CN105140465A - One-step method for preparing adhesive-free graphene electrode and used device - Google Patents
One-step method for preparing adhesive-free graphene electrode and used device Download PDFInfo
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- CN105140465A CN105140465A CN201510604953.3A CN201510604953A CN105140465A CN 105140465 A CN105140465 A CN 105140465A CN 201510604953 A CN201510604953 A CN 201510604953A CN 105140465 A CN105140465 A CN 105140465A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a device for preparing an adhesive-free graphene electrode. The device comprises a tank body, wherein a cathode chamber and an anode chamber are formed in the tank body and isolated by a porous isolating partition; the device further comprises a cathode plate which can be arranged in the cathode chamber and an anode plate which can be placed in the anode chamber, the cathode plate and the anode plate are connected to a physical power source through respective wires, and the cathode plate is further communicated with a stepping machine through a stepping machine guide rod. The invention further discloses a one-step method for preparing the adhesive-free graphene electrode. The device can prepare a lithium-inserted graphene electrode plate with the one-step method at the normal temperature, an adhesive used in the conventional electrode preparation process is avoided, and the material cost is saved. The used method is time-saving by comparison with a conventional preparation method, the thickness of an electrode layer is controllable, and the used device is simple in structure and lower in cost and has the potential of industrial production.
Description
Technical field
The present invention relates to a kind of one-step method and prepare the method for the Graphene electrodes of binder free and device used.
Background technology
Graphene is at present the thinnest two-dimensional material, and its size is less than 30 microns, and (conductive coefficient is about 5300Wm to have stable chemistry and macroscopic property
-1k
-1), (electron mobility is about 20000cm to excellent electronic conductivity
2v
-1s
-1) and strong mechanical strength (strength degree 42Nm
-1) etc. feature, effectively can be applied to the fields such as electronic device, stored energy, light sensing.
Lithium ion battery (LIB) is a kind of secondary cell, it mainly rely on lithium ion between a positive electrode and a negative electrode movement carry out work, be mainly used in the fields such as electronic product, the vehicles, national defense and military, space flight and aviation, energy storage.Ultracapacitor (EDLC) is a kind of electrochemical energy storage device between traditional capacitor and secondary cell, is mainly used in portable set, mobile radio communication equipment, ups system, wind power generation or solar power generation, electric automobile and the field such as hybrid power big bus and special car, track traffic and Aero-Space.And lithium-ion capacitor (LIC) adopts lithium ion battery and double electric layer capacitor mixed structure, positive pole adopts active carbon, and negative pole adopts the materials such as graphite.The height having double electric layer capacitor concurrently exports, the characteristic of long-life characteristics and lithium ion battery high-energy-density.
At present Graphene is mainly prepared graphene oxide by Hummer method, then obtain redox Graphene by chemical reduction method or thermal reduction, such as patent CN102502612B; By adhering on electrode current collecting body with mixing of binding agent when being applied in LIB, EDLC, LIC, such as patent CN103515110A, CN104211047A, CN103663432A.
Summary of the invention
First technical problem to be solved by this invention is, provides a kind of device that can be used for one-step method and prepare the Graphene electrodes of binder free, and this apparatus structure is simple, easy to use.
For solving above technical problem, the present invention for the preparation of the device of the Graphene electrodes of binder free,
Comprising cell body, in cell body, be provided with the anode chamber of cathode chamber and belt stirrer, being separated by porousness insulating barrier (being namely arranged with a certain amount of through hole on insulating barrier, the duct as passing through for Graphene) between cathode chamber and anode chamber;
Also comprise the cathode sheets that can be placed in cathode chamber and the anode strip that can be placed in anode chamber, described cathode sheets and anode strip are connected to physical power source by respective wire, and cathode sheets is also communicated with stepper by stepper guide rod.
Further, the thickness of described cell body is 5mm-10mm, be made up of the material of resistance to organic corrosion, be specially in polytetrafluoroethylene (PTFE), polypropylene (PP), polyvinyl chloride (PVC), Kynoar (PVDF), polyethylene (PE) or RPP (RPP) any one.
Further, described blender is any one in mechanical agitator, magnetic stirring apparatus or air-flow stirring device.
Further, described porousness insulating barrier is any one in ultra-fine fibre glass (10-G) dividing plate, polyvinyl chloride (PVC) dividing plate or polypropylene (PP) dividing plate, and the aperture in its duct is 20 μm-25 μm.
