CN114613944B - Method for preparing solid-state battery electrode through microwave process - Google Patents

Method for preparing solid-state battery electrode through microwave process Download PDF

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Publication number
CN114613944B
CN114613944B CN202210300487.XA CN202210300487A CN114613944B CN 114613944 B CN114613944 B CN 114613944B CN 202210300487 A CN202210300487 A CN 202210300487A CN 114613944 B CN114613944 B CN 114613944B
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microwave
electrode
lithium
wave
battery electrode
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CN114613944A (en
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陈宏伟
李健
孔华彬
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Huaqiao University
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Huaqiao University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139Processes of manufacture
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a method for preparing a solid-state battery electrode by a microwave process, which comprises the following steps: (1) coating the wave-absorbing material outside the active substance; (2) Uniformly mixing the active material with the core-shell structure, the conductive agent and the additive to obtain electrode mixed powder; the electrode mixed powder obtained in the step (3) is pressed into a film; (4) And (5) putting the film into a special microwave die, and then performing microwave processing to generate the battery electrode. The invention obtains the positive electrode precursor through the spraying process, so that the microwave absorbing material used as the binder is uniformly distributed, the particles are well coated, the electrode is compact and the components are more uniform at the same time through the subsequent microwave processing, and the defects and limitations of the traditional dry process can be overcome.

Description

Method for preparing solid-state battery electrode through microwave process
Technical Field
The invention belongs to the technical field of secondary battery electrode materials, and particularly relates to a method for preparing a solid-state battery electrode through a microwave process.
Background
The organic liquid electrolyte in the traditional lithium ion battery has great potential safety hazard caused by inflammability. The thermal runaway risk of the all-solid-state lithium battery is far lower than that of the traditional lithium ion battery, and lithium dendrites generated by the negative electrode in the charge and discharge process can be effectively blocked due to good mechanical property of the electrolyte, so that dead lithium is reduced, the cycle life of the battery is prolonged, and the energy density of the battery is improved, so that the development of the all-solid-state battery becomes an important direction for developing a new generation of energy storage technology.
The solid electrode is used as the core component of the all-solid battery, and the main problem existing at present is that the gaps among active substances, conductive agents and solid electrolyte particles in the electrode are larger, a large number of point-to-point contacts exist, so that a large interfacial resistance exists among the solid particles, and the transmission of lithium ions in the electrode is limited, thereby weakening the rate performance and capacity performance of the battery. Thus, the preparation of a dense and high ionic conductivity positive electrode is one of the bottlenecks in the development of all-solid-state batteries.
The commercial solid-state battery positive electrode is mostly prepared by a wet coating process, wherein the wet process is to uniformly mix a binder with an active material and a conductive agent in a liquid phase after the binder is fully dissolved or dispersed in a solvent, and then to obtain the positive electrode by drying and volatilizing the solvent after the slurry is coated. The wet process is widely used in lithium battery factories, the binder is uniformly dispersed, and the binding effect is good, but the defects of insufficient environment protection, high cost, poor conductivity, easy cracking of thick pole pieces, side reaction of residual solvent and the like exist in the use of solvents (such as NMP). The electrode plate with large porosity is left after the solvent volatilizes, so that the interface resistance is large, the lithium ion conductivity is poor, and further the problems of the rate performance and the capacity performance of the battery are caused.
In contrast, the dry process is simple, and has the advantage of reducing voids without the need for solvents. There are many technical routes for dry electrodes, among which the most mature technologies available from Maxwell corporation, specifically include the following: mixing active material, conductive agent and Polytetrafluoroethylene (PTFE) in a mixer, extruding the powder mixture to form a continuous self-supporting electrode film, and finally pressing the thin electrode and the current collector together to form the battery pole piece. The traditional dry process has the defect that each component is not easy to disperse in a polymer melt, so that the obtained electrode film has internal verification phase separation and poor mechanical property. Meanwhile, the dry electrode needs long-time hot rolling or extrusion hot processing, has high energy consumption and is easy to cause thermal degradation of materials such as polymers. It is therefore highly desirable to develop a process that solves the above-mentioned problems.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing a solid-state battery electrode by a microwave process. The anode precursor is obtained through a spraying process, so that the microwave absorbing material serving as a binder is uniformly distributed, particles are well coated, and the components are more uniform while the electrode is compact through subsequent microwave processing, so that the defects and limitations of the traditional dry process can be overcome.
