CN111092260A - Solid-like battery preparation method - Google Patents

Solid-like battery preparation method Download PDF

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CN111092260A
CN111092260A CN201911258960.7A CN201911258960A CN111092260A CN 111092260 A CN111092260 A CN 111092260A CN 201911258960 A CN201911258960 A CN 201911258960A CN 111092260 A CN111092260 A CN 111092260A
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electrolyte
precursor powder
solid
battery
plasticizer
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CN111092260B (en
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夏阳
韩熠垚
卢成炜
张文魁
黄辉
甘永平
梁初
张俊
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Zhejiang University of Technology ZJUT
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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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • 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

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Abstract

The invention belongs to the technical field of solid-state batteries, and particularly relates to a preparation method of a solid-state-like battery. The method comprises the steps of carrying out freeze ball milling on electrode material powder, a conductive agent, a plasticizer, a binder and lithium salt to form electrode precursor powder (divided into positive and negative electrodes); the plasticizer, the lithium salt, the binder and the inorganic filler are frozen and ball-milled to form electrolyte precursor powder; pressing the anode precursor powder into an anode pole piece, laying electrolyte precursor powder, pressing into an anode/electrolyte complex, laying cathode precursor powder on the electrolyte side, and pressing into a solid-state battery; and heating the battery, melting the pre-embedded plasticizer, wetting the electrode material and the electrolyte material, and improving the interface wettability of the battery. The method comprises the step of pressing and forming the anode precursor powder, the electrolyte and the cathode precursor powder with the plasticizer and the lithium salt pre-embedded layer by layer to obtain the quasi-solid battery. When the battery is prepared by adopting the method, the addition of electrolyte is not needed, the method is quick and efficient, the operation is simple, the cost is low, and the industrialization is favorably realized.

Description

Solid-like battery preparation method
Technical Field
The invention belongs to the technical field of solid-state batteries, and particularly relates to a preparation method of a solid-state-like battery.
Background
The solid-state battery has the advantages of high energy density, long cycle life, safety, reliability and the like, and is widely concerned at home and abroad. However, both the electrode and the electrolyte in the solid-state battery are solid, and a solid-solid interface formed between the electrode and the electrolyte has high interface resistance, and meanwhile, the interface wettability and the interface stability are poor, so that the electrochemical performance of the solid-state battery is influenced, and the practical application of the solid-state battery is hindered. Therefore, solving the interfacial problem of the solid-state battery is a key factor in achieving battery performance.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a preparation method of a quasi-solid-state battery, which is rapid, efficient, low in cost and simple to operate.
In order to achieve the above object, the present invention provides the following technical solutions:
a solid-state-like battery preparation method, comprising the steps of:
s1, uniformly mixing the positive electrode material powder or the negative electrode material powder with a conductive agent, a plasticizer, a binder and lithium salt according to a certain mass ratio under a freezing ball milling condition to form positive electrode precursor powder or negative electrode precursor powder;
s2, uniformly mixing a plasticizer, a lithium salt, a binder and an inorganic filler according to a certain mass ratio under a freezing ball milling condition to form electrolyte precursor powder;
s3, pressing the positive electrode precursor powder prepared in the S1 into a positive electrode piece with a certain pressure;
s4, laying the electrolyte precursor powder prepared in the S2 on the positive pole piece prepared in the S3, and pressing the electrolyte precursor powder and the positive pole piece into a positive pole/electrolyte complex by certain pressure;
s5, laying the negative electrode precursor powder prepared in the S1 on the electrolyte side of the positive electrode/electrolyte composite prepared in the S4, and pressing the mixture into a solid battery with certain pressure;
and S6, heating the similar solid-state battery for a period of time at a certain temperature to melt the pre-embedded plasticizer and fully wet the electrode material and the electrolyte material.
Preferably, the plasticizer in step S1 includes one or more of ethylene carbonate EC, vinylene carbonate VC, dimethyl carbonate DMC, and fluoroethylene carbonate FEC.