Further, described cathode sheets thickness is 10 μm-50 μm, and material is any one in copper, nickel or stainless steel.
Further, described anode strip is insoluble anode, is specially any one in stainless steel, graphite flake, platinum anode, titanium plate, titanium net, DSA Ni―Ti anode.Described anode strip thickness is 100 μm of-3mm.
Further, the voltage range of described physical power source is 10-300V, and described stepper is five-phase induction motor (0.36 degree/0.72 degree).
Second technical problem to be solved by this invention is, provides a kind of method utilizing aforementioned means to carry out one-step method to prepare the Graphene electrodes of binder free, and the method is simple and easy to realize, and saves time.
The method comprises the steps:
(1), anode strip and cathode sheets are put into respectively anode chamber and the cathode chamber of cell body, cathode sheets is close to porousness insulating barrier; Wire is connected to physical power source, is communicated with the stepper guide rod of cathode sheets to stepper;
(2), quantitative lithium salts to be joined in organic solvent and after ultrasonic mixing, to be transferred in cathode chamber; By quantitative graphite alkene (technical grade powder, lamella size < 30 μm, lamellar spacing < 5nm.) to add in organic solvent and after ultrasonic mixing, to add in anode chamber and turn on agitator, stirring means adopts the one in mechanical mixing method, magnetic agitation method or gas bubble method, and wherein adopting during gas bubble method is the stirring of inert gas method adopting nitrogen; Lithium salts and Graphene should be consistent when selecting solvent.
(3), open physical power source, the step angle of stepper be set, Graphene by behind the duct of porousness insulating barrier to be under the lithium salts effect in electric field pin deposition surperficial to cathode sheets;
(4), under the promotion of stepper, cathode sheets slowly leaves porousness insulating barrier, and meanwhile, Graphene constantly increases in the height of deposition on cathode sheets surface, the pillared Graphene line of shape; Along with leaving of cathode sheets and increasing of Graphene line, lithium salts in cathode chamber is deposited into other site deposition position of cathode sheets under electric field action simultaneously, namely do not occupied by lithium salts by the position that Graphene occupies in the deposition side of cathode sheets, lithium salts embeds between Graphene line, forms embedding lithium structure;
Lithium salts can deposit to negative electrode in the electric field, and Graphene itself is uncharged, cannot displacement in the electric field, when Graphene by the duct of porousness insulating barrier close to cathode sheets time, under the drive of lithium salts, Graphene is deposited in cathode sheets, namely Graphene according to duct pin deposition in cathode sheets, lithium salts then major sedimentary to other deposition site.
By the stirring of blender, Graphene in anode chamber constantly pours into porousness insulating barrier, and through duct, cathode sheets is under the slowly induced effect of stepper, leave porousness insulating barrier with nano level translational speed per minute, the deposit thickness of embedding lithium structure constantly increases.
(5), when the thicknesses of layers in cathode sheets reaches 50-150 μm, close physical power source and stepper, obtain the Graphene electrodes sheet of embedding lithium.
Further, organic solvent described in step (2) is the organic solvent of boiling point lower than the nontoxic or low toxicity of 200 DEG C, and the selection of lower boiling organic solvent, is convenient to the drying process of later stage negative plate.
Further, organic solvent described in step (2) is a kind of or any two kinds or the mixture two or more arbitrarily in ethanol, isopropyl alcohol, acetone or butanone.
Further, step (2) described lithium salts is a kind of or any two kinds or the mixture two or more arbitrarily in cobalt acid lithium, lithium titanate, lithium molybdate, LiMn2O4, lithium nickelate, LiFePO4, lithium nickel cobalt dioxide, nickel ion doped or nickle cobalt lithium manganate.
After adopting above technical scheme, the present invention at least has following beneficial effect:
(1) the Graphene electrodes sheet, adopting device of the present invention can carry out one-step method at normal temperatures to prepare embedding lithium, avoid the use of binding agent in traditional electrode preparation process, not only save material cost, and the internal resistance of the lithium ion battery of the Graphene electrodes sheet applying this embedding lithium, lithium-ion capacitor, ultracapacitor can be reduced in theory.