In order to achieve the above object, one of the technical solutions of the present invention is a method for preparing a solid-state battery electrode by a microwave process, specifically comprising the steps of:
(1) Coating the wave-absorbing material outside the active substance;
(2) Uniformly mixing the active material with the core-shell structure formed in the step (1) with a conductive agent and an additive to obtain electrode mixed powder;
(3) Pressing the electrode mixed powder obtained in the step (2) into a film;
(4) And (3) putting the film prepared in the step (3) into a special microwave die, and then carrying out microwave processing, wherein a wave-absorbing melting reaction occurs in the electrode, so that a compact electrode is generated.
In a preferred embodiment of the present invention, the coating process in the step (1) is a spraying process or a vapor deposition process.
In a preferred embodiment of the present invention, the wave-absorbing material in the step (1) includes one or more of a wave-absorbing carbon material, an iron-based wave-absorbing material, a wave-absorbing ceramic material, and a wave-absorbing polymer material.
Further, the wave-absorbing carbon material is preferably conductive graphite, graphene, carbon nanotubes and carbon fibers, the iron-based wave-absorbing material is preferably ferrite, the wave-absorbing ceramic material is preferably silicon carbide and silicon nitride, and the wave-absorbing polymer material is preferably an organic substance containing polar functional groups, such as polyaniline, polyethylene glycol, polythiophene, polypyrrole and the like.
Still further, the wave-absorbing polymeric material may be doped with a lithium salt prior to use, including tetrafluoroboric acid (LiBF) 4 ) Lithium perchlorate (LiClO) 4 ) Lithium hexafluoroarsenate (LiAsF) 6 ) Lithium hexafluorophosphate
(LiPF 6 ) One or more of lithium bisoxalato borate (LiBOB), lithium difluorooxalato borate (LiDFOB), lithium bisdifluorosulfimide (LiFSI) and lithium bistrifluoromethylsulfonimide (LiTFSI).
Still further, the wave-absorbing polymer material is preferably at least one of polyethylene glycol and derivatives thereof.
Further, the lithium salt is preferably lithium perchlorate (LiClO) 4 ) Or lithium bis (trifluoromethylsulfonyl) imide (LiTFSI).
Further, the mass ratio of the lithium salt to the wave-absorbing polymer material is 0.01-0.8:1.
In a preferred embodiment of the present invention, the ion conductivity of the wave-absorbing material in the step (1) is 10-10-10-1S/cm.
In a preferred embodiment of the present invention, the active material in the step (1) includes one or more of lithium iron phosphate, lithium cobalt oxide, lithium manganate, ternary cathode materials and derivatives thereof, elemental sulfur, sulfur-containing compounds and derivatives thereof, and organic materials and derivatives thereof having redox activity.
In a preferred embodiment of the present invention, the coating method in the step (1) includes a mechanical mixing method, a solid phase reaction method, a physical and chemical vapor deposition method, a dip coating method, a sol-gel method, a hydrothermal method, a co-precipitation method, an electrodeposition method, a ball milling method, a spray coating method, a microwave method, and an electrostatic spraying method.
In a preferred embodiment of the present invention, the thickness of the coating layer in the step (1) is 1nm-1cm.
In a preferred embodiment of the present invention, the mass fraction of the wave-absorbing material in the electrode mixed powder in the step (2) is 0.1% -90%.
In a preferred embodiment of the present invention, the conductive agent in the step (2) is one or more of carbon black, conductive graphite, ketjen black, super P, carbon fiber, carbon nanotube, and graphene.
In a preferred embodiment of the present invention, the additive in the step (2) is one or more of a polymer binder, a solid electrolyte and an electrolyte.