Preferably, the electrode material in step S1 includes at least one of a layered compound, a spinel-type compound, an olivine-type compound, a NASICON-type compound, an intercalation-type material, an alloy-type material, and a conversion-type material.
More preferably, the chemical formula of the positive electrode material powder in step S1 includes LixMO2(M＝Co，Ni，Mn)、LiMPO4(M＝Co，Fe，Mn，N)、LiMn2O4、LiCo2O4、LiV2O4、Li3V2(PO4)3、Li3Fe2(PO4)3、LiNi1-xCoxO2、LiNi1- xMnxO2、LiNi1-x-yCoyMnxO2、LiNi1-x-yCoyAlxO2At least one of; the chemical formula of the cathode material powder comprises C, Si/C, Li3N、Li7MnN4、Li3FeN2、Li3-xCoxN、SnO、TiO2、Li4Ti5O12At least one of (1).
Preferably, the lithium salt in step S1 includes lithium hexafluorophosphate LiPF6Lithium perchlorate LiClO4Lithium tetrafluoroborate (LiBF)4Lithium hexafluoroarsenate LiAsF6Lithium trifluoromethanesulfonate LiCF3SO3Lithium bis (trifluoromethylsulfonyl) imide LiN (CF)3SO2)2Bis (pentafluoroethylsulfonyl) iminolithium LiN (C)2F5SO2)2At least one of; the binder comprises at least one of polyethylene oxide (PEO), polymethyl methacrylate (PMMA), polyvinylidene fluoride (PVDF), Polyethylene (PE), sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR); the conductive agent comprises at least one of conductive carbon black, conductive graphite and conductive carbon fiber.
Preferably, in the step S1, the positive electrode precursor powder (or the negative electrode precursor powder) comprises 60-70% of the positive electrode material powder (or the negative electrode material powder), 1-10% of the conductive agent, 5-10% of the binder, 10-20% of the plasticizer, and 1-5% of the lithium salt.
Preferably, in the step S2, the electrolyte precursor powder comprises 30-70% of binder, 10-40% of lithium salt, 10-20% of inorganic filler and 10-20% of plasticizer.
Preferably, the temperature of the frozen ball milling in the steps S1 and S2 is-120 to-5 ℃, the rotating speed is 100 to 500rpm, and the ball-to-material ratio is 15:1 to 40: 1.
More preferably, the temperature of the frozen ball milling in the steps S1 and S2 is-50 to-5 ℃, the rotating speed is 100 to 300rpm, and the ball-to-material ratio is 15:1 to 30: 1.
Preferably, the pressing pressure in steps S3, S4 and S5 is 0.1 to 80 MPa.
More preferably, the pressing pressure in the steps S3, S4 and S5 is 12 to 40 MPa.
Preferably, the heating temperature in step S6 is 20-100 ℃, and the heating time is 0.1-48 h.
More preferably, the heating temperature in step S6 is 30-80 ℃, and the heating time is 1-24 h.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, anode material powder or cathode material powder is uniformly mixed with a conductive agent, a plasticizer, a binder and a lithium salt according to a certain mass ratio under a freezing ball milling condition to form anode precursor powder or cathode precursor powder. Uniformly mixing a plasticizer, a lithium salt, a binder and an inorganic filler under a freezing ball milling condition according to a certain mass ratio to form electrolyte precursor powder. Preparing the prepared anode precursor powder into an anode plate under certain pressure, laying the electrolyte precursor powder on the anode plate, pressing under certain pressure to form an anode/electrolyte complex, laying the cathode precursor powder on the electrolyte side of the anode/electrolyte complex, and pressing under certain pressure to form the quasi-solid battery. After the battery is formed, the battery is heated at a certain temperature, so that the preset plasticizer is melted, the electrode material and the electrolyte material are fully wetted, and the interface wettability of the battery is improved, thereby improving the performance of the solid-state battery.
The method comprises the step of pressing and forming the positive electrode, the electrolyte and the negative electrode, which are pre-buried with the plasticizer, the lithium salt and the binder, layer by layer to obtain the quasi-solid battery. When the battery is prepared by adopting the method, the addition of electrolyte is not needed, the method is quick and efficient, the operation is simple, the cost is low, and the method is favorable for realizing industrial production.
