CN108417777A - A kind of porous triple anode composite piece and preparation method thereof and its application - Google Patents
A kind of porous triple anode composite piece and preparation method thereof and its application Download PDFInfo
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- CN108417777A CN108417777A CN201810399208.3A CN201810399208A CN108417777A CN 108417777 A CN108417777 A CN 108417777A CN 201810399208 A CN201810399208 A CN 201810399208A CN 108417777 A CN108417777 A CN 108417777A
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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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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Abstract
The invention discloses a kind of porous triple anode composite pieces, it is characterised in that：Porous triple positive plate includes following material：The mass parts of ternary main material, conductive agent, binder, fast-ionic conductor, lithium salts and pore creating material, each material are respectively：Ternary main material：80 90 parts, conductive agent：15 parts, binder：25 parts, fast-ionic conductor：2 15 parts, lithium salts：3 10 parts, pore creating material：25 parts.Advantage is：In the present invention so that solid electrolyte is perfused to pole piece, while improving electrode/electrolyte interface compatibility, also enhances the ability of pole piece inner ion transmission, improves the chemical property of solid state battery entirety；Porous triple composite sheet of the present invention is applied to solid state battery field, has the possibility of large-scale mass production.
Description
Technical field
The present invention relates to field of lithium ion battery, relate to a kind of porous triple anode composite piece, further relate to a kind of porous
The preparation method of tri compound positive plate further relates to a kind of application of porous triple anode composite piece.
Background technology
All-solid lithium-ion battery substitutes traditional organic liquid electrolyte using solid electrolyte, is expected to fundamentally solve
Cell safety sex chromosome mosaicism is electric vehicle and the ideal electrochmical power source of scale energy storage, and crucial includes mainly preparing high room temperature
The solid electrolyte of conductivity and electrochemical stability and suitable for all-solid lithium-ion battery high-energy electrode material, change
Kind electrode/solid electrolyte interface compatibility.
Although solid electrolyte is substantially not present the side reaction of solid electrolyte decomposition, solid with electrode material interface
Characteristic makes electrode/electrolyte interface compatibility bad, the too high transmission for having seriously affected ion of interface impedance, eventually leads to solid
The cycle life of state battery is low, high rate performance is poor.In addition, energy density can not meet the requirement of large-sized battery.For electrode
The research of material is concentrated mainly on two aspects：First, being modified to electrode material and its interface, improve electrode/electrolyte circle
Face compatibility；Second is that exploitation new electrode materials, to further promote the chemical property of solid state battery, all-solid-state battery is just
Combination electrode is extremely generally used, further includes solid electrolyte and conductive agent other than electrode active material, plays biography in the electrodes
The effect of defeated ion and electronics, the oxide anodes such as LiCoO2, LiFePO4, LiMn2O4 are in all-solid-state battery using more general
Time.To improve electrode/electrolyte interface compatibility, the present invention develops a kind of method preparing porous anode piece, and by solid-state
Inside electrolyte perfusion to pole piece, while improving electrode/electrolyte interface compatibility, the transmission of pole piece inner ion can be enhanced
Ability, be expected to promoted solid state battery entirety chemical property.
Invention content
The purpose of the present invention is：Against the above deficiency, provide a kind of porous triple anode composite piece and preparation method thereof and
It is applied.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of porous triple anode composite piece, it is characterised in that：Porous triple positive plate includes following material：Ternary master
The mass parts of material, conductive agent, binder, fast-ionic conductor, lithium salts and pore creating material, each material are respectively：Ternary main material：80-
90 parts, conductive agent：1-5 parts, binder：2-5 parts, fast-ionic conductor：2-15 parts, lithium salts：3-10 parts, pore creating material：2-5 parts.
Ternary main material includes nickle cobalt lithium manganate (532,622,811), while can be replaced cobalt acid lithium, LiFePO4, Fu Li
Manganese base or LiMn2O4.
Conductive agent is Surpe-P, acetylene black, KS-6, CNT or graphene.
Binder is Kynoar.
Fast-ionic conductor is lithium lanthanum zirconium oxygen, Li-La-Ti oxygen or lithium lanthanum zirconium tantalum oxygen.
Lithium salts is LiTFSI, LiClO4, LiBF4, LiPF6Or LiAsF6。
Pore creating material is polyvinylpyrrolidone, urea, carbonic acid ammonia, low boiling point alcohols or ketone, and the alcohols or ketone are
Methanol, ethyl alcohol, acetone.
