CN100583501C - Lithium ion battery cathode and preparation method thereof - Google Patents
Lithium ion battery cathode and preparation method thereof Download PDFInfo
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- CN100583501C CN100583501C CN200810042492A CN200810042492A CN100583501C CN 100583501 C CN100583501 C CN 100583501C CN 200810042492 A CN200810042492 A CN 200810042492A CN 200810042492 A CN200810042492 A CN 200810042492A CN 100583501 C CN100583501 C CN 100583501C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- 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 Li-ion battery cathode and a preparation method thereof. The cathode consists of a flexible collecting-body layer, a carbon-coated silicon layer and a diaphragm bound together. The flexible collecting-body layer is comprised of acetylene black and binding agent; the carbon-coated silicon layer is comprised of carbon-coated silicon, conducting carbon black and binding agent; the diaphragm is a compound membrane composed of porous polyethylene, porous polypropylene or porous polyethylene-polypropylene. Firstly, the carbon-coated silicon layer, the conducting carbon black and the binding agent are made into slurry, and the slurry is coated on the diaphragm surface and dried to achieve the carbon-coated layer; secondly, the slurry containing acetylene black and binding agent is coated on the surface of carbon-coated silicon layer, and a Li-ion battery cathode is achieved after drying. 1mol/L LiPF6/ EC:DMC (volume ratio) is taken as electrolyte and lithium metal is taken as counter electrode to assemble a Li-ion battery with the cathode; a constant-current charging and discharging test is conducted under 0.2mA/cm<2> current density, the first cycling coulomb efficiency reaches 85 percent, and the reversible capacity can reach 1100mAh/g. To the silicon materials with large-volume variation during the charging and discharging process, the cycling stability of the cathode taking acetylene black as the flexible collecting-body layer is much higher compared with the cycling stability of any traditional cathode taking copper foil as collecting-body.
Description
Technical field
The present invention relates to a kind of battery electrode and preparation method thereof, particularly a kind of lithium ion battery negative and preparation method thereof.
Background technology
The internal structure of lithium ion battery is divided into four parts usually: positive pole, negative pole, barrier film and electrolyte.Wherein just (bear) utmost point and just comprising (bearing) utmost point collector and active material; Barrier film makes electronic isolation between positive/negative plate between positive pole and negative pole, avoid short circuit; Electrolyte mainly is adsorbed in the barrier film, is the carrier that lithium ion moves between positive/negative plate.
Existing lithium ion battery negative is made up of two parts: collector and active material layer.Wherein collector is generally used Copper Foil, and active material layer comprises active material, conductive agent and binding agent.
The conventional method of preparation lithium ion battery negative is generally: active material, conductive agent and binding agent are modulated into slurry in certain proportion, are applied on the collector, obtain lithium ion battery negative after the oven dry.When assembled battery, lithium ion battery negative is what to separate with barrier film, does not bond together.
For lithium ion battery negative material with large volume effect, in charge and discharge process, huge change in volume can take place in negative electrode active material, cause the material efflorescence to be peeled off, lose between the material granule and between the metal collector of material and rigidity and electrically contact, so that charge/discharge capacity sharply descends the very fast inefficacy of battery.For example, the silicon that 2004 the 7th phase A306 of Electrochem.Solid State Lett. magazine page or leaf has been reported 10 microns of particle diameters discharge capacity first is 1170mAh/g, and 10 times the circulation back just decays to less than 200mAh/g.
In order to reduce the bulk effect of silicon, people have attempted preparing the silica-base material of multiple pattern and structure, comprise preparation amorphous si film, nano wire, porous silicon, Si oxide, siliceous nonmetallic compound, silicon/carbon composite, silicon-metal compound (or composite material) or the like, these micro-structural silica-base materials or suppressed its volumetric expansion, perhaps improve electrically contacting of silicon, thereby improved the cyclical stability of silica-base material to a certain extent.For example, 1765 pages of Adv.Funct.Mater. magazine 2007 the 17th 11 phases of volume have reported that a kind of carbon coats silicon, and it is discharge capacity 1200mAh/g nearly first, still keeps the above capacity of 800mAh/g after 20 circulations.
So far, people improve its charge-discharge performance by suppressing the silica-base material bulk effect, do not consider the influence of electrode preparation method, still adopt conventional method mentioned above to prepare lithium ion battery negative.Therefore, be necessary by the structure of improving lithium ion battery negative and the charge-discharge performance that the preparation method improves silica-base material.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery negative and preparation method thereof.
