CN108598368A - A kind of all-solid lithium-ion battery composite negative pole and preparation method thereof - Google Patents
A kind of all-solid lithium-ion battery composite negative pole and preparation method thereof Download PDFInfo
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- CN108598368A CN108598368A CN201810688824.0A CN201810688824A CN108598368A CN 108598368 A CN108598368 A CN 108598368A CN 201810688824 A CN201810688824 A CN 201810688824A CN 108598368 A CN108598368 A CN 108598368A
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- ion battery
- composite negative
- negative pole
- lithium
- solid lithium
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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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
-
- 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
-
- 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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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 kind of preparation methods of all-solid lithium-ion battery composite negative pole, include the following steps：Slurry is prepared, bonding agent is dissolved in NMP first, adds conductive agent later, after dispersion, forms glue, graphite, inorganic powder material, lithium salts are respectively added to carry out disperseing in glue stirring being prepared into negative electrode slurry by a certain percentage；Negative electrode slurry is coated on a current collector using coating machine, roll-in is carried out to the electrode slice after drying, compacting control obtains composite negative pole pole piece in 1.4 1.8mg/cm3, cutting；The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.Advantage is：All-solid lithium-ion battery of the present invention is applied to all-solid lithium-ion battery field with composite negative pole, it is ensured that battery safety will not cause the safety accidents such as on fire, explosion, and can realize large-scale mass production.
Description
Technical field
The present invention relates to field of lithium ion battery, relate to a kind of all-solid lithium-ion battery composite negative pole, further relate to
A kind of preparation method of all-solid lithium-ion battery composite negative pole.
Background technology
In all kinds of energy storage devices, advantages are standby since energy density is big, stability is high, has extended cycle life etc. for lithium ion battery
It is paid close attention to by people.Although its development course is shorter, lithium ion battery is in field of portable electronic apparatus success instead of original
Ni-MH battery and Ni-Cr battery, are widely used.Meanwhile as the fast development of new-energy automobile and country are right in recent years
The support energetically of new-energy automobile, in emerging electric vehicle field, lithium ion battery has broad application prospects.
All-solid lithium-ion battery is assembled using solid electrolyte, is entirely free of the liquid parts such as electrolyte.Quan Gu
The operation principle of state lithium ion battery is identical as the principle of conventional lithium ion battery, and when battery charges, Li+ is from positive electrode
Abjection migrates to the cathode of battery by solid electrolyte and is embedded into negative material.While charging, electronics is logical from anode
The migration of dispatch from foreign news agency road direction cathode is crossed, discharge process is then exactly the opposite.
Current lithium ion battery mainly uses liquid organic electrolyte, and there are the security risks such as leakage, inflammable, easy waterfall, and
Safety accident caused by a lot of safety factors due to lithium battery have occurred.Therefore, improving the safety of lithium ion battery seems non-
Often urgently with necessity.All-solid lithium-ion battery is with the conventional lithium ion battery main distinction, and all solid lithium is from giving battery master
Will by solid electrolyte instead of liquid organic electrolyte, and due to solid electrolyte have preferable thermal stability and change
Stability is learned, the security performance of lithium ion battery is can effectively improve.In all-solid-state battery in charge and discharge process solid electrolytic
Matter and interelectrode side reaction are less so that the cycle and storage life of battery are long.Secondly, in all-solid lithium-ion battery
There is no diaphragm, solid-state electrolyte layer itself that can play the role of that positive and negative anodes is prevented to contact.
Invention content
The purpose of the present invention is：Against the above deficiency, a kind of all-solid lithium-ion battery composite negative pole and its system are provided
Preparation Method.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of all-solid lithium-ion battery composite negative pole, this composite negative pole include graphite, conductive agent, inorganic material powder
Body, binder, lithium salts are mixed according to following mass percent：Graphite：Conductive agent：Inorganic material powder：Binder：Lithium
Salt=60-90：1-5：1-20：1-8：1-10.
Conductive agent includes Surpe-P, acetylene black, KS-6, CNT or graphene.
Inorganic material powder includes lithium lanthanum zirconium tantalum oxygen, Li-La-Ti oxygen or lithium lanthanum zirconium oxygen.
Binder is Kynoar.
Lithium salts includes LiClO4, LiBF4, LiPF6, LiTFSI or LiAsF6.