(2), one-step method preparation process of the present invention saves time than traditional preparation methods, and controlled to the thickness of electrode layer, adds that equipment therefor structure is simple, cost is lower, has the potentiality of suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of device cathode sheets of the present invention when being close to porousness insulating barrier;
Fig. 2 is that device cathode sheets of the present invention leaves the schematic diagram after being close to porousness insulating barrier;
Fig. 3 is the structural representation of Graphene line cathode sheets depositing column;
Fig. 4 is the structural representation of lithium intercalated graphite alkene layer in cathode sheets.
In figure, 1-cell body; 11-cathode chamber; 12-anode chamber; 2-cathode sheets; 21-Graphene line; The embedding lithium structure of 22-; 3-anode strip; 4-porousness insulating barrier; 5-physical power source; 6-stepper; 7-wire; 8-stepper guide rod.
Embodiment
Embodiment 1: the device preparing the Graphene electrodes of binder free for one-step method
As shown in Figure 1 or 2, the inventive system comprises cell body 1, be provided with cathode chamber 11 and belt stirrer (blender is not shown in figures) anode chamber 12 in cell body 1, separated by porousness insulating barrier 4 between cathode chamber 11 and anode chamber 12;
The present invention also comprises the cathode sheets 2 that can be placed in cathode chamber 11 and the anode strip 3 that can be placed in anode chamber 12, described cathode sheets 2 and anode strip 3 are connected to physical power source 5 corresponding end by respective wire 7, cathode sheets 2 is also communicated with stepper 6 by stepper guide rod 8, and the stepper guide rod 8 being specially stepper 6 connects the wire 7 in cathode sheets 2.
Be more than the basic comprising of device of the present invention, wherein, in the present embodiment:
The thickness of cell body 1 is 5mm, is made up of the polytetrafluoroethylene (PTFE) of resistance to organic corrosion.
Porousness insulating barrier 4 is polyvinyl chloride (PVC) dividing plate, and the aperture in its duct is 20-25 μm.Cathode sheets 2 thickness is 10 μm, and material is copper.
Anode strip 3 is platinum anode, and thickness is 100 μm.
The voltage range of physical power source 5 is 10-300V, and stepper 6 is five-phase induction motor.
Embodiment 2: the device preparing the Graphene electrodes of binder free for one-step method
As different from Example 1, the thickness of cell body 1 is 10mm, is made up of polypropylene (PP) material of resistance to organic corrosion.
Porousness insulating barrier 4 is ultra-fine fibre glass (10-G), and the aperture in its duct is 20-25 μm μm.
Cathode sheets 2 thickness is 30 μm, and material is stainless steel.
Anode strip 3 is graphite flake, and thickness is 2mm.
The voltage range of physical power source 5 is 10-300V, and described stepper 6 is five-phase induction motor.
Embodiment 3: the device preparing the Graphene electrodes of binder free for one-step method
As different from Example 1, the thickness of cell body 1 is 8mm, is made up of polyvinyl chloride (PVC) material of resistance to organic corrosion.
Porousness insulating barrier 4 is polyvinyl chloride (PVC) dividing plate, and the aperture in its duct is 20-25 μm μm.
Cathode sheets 2 thickness is 50 μm, and material is nickel.
Anode strip 3 is DSA Ni―Ti anode (titanium net), and thickness is 800 μm.
The voltage range of physical power source 5 is 10-300V, and described stepper 6 is five-phase induction motor.
Embodiment 4: one-step method prepares the Graphene electrodes of binder free
Adopt the device of enforcement 1.
The present embodiment adopts one-step method to prepare the method for the Graphene electrodes of binder free, comprises the steps:
(1), by anode strip 3 and cathode sheets 2 put into anode chamber 12 and the cathode chamber 11 of cell body 1 respectively, cathode sheets 2 is close to porousness insulating barrier 4 (as shown in Figure 1); Wire 7 is connected to physical power source 5, is communicated with the stepper guide rod 8 of cathode sheets 2 to stepper 6;
(2), by cobalt acid lithium to be added in ethanol (cobalt acid lithium/ethanol=1mol/L) after ultrasonic mixing, to be transferred in cathode chamber 11; Graphene (lamella size < 30 μm, lamellar spacing < 5nm) to be added in ethanol (10g/L) and after ultrasonic mixing, to add in anode chamber 12 and to adopt nitrogen gas stirring;
(3), open physical power source 5 (regulation voltage is 80V), the step angle arranging stepper 6 is 0.36 degree, Graphene by behind the duct of porousness insulating barrier 4 to be under the lithium salts effect in electric field pin deposition surperficial to cathode sheets 2;
(4), under the promotion of stepper 6, cathode sheets 2 slowly leaves porousness insulating barrier 4 (as shown in Figure 2), meanwhile, Graphene constantly increases in the height of deposition on cathode sheets 2 surface, forms the structure (as shown in Figure 3) being similar to Graphene line 21; Along with leaving of cathode sheets 2 and increasing of Graphene line 21, the cobalt acid lithium in cathode chamber 11 deposits other deposition site on Zhiyin pole piece 2 simultaneously under electric field action, embeds between Graphene line 21, forms embedding lithium structure 22; Porousness insulating barrier 4 is slowly left in the promotion of the deposition of Graphene on cathode sheets 2 surface, stepper 6, cathode sheets 2, occupy (the embedding lithium) of lithium salts is synchronously carrying out.