In a preferred embodiment of the present invention, the pressing in the step (3) is performed by vacuum hot pressing, atmosphere hot pressing, isostatic pressing, hot isostatic pressing, reactive hot pressing, vibration hot pressing, isostatic pressing, or ultra-high pressure sintering.
In a preferred embodiment of the present invention, the pressing in the step (3) is performed at a pressure of 0.1-3000MPa and a temperature of 30-1500 ℃.
In a preferred embodiment of the present invention, the film thickness of the pressed film in the step (3) is 5nm to 1cm.
In a preferred embodiment of the present invention, the microwave in the step (4) is an electromagnetic wave with a frequency ranging from 300MHz to 300GHz, the microwave heating is performed at a frequency ranging from 300MHz to 300GHz, and the wave may be in the form of sine wave, cosine wave, square wave, transverse wave, longitudinal wave, or any combination thereof.
In a preferred embodiment of the present invention, the microwave power in the step (4) is 10-9000W, and the microwave time is 0.01-3600S.
In order to achieve the above object, a second aspect of the present invention is a solid-state battery electrode obtained by a method for producing a solid-state battery electrode by a microwave process.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the method can lead the microwave absorbing material used as the binder to be evenly distributed, thereby better coating the particles; the selected conductive agent not only plays a role in improving the electronic conductivity, but also has better wave absorbing performance; the fully dried powder can be in closer contact with the components through pressure, so that the electrode density is improved, the thick electrode can be prepared, the cycle performance is improved, and the service life of the battery is prolonged;
2. compared with the wet process, the method of the invention has the advantages that the powder is subjected to pressure treatment, so that the problem of poor contact between particles in the electrode is solved;
3. compared with the traditional dry method, the method can achieve better binder distribution, and the binder is melted by subsequent microwave processing, so that the internal pores of the electrode are further filled, the electrode is further densified, and the distribution of components is more uniform;
4. the invention has simple process and does not need too many mechanical stirring links so as to greatly reduce the material loss; the heating efficiency of the microwave process is high, and the time is short, so that the microwave process is more energy-saving and efficient than the traditional dry process; and the controllability is good in the microwave processing process, so that the repeatability of the sample is good.
Drawings
FIG. 1 is a basic flow chart of the preparation of a solid state electrode by the microwave process of the present invention;
FIG. 2 is a schematic illustration of an active material of the present invention undergoing coating and microwave treatment;
FIG. 3 is a TEM image of an active material coated with a microwaveable material according to example 1 of the invention;
FIG. 4 is SEM images of cross-sections of electrodes treated with and without a microwave process in example 1 and comparative example 1 of the present invention;
fig. 5 is all solid-state battery data for the electrodes prepared in examples 1-2 of the present invention and comparative example 1.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in more detail with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited to these embodiments.
A method for preparing a solid state battery electrode by a microwave process:
(1) Coating the wave-absorbing material outside the active substance;
(2) Uniformly mixing the active material with the core-shell structure formed in the step (1) with a conductive agent and an additive to obtain electrode mixed powder;
(3) Pressing the electrode mixed powder obtained in the step (2) into a film;
(4) And (3) putting the film prepared in the step (3) into a special microwave die, and then carrying out microwave processing, wherein a wave-absorbing melting reaction occurs in the electrode, so that a compact electrode is generated.
Example 1
Polyethylene glycol is used as a wave absorbing material, and a spraying process is adopted for coating. 200mg of PEG particles with a molecular weight of 60 ppm are weighed at normal temperature, added with 10ml of deionized water and stirred until the PEG particles are completely dissolved. 700mg LCO,100mg acetylene black are weighed, mixed uniformly, ground for 15min by a mortar and added with an aqueous solution of PEG. After 30min of uniform dispersion, the slurry was added to the spray gun while stirring. Cutting aluminum foil with proper size, tightly adhering to a heating table, vertically placing the heating table, and heating to 250 ℃. And (3) uniformly spraying the slurry on the aluminum foil, taking down the aluminum foil after the spraying is finished, sending the aluminum foil into an oven at 80 ℃ for 3 hours, and scraping and collecting powder on the aluminum foil after the drying is finished. The mass is called 850mg. 90mg of the mixture is placed in a press die, and the pressure is 1.2MPa for 10min. After taking out, the wafer was cut to a size of 12mm in diameter and a thickness of 150. Mu.m. And loading the cut product into a microwave die. The microwave oven was adjusted to 700W power. And (5) carrying out microwave processing for 30S, and taking out to obtain the positive pole piece with the thickness of 120 mu m.