A kind of preparation method of all-solid lithium-ion battery composite negative pole, includes the following steps：The first step：Prepare slurry
Bonding agent, is dissolved in NMP, adds conductive agent later by material first, after dispersion, glue is formed, by graphite, inorganic particle material
Material, lithium salts are respectively added to carry out disperseing in glue stirring being prepared into negative electrode slurry by a certain percentage；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 8-12 μm of collector, coating thickness is
100-300 μm, the drying temperature of coating machine is 120-135 DEG C, and the pole piece after winding carries out in 100-108 DEG C of vacuum oven
Dry, drying time 18-24h carries out roll-in to the electrode slice after drying, and compacting control is cut in 1.4-1.8mg/cm3
To composite negative pole pole piece；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
Collector is copper foil, utter misery copper foil, porous copper foil or porous utter misery copper foil.
Compared with prior art, what the present invention was reached has the technical effect that：All-solid lithium-ion battery of the present invention is with compound
Cathode is applied to all-solid lithium-ion battery field, it is ensured that battery safety will not cause the safe things such as on fire, explosion
Therefore and it can realize large-scale mass production.
Description of the drawings
Fig. 1 is solid lithium battery 0.05C charge and discharge cycles curves.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and embodiments：
Embodiment one：
A kind of all-solid lithium-ion battery composite negative pole, this composite negative pole include graphite, Surpe-P, lithium lanthanum zirconium oxygen, gather
Vinylidene, LiTFSI are mixed according to following mass percent：Graphite：Surpe-P：Lithium lanthanum zirconium oxygen：Kynoar：
LiTFSI=90：1：2：3：4.
A kind of preparation method of all-solid lithium-ion battery composite negative pole, includes the following steps：The first step：Prepare slurry
Kynoar, is dissolved in NMP, adds Surpe-P later by material first, after dispersion, glue is formed, by graphite, lithium lanthanum zirconium
Oxygen, LiTFSI, which are added to according to the above ratio in glue, disperse stirring being prepared into negative electrode slurry；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 8 μm of copper foil, coating thickness is 100 μm, is applied
The drying temperature of cloth machine is 120 DEG C, and the pole piece after winding is dried in 100 DEG C of vacuum oven, drying time 18h,
Roll-in is carried out to the electrode slice after drying, compacting control exists
1.4mg/cm3, cutting obtain composite negative pole pole piece；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
Compared with prior art, what the present invention was reached has the technical effect that：All-solid lithium-ion battery of the present invention is with compound
Cathode is applied to all-solid lithium-ion battery field, it is ensured that battery safety will not cause the safe things such as on fire, explosion
Therefore and it can realize large-scale mass production.
Embodiment two：
A kind of all-solid lithium-ion battery composite negative pole, this composite negative pole include graphite, CNT, lithium lanthanum zirconium tantalum oxygen, gather partially
Vinyl fluoride, LiAsF6 are mixed according to following mass percent：Graphite：CNT：Lithium lanthanum zirconium tantalum oxygen：Kynoar：
LiAsF6=80：3：10：4：3.
A kind of preparation method of all-solid lithium-ion battery composite negative pole, includes the following steps：The first step：Prepare slurry
Material, Kynoar is dissolved in NMP first, adds CNT later, after dispersion, formed glue, by graphite, lithium lanthanum zirconium tantalum oxygen,
LiAsF6, which is added to according to the above ratio in glue, disperse stirring being prepared into negative electrode slurry；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 9 μm of utter misery copper foil, coating thickness is 160 μ
M, the drying temperature of coating machine are 125 DEG C, and the pole piece after winding is dried in 103 DEG C of vacuum oven, and drying time is
20h carries out roll-in to the electrode slice after drying, and compacting control obtains composite negative pole pole piece in 1.5mg/cm3, cutting；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
Embodiment three：
A kind of all-solid lithium-ion battery composite negative pole, this composite negative pole include graphite, graphene, Li-La-Ti oxygen, gather
Vinylidene, LiClO4 are mixed according to following mass percent：Graphite：Graphene：Li-La-Ti oxygen：Kynoar：
LiClO4=83：2：5：6：4.