Drawings
Fig. 1 is a schematic view of a battery prepared in example 1;
fig. 2 is a graph showing cycle performance of the battery prepared in example 1.
In the figure: 1. the lithium ion battery comprises a positive pole piece pre-buried with plasticizer and lithium salt, a solid electrolyte pre-buried with plasticizer and lithium salt and a negative pole piece pre-buried with plasticizer and lithium salt.
Detailed Description
The technical solution of the present invention is further specifically described by the following embodiments with reference to the attached drawings, but the scope of the present invention is not limited thereto.
Example 1:
the first step is as follows: preparation of Positive electrode precursor powder and negative electrode precursor powder
S1 preparation of Ethylene Carbonate (EC) and LiFePO4(LFP) and conductive carbon black are uniformly mixed according to a certain proportion, then lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and PVDF are added for freezing and ball milling, the ball milling temperature is-10 ℃, the rotating speed is 250rpm, and the ball-to-material ratio is 20:1, so that uniform positive electrode precursor powder is formed (LFP: conductive carbon black: PVDF: EC: LiTFSI ═ 60:7:10:20: 3); mixing EC, Si/C and conductive carbon black uniformly according to a certain proportion, adding lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and CMC to carry out frozen ball milling at the temperature of minus 10 ℃, the rotating speed of 250rpm and the ball-to-material ratio of 20:1 to form uniform negative electrode precursor powder (Si/C: conductive carbon black: CMC: EC: LiTFSI ═ 60:6:9:20: 5).
The second step is that: preparation of electrolyte precursor powder
S2, mixing EC, PEO, LiTFSI and Al2O3Mixing at a certain ratio (PEO: LiTFSI: Al)2O3EC 40:40:10:10) were subjected to ball milling at-5 ℃, a rotation speed of 250rpm, and a ball-to-material ratio of 20:1, to form electrolyte precursor powder.
The third step: preparation of Positive electrode/electrolyte composite
S3, pressing the uniformly mixed anode precursor powder into an anode plate, wherein the pressure is 18 MPa.
S4, laying the electrolyte precursor powder on the anode plate, and pressing into an anode/electrolyte complex with the pressure of 16 MPa.
The fourth step: preparation-like solid-state battery
And S5, paving the negative electrode precursor powder on the electrolyte side of the positive electrode/electrolyte composite, pressing into a solid-state battery with the pressure of 16MPa, and adding no electrolyte in the battery loading process.
And S6, heating the prepared similar solid battery for 12 hours at 50 ℃ to melt the pre-embedded plasticizer and wet the electrode material and the electrolyte material.
FIG. 1 is a schematic diagram of the cell;
fig. 2 shows the cycle performance of the cell.
Example 2:
the first step is as follows: preparation of Positive electrode precursor powder and negative electrode precursor powder
S1 preparation of Vinylene Carbonate (VC) and LiNi0.6Co0.2Mn0.2O2Uniformly mixing the conductive carbon black and the lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) according to a certain proportion, adding the lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and PEO, and carrying out freeze ball milling at the temperature of-30 ℃, the rotating speed of 100rpm and the ball-to-material ratio of 15:1 to form uniform positive electrode precursor powder (NCM: conductive carbon black: PEO: VC: LiTFSI ═ 62:6:10:19: 3); mixing VC and Li4Ti5O12And uniformly mixing the conductive carbon black according to a certain proportion, adding LiTFSI and PEO, and carrying out freeze ball milling at the ball milling temperature of-30 ℃, the rotation speed of 100rpm and the ball-to-material ratio of 15:1 to form uniform negative electrode precursor powder (LTO: conductive carbon black: PEO: VC: LiTFSI: 62:10:5:19: 4).
The second step is that: preparation of electrolyte precursor powder
S2, mixing VC, PEO, LiTFSI and Li6.4La3Zr1.4Ta0.6O12Mixing according to a certain proportion (PEO: LiTFSI: LLZTO: VC: 70:10:10:10) and carrying out frozen ball milling at the temperature of-120 ℃, the rotating speed of 500rpm and the ball-to-material ratio of 15:1 to form the electrolyte precursor powder.