A kind of preparation method of porous triple anode composite piece, includes the following steps：
Step 1：Ternary main material, conductive agent, binder, fast-ionic conductor and lithium salts are dispersed in N- after mixing
In methylpyrrolidone solution；
Step 2：It is stirred with vacuum planetary mixer to obtain anode sizing agent；
Step 3：Finely dispersed pore creating material is added later, is stirred with vacuum planetary mixer, obtains compound
Anode sizing agent；
Step 4：Anode composite slurry is coated on 12-16um conductive coating aluminium foils with coating machine, coating thickness is
150-200 μm, using classification stoving process, 80-100 DEG C of level-one drying temperature, 110-130 DEG C of two level drying temperature, operation speed
Degree is 500-800mm/min, and the pole piece after winding is dried 12-24h in 100-110 DEG C of vacuum bakeout case again, will consolidate
The pole piece of state electrolyte coating after the drying, vacuumize process make electrolyte be fully infiltrated into pole piece, form composite pole
Piece；
Step 5：Pole piece after will be compound is placed in 80-90 DEG C of vacuum drying chamber dry 12-24h, to the electrode after drying
Piece carries out roll-in, and (compacting control is in 3-3.4mg/cm3), cutting obtains anode composite piece.
A kind of application of porous triple anode composite piece, obtained porous triple anode composite piece and solid electrolyte, lithium
Foil carries out lamination, assembling obtains solid lithium ion battery, will obtain solid lithium ion battery in 0.2C charge and discharge, charge and discharge cut-off
Charge and discharge cycles test is carried out under conditions of voltage 3.0-4.2V, first discharge specific capacity 135-155mAh/g is recycled 300 weeks
Afterwards, capacity retention ratio 80-90%
Compared with prior art, what the present invention was reached has the technical effect that：In the present invention so that solid electrolyte is perfused
To pole piece, while improving electrode/electrolyte interface compatibility, the ability of pole piece inner ion transmission is also enhanced,
Improve the chemical property of solid state battery entirety；Porous triple composite sheet of the present invention is applied to solid state battery field, has big
The possibility of scale batch production.
Description of the drawings
Fig. 1 is the button electricity cycle figure of solid lithium ion battery.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and embodiments：
Embodiment one：
A kind of porous triple anode composite piece, it is characterised in that：Porous triple positive plate includes following material：Ternary 532,
Surpe-P, Kynoar, lithium lanthanum zirconium tantalum oxygen, LiTFSI and acetone, the mass parts of each material are respectively：Ternary 532：80
Part, Surpe-P：5 parts, Kynoar：5 parts, lithium lanthanum zirconium tantalum oxygen：15 parts, LiTFSI：10 parts, acetone：5 parts.
A kind of preparation method of porous triple anode composite piece, includes the following steps：Step 1：By ternary 532, Surpe-
P, Kynoar, lithium lanthanum zirconium tantalum oxygen and LiTFSI are dispersed in after mixing in N-Methyl pyrrolidone solution；
Step 2：It is stirred with vacuum planetary mixer to obtain anode sizing agent；
Step 3：Finely dispersed acetone is added later, is stirred with vacuum planetary mixer, obtain it is compound just
Pole slurry；
Step 4：Anode composite slurry is coated on 12um conductive coating aluminium foils with coating machine, coating thickness is 150 μ
M, using classification stoving process, 80 DEG C of level-one drying temperature, 110 DEG C, speed of service 800mm/min of two level drying temperature is received
12h is dried in 100 DEG C of vacuum bakeout case again in pole piece after volume, by the pole piece table of solid electrolyte coating after the drying
Face, vacuumize process make electrolyte be fully infiltrated into pole piece, form composite pole piece；
Step 5：Pole piece after will be compound is placed in drying in 90 DEG C of vacuum drying chambers and for 24 hours, is carried out to the electrode slice after drying
(compacting control is in 3-3.4mg/cm for roll-in3), cutting obtains anode composite piece.
A kind of application of porous triple anode composite piece, obtained porous triple anode composite piece and solid electrolyte, lithium
Foil carries out lamination, assembling obtains solid lithium ion battery, will obtain solid lithium ion battery in 0.2C charge and discharge, charge and discharge cut-off
Progress charge and discharge cycles test under conditions of voltage 3.0-4.2V, first discharge specific capacity 135mAh/g, after recycling 300 weeks,
Capacity retention ratio is 80%
Compared with prior art, what the present invention was reached has the technical effect that：In the present invention so that solid electrolyte is perfused
To pole piece, while improving electrode/electrolyte interface compatibility, the ability of pole piece inner ion transmission is also enhanced,
Improve the chemical property of solid state battery entirety；Porous triple composite sheet of the present invention is applied to solid state battery field, has big
The possibility of scale batch production.
