CN111525086A - Preparation method of lithium battery electrode based on laser shock technology - Google Patents
Preparation method of lithium battery electrode based on laser shock technology Download PDFInfo
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- CN111525086A CN111525086A CN202010339417.6A CN202010339417A CN111525086A CN 111525086 A CN111525086 A CN 111525086A CN 202010339417 A CN202010339417 A CN 202010339417A CN 111525086 A CN111525086 A CN 111525086A
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
- B23K26/356—Working by laser beam, e.g. welding, cutting or boring for surface treatment by shock processing
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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 preparation method of a lithium battery electrode based on laser shock, which is characterized in that an absorption layer and a restraint layer are laid on the surface of a copper foil for laser treatment; adding silicon nanoparticles and polyvinylpyrrolidone into ethanol for end capping to obtain stable silicon nanoparticle dispersion liquid; dripping silicon nanoparticle dispersion liquid on the pretreated copper foil, drying, dripping graphene oxide dispersion liquid, and sequentially circulating; and carrying out ultrasonic impact treatment on the test piece subjected to the dripping coating, then paving an absorption layer and a constraint layer on the surface, carrying out laser treatment, and finally carrying out annealing treatment to obtain the lithium battery electrode. The invention provides a preparation method of a lithium battery electrode which is environment-friendly, strong in controllability and large in battery capacity.
Description
Technical Field
The invention relates to a lithium battery electrode preparation method based on a laser shock technology, and belongs to the field of battery electrode manufacturing.
Background
The lithium ion battery is widely applied to electronic products, military products and aerospace products as a battery with high energy density, long service life and high output power. The lithium battery electrode, particularly the anode, has a great influence on the maximum performance of the lithium ion battery. The elemental silicon and graphene have excellent conductivity and are often used as electrode materials of batteries.
Silicon is a common element, often exists in nature in the form of silicate or silicon dioxide, and simple substance silicon is a good semiconductor material, is often used for manufacturing electric elements such as transistors, photocells, chips and the like, and is a widely used anode material. However, the silicon-based material expands greatly during charging and discharging, so that the electrode is powdered, the battery capacity is reduced rapidly, and the battery is disabled. Graphene is a light two-dimensional material discovered in recent years, has the advantages of good electronic conductivity, high mechanical strength, excellent heat conduction performance, good optical performance and the like, and is widely applied to the fields of batteries, sensors and the like. Graphene with good mechanical stability and high conductivity can be used as an electrode matrix, and the electrochemical performance of the electrode is improved. Therefore, the combination of graphene and silicon nanoparticles (SiNPs) will effectively solve the disadvantages of silicon substrate electrodes.
How to combine graphene and silicon nanoparticles is a key issue. Random mixing of the two would result in a large amount of silicon nanoparticle aggregates, resulting in poor uniformity of the composite and reduced battery capacity; the high specific surface area of the silicon nanoparticles requires the use of a high weight ratio of inert polymer binder for bonding, which significantly reduces the specific capacity of the battery and increases cost. Therefore, it is necessary to invent a new technology for combining graphene and silicon nanoparticles.
Laser machining techniques are widely used in the manufacturing field. Laser processing techniques are mainly classified into two major categories, one category is processing techniques using Laser thermal effects, including Laser Welding (LW), Laser Cutting (LC), Laser Surface Texturing (LST), Laser thermoforming (LF), and the like; the other type is a processing technology using a Laser force effect, including Laser Shock Peening (LSP), Laser Shock Forming (LSF), Laser Shock Texturing (LPT), and the like, and these technologies are all based on a Laser Shock technology. The laser shock technique is a processing technique for plastically deforming a material using a shock wave generated by an intense laser beam. The laser impact technology utilizes the force effect of laser, and can effectively avoid the defect caused by the influence of the heat effect. This technique has a significant advantage: under the action of transient huge laser impact pressure, the surface and the subsurface of the material generate grain refining effect, and a deeper residual compressive stress layer is formed, so that the mechanical and physical properties of the material are enhanced. The laser impact technology is utilized to combine the graphene and the silicon nano particles to prepare the battery electrode, and the preparation method is a brand new preparation method.