The TEM image of the active material coated with the microwaveable material in this example is shown in fig. 3, and it can be seen from fig. 3 that the active material exhibits a complete coating.
Example 2
Titanium nitride is used as a wave absorbing material, and a vapor deposition process is used for coating. LCO700mg was charged into the reaction chamber. Repeatedly vacuumizing and filling nitrogen, and taking titanium tetrachloride and ammonia as precursors under the protection of the nitrogen, wherein the two gases enter a reaction chamber through independent gas paths. Wherein nitrogen is used as a carrier gas to carry vaporized titanium tetrachloride into the reaction chamber through a bubbler in series. The carrier gas flows of ammonia and titanium tetrachloride were 80 and 150ml/min, respectively, and the nitrogen flow as the shielding gas was 670ml/min, the deposition temperature was 580 ℃, and the deposition time was 360S. And taking out after the deposition is finished, and sending the mixture into an oven at 80 ℃ for 3 hours. And scraping and collecting the powder on the aluminum foil after the drying is finished. The mass is 800mg. 90mg of the mixture is placed in a press die, and the pressure is 5MPa and maintained for 50min. After taking out, the wafer was cut to a size of 12mm in diameter and a thickness of 150. Mu.m. And loading the cut product into a microwave die. The microwave oven was adjusted to 800W power. And (5) carrying out microwave processing for 500S, and taking out to obtain the positive electrode plate with the thickness of 90 mu m.
Comparative example 1
The comparative example provides a conventional lithium ion battery, which is used for preparing a battery anode according to a conventional liquid coating preparation method, and does not comprise the anode plate of the microwave coating process. 700mg of LCO (liquid crystal on silicon) and 100mg of acetylene black are weighed, ground and uniformly mixed, then added into NMP (N-methyl pyrrolidone) solvent of polyvinylidene fluoride (PVDF), continuously ground for 15min, and mapped on an aluminum foil by a coating machine to obtain the anode with the thickness of 100 mu m.
The void ratios of the positive electrodes of the solid-state batteries produced in examples 1, 2 and comparative example 1 are shown in the following table.
Table 1 porosity of different samples
Sample of Porosity of the porous material
Comparative example 34%
Example 1 3%
Example 2 2%
Fig. 4 is SEM images of cross sections of the electrodes of example 1 and comparative example 1 treated and not treated by the microwave process; from the figure, the electrodes after microwave treatment were denser.
Example 3
The positive electrode sheets prepared in example 1, example 2 and comparative example 1 were assembled into solid-state batteries, respectively, and solid-state battery assembly tests were performed. The test results are shown in fig. 5, from which it is clear that the electrodes (examples 1 and 2) subjected to the microwave process exhibit better cycle performance.
The above embodiments are merely preferred embodiments of the present invention to illustrate the principles and the effects of the present invention, and are not intended to limit the invention. It should be noted that modifications to the above-described embodiments may be made by one skilled in the art without departing from the spirit and scope of the invention, and such modifications should also be considered as being within the scope of the invention.

Claims (8)

1. A method for preparing a solid state battery electrode by a microwave process, comprising the steps of:
(1) Coating the wave-absorbing material outside the active substance; the wave-absorbing material is a wave-absorbing polymer material, and the wave-absorbing polymer material comprises at least one of polyaniline, polythiophene, polypyrrole, polyethylene glycol, polyamide, polyimide, polyester, polyether, polysulfone and derivatives thereof;
(2) Uniformly mixing the active material with the core-shell structure formed in the step (1) with a conductive agent and an additive to obtain electrode mixed powder;
(3) Pressing the electrode mixed powder obtained in the step (2) into a film;
(4) And (3) filling the film prepared in the step (3) into a die, and then carrying out microwave processing to generate the battery electrode.