Embodiment two：
A kind of porous triple anode composite piece, it is characterised in that：Porous triple positive plate includes following material：Ternary 532,
Acetylene black, Kynoar, Li-La-Ti oxygen, LiClO4And polyvinylpyrrolidone, the mass parts of each material are respectively：Ternary
532：85 parts, acetylene black：2 parts, Kynoar：3 parts, Li-La-Ti oxygen：7 parts, LiClO4：4 parts, polyvinylpyrrolidone：4
Part.
A kind of preparation method of porous triple anode composite piece, includes the following steps：Step 1：By ternary 532, acetylene
Black, Kynoar, Li-La-Ti oxygen and LiClO4It is dispersed in after mixing in N-Methyl pyrrolidone solution；
Step 2：It is stirred with vacuum planetary mixer to obtain anode sizing agent；
Step 3：Finely dispersed polyvinylpyrrolidone is added later, is stirred with vacuum planetary mixer,
Obtain anode composite slurry；
Step 4：Anode composite slurry is coated on 14um conductive coating aluminium foils with coating machine, coating thickness is 170 μ
M, using classification stoving process, 90 DEG C of level-one drying temperature, 120 DEG C, speed of service 800mm/min of two level drying temperature is received
18h is dried in 105 DEG C of vacuum bakeout case again in pole piece after volume, by the pole piece table of solid electrolyte coating after the drying
Face, vacuumize process make electrolyte be fully infiltrated into pole piece, form composite pole piece；
Step 5：Pole piece after will be compound is placed in drying in 90 DEG C of vacuum drying chambers and for 24 hours, is carried out to the electrode slice after drying
(compacting control is in 3-3.4mg/cm for roll-in3), cutting obtains anode composite piece.
A kind of application of porous triple anode composite piece, obtained porous triple anode composite piece and solid electrolyte, lithium
Foil carries out lamination, assembling obtains solid lithium ion battery, will obtain solid lithium ion battery in 0.2C charge and discharge, charge and discharge cut-off
Progress charge and discharge cycles test under conditions of voltage 3.0-4.2V, first discharge specific capacity 140mAh/g, after recycling 300 weeks,
Capacity retention ratio is 85%
Compared with prior art, what the present invention was reached has the technical effect that：In the present invention so that solid electrolyte is perfused
To pole piece, while improving electrode/electrolyte interface compatibility, the ability of pole piece inner ion transmission is also enhanced,
Improve the chemical property of solid state battery entirety；Porous triple composite sheet of the present invention is applied to solid state battery field, has big
The possibility of scale batch production.
Embodiment three：
A kind of porous triple anode composite piece, it is characterised in that：Porous triple positive plate includes following material：Ternary 532,
Graphene, Kynoar, lithium lanthanum zirconium oxygen, LiPF6And carbonic acid ammonia, the mass parts of each material are respectively：Ternary 532：90 parts,
Graphene：1 part, Kynoar：2 parts, lithium lanthanum zirconium oxygen：2 parts, LiPF6：3 parts, carbonic acid ammonia：2 parts.
A kind of preparation method of porous triple anode composite piece, includes the following steps：Step 1：By ternary 532, graphite
Alkene, Kynoar, lithium lanthanum zirconium oxygen, LiPF6It is dispersed in after mixing in N-Methyl pyrrolidone solution；
Step 2：It is stirred with vacuum planetary mixer to obtain anode sizing agent；
Step 3：Finely dispersed carbonic acid ammonia is added later, is stirred with vacuum planetary mixer, obtains compound
Anode sizing agent；
Step 4：Anode composite slurry is coated on 16um conductive coating aluminium foils with coating machine, coating thickness is 200 μ
M, using classification stoving process, 100 DEG C of level-one drying temperature, 130 DEG C, speed of service 800mm/min of two level drying temperature is received
Pole piece after volume is dried in 110 DEG C of vacuum bakeout case for 24 hours again, by the pole piece table of solid electrolyte coating after the drying
Face, vacuumize process make electrolyte be fully infiltrated into pole piece, form composite pole piece；
Step 5：Pole piece after will be compound is placed in drying in 90 DEG C of vacuum drying chambers and for 24 hours, is carried out to the electrode slice after drying
(compacting control is in 3-3.4mg/cm for roll-in3), cutting obtains anode composite piece.
A kind of application of porous triple anode composite piece, obtained porous triple anode composite piece and solid electrolyte, lithium
Foil carries out lamination, assembling obtains solid lithium ion battery, will obtain solid lithium ion battery in 0.2C charge and discharge, charge and discharge cut-off
Progress charge and discharge cycles test under conditions of voltage 3.0-4.2V, first discharge specific capacity 155mAh/g, after recycling 300 weeks,
Capacity retention ratio is 90%
Compared with prior art, what the present invention was reached has the technical effect that：In the present invention so that solid electrolyte is perfused
To pole piece, while improving electrode/electrolyte interface compatibility, the ability of pole piece inner ion transmission is also enhanced,
Improve the chemical property of solid state battery entirety；Porous triple composite sheet of the present invention is applied to solid state battery field, has big
The possibility of scale batch production.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of porous triple anode composite piece, it is characterised in that：Porous triple positive plate includes following material：Ternary main material,
The mass parts of conductive agent, binder, fast-ionic conductor, lithium salts and pore creating material, each material are respectively：Ternary main material：80-90
Part, conductive agent：1-5 parts, binder：2-5 parts, fast-ionic conductor：2-15 parts, lithium salts：3-10 parts, pore creating material：2-5 parts.
2. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The ternary main material includes nickel
Cobalt manganic acid lithium (532,622,811), while cobalt acid lithium is can be replaced, LiFePO4, lithium-rich manganese-based or LiMn2O4.
3. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The conductive agent is Surpe-
P, acetylene black, KS-6, CNT or graphene.
4. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The binder is to gather inclined fluorine
Ethylene.
5. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The fast-ionic conductor is lithium
Lanthanum zirconium oxygen, Li-La-Ti oxygen or lithium lanthanum zirconium tantalum oxygen.
6. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The lithium salts is LiTFSI,
LiClO4, LiBF4, LiPF6Or LiAsF6。
7. a kind of porous triple anode composite piece according to claim 1, it is characterised in that：The pore creating material is polyethylene
Pyrrolidones, urea, carbonic acid ammonia, low boiling point alcohols or ketone, the alcohols or ketone are methanol, ethyl alcohol, acetone.
8. a kind of preparation method of porous triple anode composite piece, it is characterised in that：Include the following steps：Step 1：By ternary
Main material, conductive agent, binder, fast-ionic conductor and lithium salts are dispersed in after mixing in N-Methyl pyrrolidone solution；
Step 2：It is stirred with vacuum planetary mixer to obtain anode sizing agent；
Step 3：Finely dispersed pore creating material is added later, is stirred with vacuum planetary mixer, obtains anode composite
Slurry；
Step 4：Anode composite slurry is coated on 12-16um conductive coating aluminium foils with coating machine, coating thickness 150-
200 μm, using classification stoving process, 80-100 DEG C of level-one drying temperature, 110-130 DEG C of two level drying temperature, the speed of service is
12-24h is dried in 100-110 DEG C of vacuum bakeout case again in 500-800mm/min, the pole piece after winding, by solid-state electricity
The pole piece of matter coating after the drying is solved, vacuumize process makes electrolyte be fully infiltrated into pole piece, forms composite pole piece；
Step 5：Pole piece after will be compound is placed in 80-90 DEG C of vacuum drying chamber dry 12-24h, to the electrode slice after drying into
(compacting control is in 3-3.4mg/cm for row roll-in3), cutting obtains porous triple anode composite piece.
9. a kind of application of porous triple anode composite piece, it is characterised in that：Obtained porous triple anode composite piece and solid
Electrolyte, lithium foil carries out lamination, assembling obtains solid lithium ion battery, will obtain solid lithium ion battery in 0.2C charge and discharge,
Charge and discharge cycles test, first discharge specific capacity 135-155mAh/ are carried out under conditions of charge and discharge blanking voltage 3.0-4.2V
G, cycle is after 300 weeks, capacity retention ratio 80-90%.
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| CN111490227A (en) * | 2019-01-29 | 2020-08-04 | 中南大学 | Porous composite pole piece, preparation thereof and application thereof in all-solid-state lithium battery |
| CN111509186A (en) * | 2020-05-22 | 2020-08-07 | 清陶（昆山）能源发展有限公司 | Lithium ion solid-state battery anode, preparation process thereof and lithium ion solid-state battery |
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| CN111682187B (en) * | 2020-07-08 | 2021-09-10 | 清陶（昆山）能源发展有限公司 | Coated composite cathode material, preparation method and application thereof |
| CN111900338A (en) * | 2020-09-15 | 2020-11-06 | 天津市捷威动力工业有限公司 | Preparation method of high-power thick electrode |
| CN112289995A (en) * | 2020-10-29 | 2021-01-29 | 上海电气集团股份有限公司 | Composite positive electrode slurry, positive electrode plate and solid-state battery |
| CN113140730A (en) * | 2021-03-26 | 2021-07-20 | 万向一二三股份公司 | High-nickel ternary lithium ion battery |
| CN112864353A (en) * | 2021-04-01 | 2021-05-28 | 清华大学深圳国际研究生院 | Positive electrode material, preparation method thereof, positive electrode and all-solid-state lithium ion battery |
| CN113437352A (en) * | 2021-06-24 | 2021-09-24 | 珠海冠宇电池股份有限公司 | Battery and preparation method thereof |
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