At present, the preparation methods of the relevant lithium battery electrode and the relevant materials can be searched, such as the invention named as "a preparation method of silicon/folded graphene electrode material" (patent number: ZL201811228460.4), and the electrode material preparation process is as follows: adding silicon-aluminum alloy particles into the graphene oxide solution, and performing suction filtration to obtain a composite film; and adding the film into dilute hydrochloric acid for reaction, taking out and drying, reducing graphene oxide by using a hydriodic acid solution, and finally cleaning by using ethanol to obtain the silicon/folded graphene electrode material. The method can effectively improve the charging performance and the electricity storage performance of the lithium battery, and the space between the folded graphene and the silicon particles can be compressed, so that the volume expansion of silicon can be effectively buffered. For another invention named as "a carbon-silicon material for lithium ion battery negative electrode and its preparation method" (patent number: ZL201810378656.5), the electrode material preparation process is as follows: firstly, cleaning silicon powder by using dilute hydrochloric acid, then, putting the silicon powder into a mixed solution of AgNO3 and HF, plating Ag of nano particles on the surface of the silicon, and then, putting the silicon powder into a mixed solution of HF and H2O2 for reaction to obtain silicon with a pore structure; then preparing a carbonization precursor of the carbon-silicon material by an electrostatic spinning technology; and finally, oxidizing and sintering the carbonized precursor to obtain the carbon-silicon electrode material. The method can improve the conductivity and enhance the initial efficiency and the cycle stability of the lithium ions, but the method has the disadvantages of complicated steps, complex process and more chemical reagents. In another example of the invention named as "method for manufacturing lithium ion battery electrode based on selective melting technology" (patent No. ZL201711252278.8), the electrode manufacturing process is as follows: and (2) uniformly pre-arranging aluminum-silicon powder on a copper current collector, cladding the aluminum-silicon powder by using a selective laser melting technology to prepare an electrode precursor, and then removing element aluminum in precursor alloy by using a dealloying technology to obtain a porous silicon structure metallurgically combined with the current collector, thereby completing the preparation of the electrode. The manufacturing method is mature and simple in technology and low in cost, but the laser cladding technology is adopted, so that a heat affected zone exists, and the performance of the electrode is influenced to a certain extent. Therefore, a new method which is simple in process, green and environment-friendly and has good performance of the prepared electrode needs to be invented.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the technical problem that the lithium battery prepared by the existing preparation method of the lithium battery electrode based on the laser shock technology is poor in click performance is solved.
In order to solve the technical problem, the invention provides a preparation method of a lithium battery electrode based on a laser shock technology, which is characterized by comprising the following steps of:
step 1): laying an absorption layer on the surface of the clean copper foil; laying a restraint layer above the absorption layer, carrying out laser treatment, enabling laser beams to be absorbed by the absorption layer through the restraint layer, then generating plasma explosion to form shock waves, and punching the copper foil to form a micro-pit array to obtain a pretreated copper foil;
step 2): adding silicon nano particles and polyvinylpyrrolidone into ethanol for end capping under magnetic stirring, centrifugally cleaning the end-capped silicon nano particles, and removing excessive polyvinylpyrrolidone to obtain a stable silicon nano particle dispersion liquid;
step 3): placing graphene oxide in water, carrying out ultrasonic treatment to obtain a graphene oxide dispersion liquid, and diluting the dispersion liquid with ethanol according to production requirements;
step 4): dripping silicon nanoparticle dispersion liquid on the pretreated copper foil, drying, dripping graphene oxide dispersion liquid, and circularly dripping two kinds of dispersion liquid in sequence, wherein the circulation times are determined according to production requirements;
step 5): carrying out ultrasonic impact treatment on the test piece subjected to dropping coating, reducing the distance between the silicon nano particles and the graphene oxide, and increasing the contact area between the silicon nano particles and the graphene oxide;
step 6): laying an absorption layer on the surface of the test piece subjected to ultrasonic impact, laying a restraint layer above the absorption layer, performing laser treatment, allowing laser beams to penetrate through the restraint layer and be absorbed by the absorption layer, and then generating plasma explosion to form shock waves, so that the contact area between the silicon nano particles and the graphene oxide is further increased;
step 7): and annealing the test piece subjected to laser impact in a protective gas environment to obtain the lithium battery electrode.
Preferably, the absorption layer in step 1) is black paint or black polytetrafluoroethylene tape, and the function of the absorption layer is to absorb laser energy to generate plasma and form shock waves.
Preferably, the constraint layer in step 1) is water or optical glass, and the function of the constraint layer is to increase the amplitude of the laser impact pressure and prolong the pressure action time.
Preferably, the laser beam in the step 1) is generated by a laser, and the laser adopts a high-power Q-switched Nd: YAG laser.
Preferably, the laser beam in step 1) and step 6) is transmitted through the constraint layer after being changed in transmission direction by an optical device and focused, and then is absorbed by the absorption layer.
Preferably, the ratio of the silicon nanoparticles, the polyvinylpyrrolidone and the ethanol in the step 2) is 1 g: 5 g: 100 mL.