A kind of lithium ion battery negative of the present invention is bonded together by flexible current-collecting body layer, carbon coating silicon layer and barrier film and constitutes;
The thickness of flexible current-collecting body layer is 8～12 microns, form by acetylene black and binding agent, binder content is 6～18wt%, wherein binding agent is butadiene-styrene rubber-sodium carboxymethylcellulose emulsion, its solid content is 0.5wt%～5wt%, the 1-Methyl-2-Pyrrolidone solution of Kynoar, and its concentration is 0.01～0.10g/ml, or acrylic acid aqueous binding agent, its solid content is 1wt%～15wt%;
The thickness that carbon coats silicon layer is 12～25 microns, coating silicon, conductive carbon black and binding agent by carbon forms, conductive carbon black content is 3～6wt%, binder content is 6～12wt%, wherein the particle size range of carbon coating silicon is 60～130 nanometers, the average grain diameter of conductive carbon black is 40 nanometers, binding agent is butadiene-styrene rubber-sodium carboxymethylcellulose emulsion, its solid content is 0.5wt%～5wt%, the 1-Methyl-2-Pyrrolidone solution of Kynoar, its concentration is 0.01～0.10g/ml, or acrylic acid aqueous binding agent, and its solid content is 1wt%～15wt%;
The thickness of barrier film is 18～22 microns, is porous polyethylene, porous polypropylene or porous polyethylene-polypropylene composite film.
Structural group prejudice Fig. 1 of a kind of lithium ion battery negative of the present invention.
The concrete preparation method of a kind of lithium ion battery negative of the present invention is as follows:
(1) the carbon coating silicon with 82～91 weight portions mixes stirring 4～10 hours with conductive carbon black, 6～12 parts by weight of adhesive of 3～6 weight portions, is applied to membrane surface then, 40～50 ℃ of vacuumizes 8～12 hours, obtains carbon and coats silicon layer;
(2) acetylene black of 82～94 weight portions is mixed stirring 4～10 hours with 6～18 parts by weight of adhesive, be coated with or spray to carbon then and coat silicon surface,, obtain a kind of lithium ion battery negative 40～50 ℃ of vacuumizes 8～12 hours.
The particle size range that the carbon that the present invention uses coats silicon is 60～130 nanometers.
The average grain diameter of the conductive carbon black that the present invention uses is 40 nanometers.
The binding agent that the present invention uses is butadiene-styrene rubber-sodium carboxymethylcellulose emulsion, its solid content is 0.5wt%～5wt%, the 1-Methyl-2-Pyrrolidone solution of Kynoar, and its concentration is 0.01～0.10g/ml, or acrylic acid aqueous binding agent, its solid content is 1wt%～15wt%.
The preparation method that the carbon that the present invention uses coats silicon rolled up 1572 pages of the 10th phases referring to chemical journal in 2003 61.
In a kind of lithium ion battery negative of the present invention, carbon coats silicon layer and closely is clipped between flexible barrier film and the flexible current-collecting body layer, has improved the adhesion strength between carbon coating silicon layer and the flexible current-collecting body layer.The flexible current-collecting body layer can coat the deformation of silicon layer and respective change along with carbon, has reduced carbon and has coated mechanical stress between silicon layer and the flexible current-collecting body layer, thereby improved the interface electric contact state, the cyclical stability of carbon coating silicon has been had significantly improve.
With metal lithium sheet is to electrode, and a kind of lithium ion battery negative of the present invention is assembled into lithium ion battery.Contain the electrolyte with lithium salts and solvent composition in the lithium ion battery, its lithium salts comprises lithium hexafluoro phosphate (LiPF
6), LiBF4 (LiBF
4) or lithium perchlorate (LiClO
4) etc. mineral-type salt and biethyl diacid lithium borate (LiBOB), two (trifluoromethane sulfonic acid) imines lithium organic class salt such as (LiTFSI), its solvent comprises at least a in ethylene carbonate (EC), propene carbonate (PC), dimethyl carbonate (DMC) and the diethyl carbonate (DEC), and lithium salt is less than 2mol/L in the electrolyte.At 0.2mA/cm
2Carry out charge-discharge test under the current density, battery first coulombic efficiency reach 85%, 20 time the circulation after reversible capacity be 1100mAh/g.
Comparing traditional is the lithium ion battery negative of collector with the Copper Foil, and a kind of lithium ion battery negative of the present invention has good cycle, the advantage that reversible capacity is big.
Description of drawings
Fig. 1 is a kind of structural representation of lithium ion battery negative.
The charging and discharging curve that the lithium ion battery that Fig. 2 assembles for a kind of lithium ion battery negative that obtains with embodiment 13 times circulates.
Fig. 3 is the capacity-cycle-index curve of preceding 20 circulations of lithium ion battery of a kind of lithium ion battery negative assembling that obtains with embodiment 1.
Fig. 4 obtains for comparative example 1 is the capacity-cycle-index curve of preceding 20 circulations of lithium ion battery of the lithium ion battery negative assembling of collector with the Copper Foil.
