inert atmosphere, at 400～1200 DEG C of temperature, pickling and washing successively after heating 0.5～12h, after drying, roll-in obtains electrode plates.
9. preparation method according to claim 8, it is characterised in that step 1) described in slurry solid content be 2%～5%.
10. preparation method according to claim 8, it is characterized in that, step 2) described in pore creating material be the combination of one or more in potassium hydroxide, potassium oxide, potassium carbonate, sodium carbonate, sodium oxide, sodium hydroxide, metallic nickel granule, iron granule and metallic cobalt granule; The mass ratio of the Graphene that described pore creating material is prepared with chemical oxidization method is 2:1.
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| CN106475092A (en) * | 2016-11-23 | 2017-03-08 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of alumina base platinum catalyst |
| CN107342173A (en) * | 2017-07-10 | 2017-11-10 | 中国科学院宁波材料技术与工程研究所 | A kind of flexible super capacitor electrode and preparation method thereof |
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