A kind of preparation method of all-solid lithium-ion battery composite negative pole, includes the following steps：The first step：Prepare slurry
Kynoar, is dissolved in NMP, adds graphene later by material first, after dispersion, glue is formed, by graphite, Li-La-Ti
Oxygen, LiClO4, which are added to according to the above ratio in glue, disperse stirring being prepared into negative electrode slurry；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 10 μm of porous copper foil, coating thickness 240
μm, the drying temperature of coating machine is 130 DEG C, and the pole piece after winding is dried in 106 DEG C of vacuum oven, and drying time is
22h carries out roll-in to the electrode slice after drying, and compacting control obtains composite negative pole pole piece in 1.6mg/cm3, cutting；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
Example IV：
A kind of all-solid lithium-ion battery composite negative pole, this composite negative pole include graphite, acetylene black, lithium lanthanum zirconium tantalum oxygen,
Kynoar, LiPF6 are mixed according to following mass percent：Graphite：Acetylene black：Lithium lanthanum zirconium tantalum oxygen：Polyvinylidene fluoride
Alkene：LiPF6=60：5：20：5：10.
A kind of preparation method of all-solid lithium-ion battery composite negative pole, includes the following steps：The first step：Prepare slurry
Kynoar, is dissolved in NMP, adds acetylene black later by material first, after dispersion, glue is formed, by graphite, lithium lanthanum zirconium tantalum
Oxygen, LiPF6, which are added to according to the above ratio in glue, disperse stirring being prepared into negative electrode slurry；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 12 μm of porous utter misery copper foil, coating thickness
It it is 300 μm, the drying temperature of coating machine is 135 DEG C, and the pole piece after winding is dried in 108 DEG C of vacuum oven, dry
Time is for 24 hours, to carry out roll-in to the electrode slice after drying, compacting control obtains composite negative pole pole piece in 1.8mg/cm3, cutting；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
Embodiment five：
Wherein in order to verify composite negative pole performance, need to prepare anode composite piece, and by electrolyte slurry coated in compound
Positive plate and composite negative plate surface, and it is overlapped pack, form all-solid-state battery.
Wherein, the preparation method about anode composite piece is as follows：
Anode composite piece is prepared, first, prepares anode sizing agent：It is molten that Kynoar is dissolved in N-Methyl pyrrolidone first
In liquid, carbon nano-fiber is added later, after dispersion, continues to add Surpe-P, later by ternary NCM anodes, lithium lanthanum zirconium tantalum oxygen
And LiTFSI is respectively added to carry out dispersion stirring in glue according to mass ratio, is prepared into anode sizing agent.NCM523：Nano-sized carbon
Fiber：Surpe-P：PVDF：Lithium lanthanum zirconium tantalum oxygen：LiTFSI=86：0.5：1.5：2：5：5；
Secondly, slurry coating：Use coating machine that anode sizing agent is coated on thickness as on 16 μm of aluminium foil, coating thickness is
200 μm, the drying temperature of coating machine is 120 DEG C, and the pole piece after winding is dried in 100 DEG C of vacuum oven, when dry
Between be 18h, roll-in is carried out to the electrode slice after drying, in 2.9mg/cm3, cutting obtains anode composite pole piece for compacting control.
A kind of application of all-solid-state battery composite negative pole, step 1：Electrolyte slurry after preparation is poured over coating
In machine hopper；
Step 2：Start coating machine, adjusts the speed of coating machine, be allowed to that with the speed of 300mm/s chylema will be electrolysed respectively
Surface of the material coated in anode composite piece and composite negative plate adjusts coating height so that coating by adjusting scraper height
Altitude range is 300 μm；
Step 3：Adjust oven temperature at 100 DEG C, to after wet coating anode composite piece and composite negative plate dry
It is roasting；
Step 4：The dry anode composite piece of coating and composite negative plate are wound finally by wind-up roll, then
Size cuts pole piece as desired, for use；
Step 5：In glove box by the anode composite piece of brushing electrolyte slurry layer and composite negative plate carry out lamination,
Assembling obtains solid lithium ion battery, by obtained solid lithium ion battery in 25 DEG C, 0.1C charge and discharge, charge and discharge blanking voltage
4.2V-3.0V charge and discharge cycles test is carried out under conditions of.