(5), close physical power source 5 and stepper 6, obtain the Graphene electrodes sheet (as shown in Figure 4) of embedding lithium.
Embodiment 5: one-step method prepares the Graphene electrodes of binder free
Adopt the device of enforcement 2.
As different from Example 4,
In step (2), lithium nickelate and lithium nickel cobalt dioxide (with mol ratio 1:1 mixing) are joined in isopropyl alcohol (lithium salts/isopropyl alcohol=0.1mol/L) ultrasonic mix after, be transferred in cathode chamber 11; Graphene (lamella size < 30 μm, lamellar spacing < 5nm) to be added in isopropyl alcohol (10g/L) and after ultrasonic mixing, to add in anode chamber 12, and adopt magnetic agitation.
The voltage of step (3) physical power source 5 is set to 280V.
The step angle of stepper 6 is set to 0.72 degree.
Embodiment 6: one-step method prepares the Graphene electrodes of binder free
Adopt the device of enforcement 3.
As different from Example 4,
In step (2), LiFePO4 is infiltrated in butanone (LiFePO4/butanone=0.5mol/L) ultrasonic mix after, be transferred in cathode chamber 11; By Graphene (lamella size < 30 μm, lamellar spacing < 5nm) to add in butanone (10g/L) and after ultrasonic mixing, to add in anode chamber 12 and to adopt mechanical agitation to stir.
The voltage of step (3) physical power source 5 is set to 150V.
The step angle of stepper 6 is set to 0.72 degree.
Claims (13)
1., for the preparation of a device for the Graphene electrodes of binder free, it is characterized in that this device
Comprise cell body (1), be provided with the anode chamber (12) of cathode chamber (11) and belt stirrer in cell body (1), separated by porousness insulating barrier (4) between cathode chamber (11) and anode chamber (12);
Also comprise the cathode sheets (2) that can be placed in cathode chamber (11) and the anode strip (3) that can be placed in anode chamber (12), described cathode sheets (2) and anode strip (3) are connected to physical power source (5) by respective wire (7), and cathode sheets (2) is also communicated with stepper (6) by stepper guide rod (8).
2. the device of the Graphene electrodes for the preparation of binder free according to claim 1, is characterized in that: the thickness of described cell body (1) is 5mm-10mm, is made up of the material of resistance to organic corrosion.
3. the device of the Graphene electrodes for the preparation of binder free according to claim 2, is characterized in that: the material of the resistance to organic corrosion of described making cell body (1) is any one in polytetrafluoroethylene, polypropylene, polyvinyl chloride, Kynoar, polyethylene or RPP.
4. the device of the Graphene electrodes for the preparation of binder free according to claim 1, is characterized in that: described blender is any one in mechanical agitator, magnetic stirring apparatus or air-flow stirring device.
5. the device of the Graphene electrodes for the preparation of binder free according to claim 1, it is characterized in that: described porousness insulating barrier (4) is superfine glass fibre partition board, any one in polyvinyl chloride dividing plate or polypropylene separator, and the aperture in its duct is 20 μm-25 μm.
6. the device of the Graphene electrodes for the preparation of binder free according to claim 1, is characterized in that: described cathode sheets (2) thickness is 10 μm-50 μm, and material is any one in copper, nickel or stainless steel.
7. the device of the Graphene electrodes for the preparation of binder free according to claim 1, is characterized in that: described anode strip (3) is insoluble anode, and thickness is 100 μm of-3mm.
8. the device of the Graphene electrodes for the preparation of binder free according to claim 7, is characterized in that: described anode strip (3) is stainless steel, any one in graphite flake, platinum anode, titanium plate, titanium net, DSA Ni―Ti anode.