2. The method for preparing a solid state battery electrode by a microwave process according to claim 1, wherein the wave-absorbing polymer material is doped with a lithium salt before use, the lithium salt comprising one or more of lithium perchlorate, lithium hexafluoroarsenate, lithium hexafluorophosphate, lithium bisoxalato borate, lithium difluorooxalato borate, lithium bisdifluorosulfonimide and lithium bistrifluoromethylsulfonimide.
3. The method for producing a solid-state battery electrode by a microwave process according to claim 1, wherein the ion conductivity of the wave-absorbing material in the step (1) is 10 -10 -10 -1 S/cm。
4. The method for preparing a solid state battery electrode by a microwave process according to claim 1, wherein the coating method in the step (1) comprises a mechanical mixing method, a solid phase reaction method, a physical and chemical vapor deposition method, a dip coating method, a sol-gel method, a hydrothermal method, a co-precipitation method, an electrodeposition method, a ball milling method, a spray coating method, a microwave method, an electrostatic spray method.
5. The method according to claim 1, wherein the conductive agent in the step (2) is one or more of carbon black, conductive graphite, ketjen black, carbon fiber, carbon nanotube, graphene and mixed conductive agents thereof, and the additive is one or more of a polymer binder, a solid electrolyte and an electrolyte.
6. The method for preparing a solid state battery electrode by a microwave process according to claim 1, wherein the pressing in the step (3) is vacuum hot pressing, atmosphere hot pressing, isostatic pressing, hot isostatic pressing, reaction hot pressing, vibration hot pressing, isostatic pressing, and ultra-high pressure sintering.
7. The method for preparing a solid-state battery electrode according to claim 1, wherein the microwaves in the step (4) are electromagnetic waves with a frequency of 300MHz-300GHz, the waves are in the form of sine waves, cosine waves, square waves, transverse waves and combinations thereof, the microwave power is 10-9000W, and the microwave time is 0.01-3600S.
8. A solid state battery electrode obtained by the method of any one of claims 1-7.
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CN114824280B (en) * 2022-06-27 2022-09-06 蚂蚁新能源科技(天津)有限公司 Composite positive electrode material for lithium ion battery dry-method electrode and preparation method and application thereof

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CN102664247A (en) * 2012-04-01 2012-09-12 上海锦众信息科技有限公司 Method for preparing LiFePO4/SiC lithium battery positive plate by microwave heating
CN112186162A (en) * 2020-09-30 2021-01-05 西安交通大学 High-load high-surface-capacity lithium-sulfur battery positive electrode and preparation method and application thereof
CN112234249A (en) * 2020-09-24 2021-01-15 中国科学院化学研究所 Composite solid electrolyte, preparation method thereof and application thereof in solid secondary battery
CN114122317A (en) * 2021-11-23 2022-03-01 蜂巢能源科技(无锡)有限公司 Positive pole piece for solid-state battery and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10115928A1 (en) * 2001-03-30 2002-10-10 Creavis Tech & Innovation Gmbh Electrolyte membrane, this comprehensive membrane electrode assembly, manufacturing method and special uses
CN102664247A (en) * 2012-04-01 2012-09-12 上海锦众信息科技有限公司 Method for preparing LiFePO4/SiC lithium battery positive plate by microwave heating
CN112234249A (en) * 2020-09-24 2021-01-15 中国科学院化学研究所 Composite solid electrolyte, preparation method thereof and application thereof in solid secondary battery
CN112186162A (en) * 2020-09-30 2021-01-05 西安交通大学 High-load high-surface-capacity lithium-sulfur battery positive electrode and preparation method and application thereof
CN114122317A (en) * 2021-11-23 2022-03-01 蜂巢能源科技(无锡)有限公司 Positive pole piece for solid-state battery and preparation method and application thereof

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