Compared with prior art, what the present invention was reached has the technical effect that：All-solid lithium-ion battery of the present invention is with compound
Cathode is applied to all-solid lithium-ion battery field, it is ensured that battery safety will not cause the safe things such as on fire, explosion
Therefore and it can realize large-scale mass 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 (7)
1. a kind of all-solid lithium-ion battery composite negative pole, it is characterised in that：This composite negative pole includes graphite, conductive agent, nothing
Machine material powder, binder, lithium salts are mixed according to following mass percent：Graphite：Conductive agent：Inorganic material powder：It is viscous
Tie agent：Lithium salts=60-90：1-5：1-20：1-8：1-10.
2. a kind of all-solid lithium-ion battery composite negative pole according to claim 1, it is characterised in that：The conductive agent
Including Surpe-P, acetylene black, KS-6, CNT or graphene.
3. a kind of all-solid lithium-ion battery composite negative pole according to claim 1, it is characterised in that：The inorganic material
Feed powder body includes lithium lanthanum zirconium tantalum oxygen, Li-La-Ti oxygen or lithium lanthanum zirconium oxygen.
4. a kind of all-solid lithium-ion battery composite negative pole according to claim 1, it is characterised in that：The binder
For Kynoar.
5. a kind of all-solid lithium-ion battery composite negative pole according to claim 1, it is characterised in that：The lithium salts packet
Include LiClO4, LiBF4, LiPF6, LiTFSI or LiAsF6.
6. a kind of preparation method of all-solid lithium-ion battery composite negative pole, it is characterised in that：Include the following steps：First
Step：Slurry is prepared, bonding agent is dissolved in NMP first, adds conductive agent later, after dispersion, glue is formed, by graphite, nothing
Machine powder body material, lithium salts are respectively added to carry out disperseing in glue stirring being prepared into negative electrode slurry by a certain percentage；
Second step：Use coating machine that negative electrode slurry is coated on thickness as on 8-12 μm of collector, coating thickness 100-300
μm, the drying temperature of coating machine is 120-135 DEG C, and the pole piece after winding is dried in 100-108 DEG C of vacuum oven, is done
The dry time is 18-24h, carries out roll-in to the electrode slice after drying, compacting control obtains compound in 1.4-1.8mg/cm3, cutting
Cathode pole piece；
Third walks：The composite negative plate of cutting is taken out, roll-in, punching are carried out, vacuum preserves.
7. a kind of preparation method of all-solid lithium-ion battery composite negative pole according to claim 6, it is characterised in that：
The collector is copper foil, utter misery copper foil, porous copper foil or porous utter misery copper foil.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109841908A (en) * | 2018-12-20 | 2019-06-04 | 上海力信能源科技有限责任公司 | A kind of high flame retardant preparation method of lithium ion battery |
| CN113851648A (en) * | 2020-06-28 | 2021-12-28 | 宝山钢铁股份有限公司 | Composite negative electrode for solid-state battery, preparation method of composite negative electrode and solid-state battery |
| CN114094110A (en) * | 2022-01-24 | 2022-02-25 | 河南电池研究院有限公司 | Graphite negative electrode for solid lithium ion battery |
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| CN103474620A (en) * | 2013-09-16 | 2013-12-25 | 向勇 | Solid-state lithium ion electrode, solid-state lithium ion battery and preparation method of solid-state lithium ion electrode |
| CN106654276A (en) * | 2016-11-22 | 2017-05-10 | 上海空间电源研究所 | Preparation method of solid-state lithium ion battery electrode taking PEO (Polyethylene Oxide) as binding agent |
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| CN114094110A (en) * | 2022-01-24 | 2022-02-25 | 河南电池研究院有限公司 | Graphite negative electrode for solid lithium ion battery |
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Address after: 215000 3 floors of No. 3 Shengzhao Road, Kunshan Development Zone, Suzhou City, Jiangsu Province Applicant after: Suzhou Qingtao New Energy Technology Co., Ltd. Address before: 215000 Three Floors of Building 3, Dongchuang Science and Technology Center, No. 1 Hongfeng Road, Jinqian East Road Enterprise Science and Technology Park, Kunshan Development Zone, Suzhou City, Jiangsu Province Applicant before: Qing Tao (Kunshan) New Energy Material Research Institute Co., Ltd. |
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Application publication date: 20180928 |