The third step: preparation of Positive electrode/electrolyte composite
S3, pressing the uniformly mixed anode precursor powder into an anode plate, wherein the pressure is 40 MPa.
S4, laying the electrolyte precursor powder on the anode plate, and pressing into an anode/electrolyte complex with the pressure of 2 MPa.
The fourth step: preparation-like solid-state battery
And S5, paving the uniformly mixed negative electrode precursor powder on the electrolyte side of the positive electrode/electrolyte composite, pressing into a solid-state-like battery, wherein the pressure is 40MPa, and no electrolyte is required to be added in the battery loading process.
And S6, heating the prepared similar solid battery for 0.1h at 100 ℃ to melt the pre-embedded plasticizer and wet the electrode material and the electrolyte material.
Example 3:
the first step is as follows: preparation of Positive electrode precursor powder and negative electrode precursor powder
S1 preparation of fluoroethylene carbonate (FEC) and LiNi0.6Co0.2Mn0.2O2Uniformly mixing the carbon fibers and the lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) according to a certain proportion, adding the lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and the PVDF into the mixture, and carrying out freeze ball milling at the ball milling temperature of-50 ℃, the rotation speed of 500rpm and the ball-to-material ratio of 40:1 to form uniform positive precursor powder (NCM: conductive carbon fibers: PVDF: FEC: LiTFSI ═ 70:1:5:20: 4); and uniformly mixing the FEC, the Si/C and the conductive carbon fiber according to a certain proportion, adding lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) and SBR, and carrying out freeze ball milling at the ball milling temperature of-50 ℃, the rotation speed of 500rpm and the ball-to-material ratio of 40:1 to form uniform negative electrode precursor powder (Si/C: conductive carbon fiber: SBR: FEC: LiTFSI: 63:4:9:19: 5).
The second step is that: preparation of electrolyte precursor powder
S2, mixing FEC, PEO, LiTFSI and Li6.4La3Zr1.4Ta0.6O12Mixing according to a certain proportion (PEO: LiTFSI: LLZTO: FEC: 30:20:20) and carrying out frozen ball milling at the temperature of-50 ℃, the rotating speed of 500rpm and the ball-to-material ratio of 40:1 to form the electrolyte precursor powder.
The third step: preparation of Positive electrode/electrolyte composite
S3, pressing the uniformly mixed anode precursor powder into an anode plate, wherein the pressure is 80 MPa.
S4, laying the electrolyte precursor powder on the anode plate, and pressing into an anode/electrolyte complex with the pressure of 0.1 MPa.
The fourth step: preparation-like solid-state battery
And S5, paving the uniformly mixed negative electrode precursor powder on the electrolyte side of the positive electrode/electrolyte composite, pressing into a solid-state battery, wherein the pressure is 80MPa, and no electrolyte is required to be added in the battery loading process.
And S6, heating the prepared similar solid battery for 48 hours at the temperature of 20 ℃ to melt the pre-embedded plasticizer and wet the electrode material and the electrolyte material.
In summary, the solid-state battery obtained by the method improves the wettability of the solid-solid interface, so that the electrochemical performance of the solid-state battery is further improved, and the method does not need to add electrolyte in the process of preparing the solid-state battery, is simple and convenient to operate, is rapid and efficient, and has remarkable economic benefit.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.

Claims (10)

1. A method for preparing a quasi-solid-state battery is characterized by comprising the following steps:
s1, uniformly mixing the positive electrode material powder or the negative electrode material powder with a conductive agent, a plasticizer, a binder and lithium salt according to a certain mass ratio under a freezing ball milling condition to form positive electrode precursor powder or negative electrode precursor powder;
s2, uniformly mixing a plasticizer, a lithium salt, a binder and an inorganic filler according to a certain mass ratio under a freezing ball milling condition to form electrolyte precursor powder;
s3, pressing the positive electrode precursor powder prepared in the S1 into a positive electrode piece with a certain pressure;
s4, laying the electrolyte precursor powder prepared in the S2 on the positive pole piece prepared in the S3, and pressing the electrolyte precursor powder and the positive pole piece into a positive pole/electrolyte complex by certain pressure;
s5, laying the negative electrode precursor powder prepared in the S1 on the electrolyte side of the positive electrode/electrolyte composite prepared in the S4, and pressing the mixture into a solid battery with certain pressure;
and S6, heating the similar solid-state battery for a period of time at a certain temperature to melt the pre-embedded plasticizer and fully wet the electrode material and the electrolyte material.