9. the device of the Graphene electrodes for the preparation of binder free according to claim 1, is characterized in that: the voltage range of described physical power source (5) is 10-300V, and described stepper (6) is five-phase induction motor.
10. the method utilizing the device described in claim 1-9 any one claim to carry out one-step method to prepare the Graphene electrodes of binder free, is characterized in that the method comprises the steps:
(1), by anode strip (3) and cathode sheets (2) put into anode chamber (12) and the cathode chamber (11) of cell body (1) respectively, cathode sheets (2) is close to porousness insulating barrier (4); Wire (7) is connected to physical power source (5), is communicated with the stepper guide rod (8) of cathode sheets (2) to stepper (6);
(2), by quantitative lithium salts to join in organic solvent and after ultrasonic mixing, to be transferred in cathode chamber (11); Quantitative graphite alkene to be added in organic solvent and after ultrasonic mixing, to add in anode chamber (12) and turn on agitator;
(3), physical power source (5) is opened, the step angle of stepper (6) is set, Graphene by behind the duct of porousness insulating barrier (4) to be in pin deposition under the lithium salts effect in electric field surperficial to cathode sheets (2);
(4), under the promotion of stepper (6), cathode sheets (2) slowly leaves porousness insulating barrier (4), simultaneously, Graphene constantly increases in the height of deposition on cathode sheets (2) surface, the pillared Graphene line (21) of shape; Along with leaving of cathode sheets (2) and increasing of Graphene line (21), lithium salts in cathode chamber (11) is deposited into cathode sheets (2) other deposition site under electric field action simultaneously, forms embedding lithium structure (22);
(5), when the thicknesses of layers in cathode sheets (2) reaches 50-150 μm, close physical power source (5) and stepper (6), obtain the Graphene electrodes sheet of embedding lithium.
11. one-step method according to claim 10 prepare the method for the Graphene electrodes of binder free, it is characterized in that: organic solvent described in step (2) is the organic solvent of boiling point lower than the nontoxic or low toxicity of 200 DEG C.
12. one-step method according to claim 11 prepare the method for the Graphene electrodes of binder free, it is characterized in that: organic solvent described in step (2) is a kind of or any two kinds or mixtures two or more arbitrarily in ethanol, isopropyl alcohol, acetone or butanone.
13. one-step method according to claim 10 prepare the method for the Graphene electrodes of binder free, it is characterized in that: step (2) described lithium salts is a kind of or any two kinds or mixtures two or more arbitrarily in cobalt acid lithium, lithium titanate, lithium molybdate, LiMn2O4, lithium nickelate, LiFePO4, lithium nickel cobalt dioxide, nickel ion doped or nickle cobalt lithium manganate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106206046A (en) * | 2016-07-31 | 2016-12-07 | 肖丽芳 | A kind of Graphene is combined Li2moO3the preparation method of positive electrode |
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| JP2012224526A (en) * | 2011-04-21 | 2012-11-15 | Hiroshima Univ | Method for producing graphene |
| CN103903878A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Graphene electrode plate and preparing method thereof |
| CN205004385U (en) * | 2015-09-21 | 2016-01-27 | 上海展枭新能源科技有限公司 | A device for preparing binderless's graphite alkene electrode |
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| JP2012224526A (en) * | 2011-04-21 | 2012-11-15 | Hiroshima Univ | Method for producing graphene |
| CN103903878A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Graphene electrode plate and preparing method thereof |
| CN205004385U (en) * | 2015-09-21 | 2016-01-27 | 上海展枭新能源科技有限公司 | A device for preparing binderless's graphite alkene electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106206046A (en) * | 2016-07-31 | 2016-12-07 | 肖丽芳 | A kind of Graphene is combined Li2moO3the preparation method of positive electrode |
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Effective date of registration: 20220615 Address after: 333000 north of Zhihang Road, high tech Zone, Changjiang District, Jingdezhen City, Jiangxi Province (within Jingdezhen Weihang Technology Co., Ltd.) Patentee after: Jiangxi Zhanxiao New Energy Technology Co.,Ltd. Address before: 201199 room C307, huilide Industrial Park, No. 1-7, Lane 1356, Xinyuan Road, Minhang District, Shanghai Patentee before: SHANGHAI CAPENERGY TECHNOLOGY Co.,Ltd. |