Preferably, the temperature of the end-capping reaction in the step 2) is 70 ℃.
Preferably, the washing in step 2) is performed by using ethanol for multiple times.
Preferably, the protective gas in step 7) is an inert gas.
Preferably, the process parameters of the annealing treatment in the step 7) are as follows: 600 ℃ for 2 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention provides a battery electrode preparation method based on a laser shock technology, which is a brand new processing technology; compared with the existing processing technology, the invention adopts the laser impact technology as the main processing means, and has the advantages of strong controllability, environmental friendliness and the like.
(2) According to the invention, the micro-pit array is punched on the copper foil by the first laser shock treatment, the specific surface area of the copper foil is obviously increased, and more silicon nano particles can be borne; the second laser shock treatment can further reduce the distance between the silicon nano particles and the graphene oxide and increase the contact area of the silicon nano particles and the graphene oxide; the two laser shock treatments can greatly increase the capacity of the battery.
(3) Certain gaps exist between the silicon nanoparticles and the graphene oxide sheets, and can help to relieve stress caused by volume expansion of silicon.
(4) In the impact process of the sample, the graphene oxide will generate defects (such as holes, cracks and the like) to a certain extent, which is helpful for lithium ions to penetrate through the graphene oxide, and improves the conductivity of the electrode.
Drawings
FIG. 1 is a flow chart of pretreatment in the preparation method provided by the present invention;
FIG. 2 is a flow chart of a dispensing process in the manufacturing method provided by the present invention;
FIG. 3 is a flow chart of the main processing technology of the preparation method provided by the invention;
FIG. 4 is a microscopic variation of the drop coating;
fig. 5 is a schematic illustration of a laser shock process.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Examples
A preparation method of a lithium battery electrode based on a laser shock technology comprises the following steps:
step 1: laying an absorption layer 4 (black polytetrafluoroethylene tape) on the surface of the clean copper foil 1; laying a layer of restraint layer 3 (water) above the absorption layer 4; fixing the test piece paved with the absorption layer 4 and the restraint layer 3 on a clamp 5 of a six-axis robot 21; determining various parameters of laser shock according to a production scheme; a laser 24 (Q-switched Nd: YAG laser) is used for outputting a laser beam 5, the laser firstly changes the transmission direction through an optical device 22 and is focused, then the laser is absorbed by an absorption layer 4 through a constraint layer 3, plasma explosion is generated to form shock waves, and a micro-pit array is formed on a copper foil 1 in an impact mode, so that a pretreated copper foil 6 is obtained (as shown in figure 1, an arrow above the constraint layer 3 is the moving direction of a test piece in the figure);
step 2: adding silicon nano particles and polyvinylpyrrolidone (PVP) into an ethanol solution, and placing the solution in an environment of 70 ℃ for PVP end capping under the condition of magnetic stirring; centrifuging the end-capped silicon nanoparticles and washing the end-capped silicon nanoparticles with ethanol for several times to remove excessive PVP to obtain a stable silicon nanoparticle dispersion liquid 8; wherein the proportion of the silicon nanoparticles, the polyvinylpyrrolidone and the ethanol is 1 g: 5 g: 100 mL;
and step 3: placing graphene oxide in water, carrying out ultrasonic treatment for 2 hours to obtain graphene oxide dispersion liquid 10, and diluting the dispersion liquid with ethanol according to production requirements;
and 4, step 4: dripping silicon nanoparticle dispersion liquid 8 on the pretreated copper foil 6 obtained in the step 1 to obtain a test piece 9, dripping graphene oxide dispersion liquid 10 on the test piece 9 after drying, sequentially and circularly dripping the two dispersion liquids, determining the number of circulation times according to production requirements, and finally obtaining a test piece 13 (shown in figure 2) which is finished in dripping coating and is finished in dripping coating;
and 5: placing the test piece 13 subjected to the dropping coating on a workbench 15 of an ultrasonic impact device for ultrasonic impact treatment, reducing the distance between the silicon nanoparticles 19 and the graphene oxide 20, and increasing the contact area between the silicon nanoparticles and the graphene oxide (as shown in A in FIG. 4);
step 6: laying an absorption layer 4 (black polytetrafluoroethylene tape) on the surface of the test piece 16 subjected to ultrasonic impact, and laying a restraint layer 3 (water) above the absorption layer 4; fixing the test piece paved with the absorption layer 4 and the constraint layer 3 on a clamp 5 of a six-axis robot 21, outputting a laser beam 2 by using a laser 24 (the laser 24 is arranged on a precise optical shock insulation table 23, and a Q-switched Nd: YAG laser), wherein the laser firstly changes the transmission direction through an optical device 22 and focuses, then is absorbed by the absorption layer 4 through the constraint layer 3 to generate plasma explosion to form shock waves, and further increases the contact area between the silicon nanoparticles 19 and the graphene oxide 20 to obtain a test piece 17 after laser impact (the process is shown as B in figures 3 and 4, the device is shown as figure 5, and the arrows above the test piece 13 and the constraint layer 3 which are coated in the figure 3 are the moving direction of the test piece);
step 7: under the protection of nitrogen gas, the test piece 17 after laser impact is transferred to a furnace at 600 ℃ for annealing treatment for 2 hours, and finally the required lithium battery electrode 18 is obtained.