2. The method as claimed in claim 1, wherein the plasticizer in step S1 includes one or more of ethylene carbonate EC, vinylene carbonate VC, dimethyl carbonate DMC, and fluoroethylene carbonate FEC.
3. The solid-state battery-like production method according to claim 1, wherein the electrode material in step S1 includes at least one of a layered compound, a spinel-type compound, an olivine-type compound, a NASICON-type compound, an intercalation-type material, an alloy-type material, and a conversion-type material.
4. The method of claim 3, wherein the chemical formula of the positive electrode material powder in step S1 includes LixMO2(M＝Co，Ni，Mn)、LiMPO4(M＝Co，Fe，Mn，N)、LiMn2O4、LiCo2O4、LiV2O4、Li3V2(PO4)3、Li3Fe2(PO4)3、LiNi1-xCoxO2、LiNi1-xMnxO2、LiNi1-x-yCoyMnxO2、LiNi1-x-yCoyAlxO2At least one of; the chemical formula of the cathode material powder comprises C, Si/C, Li3N、Li7MnN4、Li3FeN2、Li3-xCoxN、SnO、TiO2、Li4Ti5O12At least one of (1).
5. The method of claim 1, wherein the lithium salt in step S1 includes lithium hexafluorophosphate LiPF6Lithium perchlorate LiClO4Lithium tetrafluoroborate (LiBF)4Lithium hexafluoroarsenate LiAsF6Lithium trifluoromethanesulfonate LiCF3SO3Lithium bis (trifluoromethylsulfonyl) imide LiN (CF)3SO2)2Bis (pentafluoroethylsulfonyl) iminolithium LiN (C)2F5SO2)2At least one of; the binder comprises polyethylene oxide PEO, polymethyl methacrylate PMMA, polyvinylidene fluoride PVDF, polyethylene PE, sodium carboxymethyl cellulose CMC and styrene butadiene rubber SBRAt least one of (a); the conductive agent comprises at least one of conductive carbon black, conductive graphite and conductive carbon fiber.
6. The method for preparing a solid-state battery as claimed in claim 1, wherein the ratio of the positive electrode precursor powder or the negative electrode precursor powder in step S1 is 60-70% of the positive electrode material powder or the negative electrode material powder, 1-10% of the conductive agent, 5-10% of the binder, 10-20% of the plasticizer, and 1-5% of the lithium salt.
7. The method for preparing a solid-state battery as claimed in claim 1, wherein the electrolyte precursor powder in step S2 comprises 30-70% of binder, 10-40% of lithium salt, 10-20% of inorganic filler and 10-20% of plasticizer.
8. The method for preparing the quasi-solid battery as claimed in claim 1, wherein the temperature of the frozen ball milling in the steps S1 and S2 is-120 to-5 ℃, the rotation speed is 100 to 500rpm, and the ball-to-material ratio is 15:1 to 40: 1; the pressing pressure in the steps S3, S4 and S5 is 0.1-80 MPa; in the step S6, the heating temperature is 20-100 ℃, and the heating time is 0.1-48 h.
9. The method for preparing a solid-state battery as claimed in claim 1 or 8, wherein the temperature of the frozen ball milling in steps S1 and S2 is-50 to-5 ℃, the rotation speed is 100 to 300rpm, and the ball-to-material ratio is 15:1 to 30: 1.
10. The solid-state battery-like production method according to claim 1 or 8, wherein the pressing pressure in steps S3, S4 and S5 is 12 to 40 MPa; in the step S6, the heating temperature is 30-80 ℃, and the heating time is 1-24 h.
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