Claims (10)
1. A preparation method of a lithium battery electrode based on a laser shock technology is characterized by comprising the following steps:
step 1): laying an absorption layer (4) on the surface of the clean copper foil (1); laying a layer of restraint layer (3) above the absorption layer (4), carrying out laser treatment, enabling the laser beam (2) to be absorbed by the absorption layer (4) through the restraint layer (3), then generating plasma explosion to form shock waves, and punching the copper foil (1) to form a micro-pit array to obtain a pretreated copper foil (6);
step 2): under magnetic stirring, adding silicon nanoparticles and polyvinylpyrrolidone into ethanol for end capping, centrifugally cleaning the end-capped silicon nanoparticles, and removing excessive polyvinylpyrrolidone to obtain a stable silicon nanoparticle dispersion liquid (8);
step 3): placing graphene oxide in water, carrying out ultrasonic treatment to obtain a graphene oxide dispersion liquid (10), and diluting the dispersion liquid with ethanol according to production requirements;
step 4): dripping silicon nanoparticle dispersion liquid (8) on the pretreated copper foil (6), dripping graphene oxide dispersion liquid (10) after drying, and circularly dripping two kinds of dispersion liquid in sequence, wherein the circulation times are determined according to production requirements;
step 5): carrying out ultrasonic impact treatment on the test piece (13) subjected to dropping coating, reducing the distance between the silicon nano particles (19) and the graphene oxide (20), and increasing the contact area between the silicon nano particles and the graphene oxide;
step 6): laying an absorption layer (4) on the surface of a test piece (16) subjected to ultrasonic impact, laying a restraint layer (3) above the absorption layer (4), carrying out laser treatment, enabling a laser beam (2) to penetrate through the restraint layer (3) and be absorbed by the absorption layer (4), then generating plasma explosion to form shock waves, and further increasing the contact area between silicon nano particles (19) and graphene oxide (20);
step 7): and annealing the test piece (17) subjected to laser shock in a protective gas environment to obtain the lithium battery electrode (18).
2. The method for preparing a lithium battery electrode based on laser shock according to claim 1, wherein the absorbing layer (4) in the step 1) is black paint or black teflon tape.
3. The method for preparing a lithium battery electrode based on laser shock according to claim 1, wherein the constraining layer (3) in step 1) is water or optical glass.
4. The method for preparing the lithium battery electrode based on laser shock according to claim 1, wherein the laser beam (2) in the step 1) is generated by a laser (24), and the laser (24) adopts a high-power Q-switched Nd: YAG laser.
5. The method for preparing the lithium battery electrode based on laser shock according to claim 1, wherein the laser beam (2) in the steps 1) and 6) is transmitted through the optical device (22) to change the transmission direction and focused, and then is absorbed by the absorption layer (4) through the constraint layer (3).
6. The method for preparing a lithium battery electrode based on laser shock according to claim 1, wherein the ratio of the silicon nanoparticles, the polyvinylpyrrolidone and the ethanol in step 2) is 1 g: 5 g: 100 mL.
7. The method for preparing a laser shock based lithium battery electrode as claimed in claim 1, wherein the temperature of the capping reaction in the step 2) is 70 ℃.
8. The method for preparing a laser shock based lithium battery electrode as claimed in claim 1, wherein the washing in the step 2) is performed a plurality of times using ethanol.
9. The method for preparing a laser shock based lithium battery electrode as claimed in claim 1, wherein the protective gas in the step 7) is an inert gas.
10. The method for preparing a lithium battery electrode based on laser shock according to claim 1, wherein the annealing treatment in the step 7) comprises the following process parameters: 600 ℃ for 2 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113322374A (en) * | 2021-05-17 | 2021-08-31 | 武汉大学 | Laser shock method based on suspension drop enhancement and application thereof |
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