Capacity-cycle-index the curve of preceding 20 circulations of lithium ion battery of the lithium ion battery negative assembling that does not contain current collector layers that Fig. 5 obtains for comparative example 2.
Embodiment
Following examples further specify the present invention, but the present invention is not limited to following examples.
In order to illustrate that a kind of lithium ion battery negative of the present invention compares with the lithium ion battery negative that with the Copper Foil is collector, charge-discharge performance is significantly improved, and the spy provides comparative example 1.
In order to illustrate that the flexible current-collecting body layer in a kind of lithium ion battery negative of the present invention plays the effect that improves chemical property, the spy provides comparative example 2.
Battery assembling and method of testing:
The drift of a kind of used as negative electrode of Li-ion battery diameter of the present invention 12～16mm is washed into pole piece, puts into vacuum drying oven and descended dry 8～12 hours, transfer to then in the glove box that is full of argon gas at 40 ℃～60 ℃.With metal lithium sheet is to electrode, and Cellgard 2400 is a barrier film, 1molL
-1The ethylene carbonate of lithium hexafluoro phosphate and dimethyl carbonate (volume ratio 1: 1) mixed solution is an electrolyte, be assembled into the CR2016 button cell, on LAND battery test system (the blue electric Electronics Co., Ltd. in Wuhan provides), carry out the constant current charge-discharge performance test, discharge and recharge cut-ff voltage with respect to Li/Li
+Be 0.01～1.5V, charging and discharging currents density is 0.2mA/cm
2
Embodiment 1
(1) 0.85g carbon is coated silicon and mix stirring 6 hours with 0.05g conductive carbon black, 10g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 1wt%), be applied to the porous polyethylene membrane surface of 20 micron thickness then, obtained carbon in 8 hours 40 ℃ of vacuumizes and coat silicon layer;
(2) 0.9g acetylene black and 10g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 1wt%) are mixed stirring 4 hours, be applied to carbon then and coat silicon surface,, obtain a kind of lithium ion battery negative 50 ℃ of vacuumizes 10 hours.
The lithium ion battery negative that makes is assembled into lithium ion battery carries out charge-discharge test, 3 times charging and discharging curve as shown in Figure 2, preceding 20 times the circulation capacity-the cycle-index curve as shown in Figure 3.Its first charge-discharge coulombic efficiency is that 85%, 20 reversible capacity after the circulation is 1100mAh/g.
(1) 0.85g carbon is coated silicon and mix stirring 8 hours with 0.05g conductive carbon black, 5g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 2wt%), be applied to the porous polyethylene membrane surface of 20 micron thickness then, obtained carbon in 10 hours 50 ℃ of vacuumizes and coat silicon layer;
(2) 0.88g acetylene black and 6g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 2wt%) are mixed stirring 6 hours, evenly spray to carbon then and coat silicon surface,, obtain a kind of lithium ion battery negative 40 ℃ of vacuumizes 12 hours.
The lithium ion battery negative that makes is assembled into lithium ion battery carries out charge-discharge test, the first charge-discharge coulombic efficiency is that 88%, 20 reversible capacity after the circulation is 1000mAh/g.
Embodiment 3
(1) 0.85g carbon is coated silicon and mix stirring 8 hours with the 1-Methyl-2-Pyrrolidone solution (concentration 0.02g/ml) of 0.05g conductive carbon black, 5ml Kynoar, be applied to the porous polyethylene membrane surface of 20 micron thickness then, obtained carbon in 12 hours 40 ℃ of vacuumizes and coat silicon layer;
(2) the 1-Methyl-2-Pyrrolidone solution (concentration 0.02g/ml) with 0.88g acetylene black and 6ml Kynoar mixes stirring 4 hours, is applied to carbon then and coats silicon surface, 40 ℃ of vacuumizes 12 hours, obtains a kind of lithium ion battery negative.
The lithium ion battery negative that makes is assembled into lithium ion battery carries out charge-discharge test, the first charge-discharge coulombic efficiency is that 55%, 20 reversible capacity after the circulation is 900mAh/g.
Comparative example 1
0.85g carbon is coated silicon mix stirring 6 hours with 0.05g conductive carbon black, 10g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 1wt%), be applied to the copper foil surface of 20 micron thickness then, 80 ℃ of vacuumizes 10 hours, obtaining with the Copper Foil was the lithium ion battery negative of collector.
The lithium ion battery negative that makes is assembled into lithium ion battery carries out charge-discharge test, preceding 20 times the circulation capacity-the cycle-index curve as shown in Figure 4.Its first charge-discharge coulombic efficiency is that 81%, 12 reversible capacity after the circulation drops to below the 200mAh/g, and the reversible capacity after 20 circulations decays to 60mAh/g.
Comparative example 2
0.85g carbon is coated silicon mix stirring 6 hours with 0.05g conductive carbon black, 10g butadiene-styrene rubber-sodium carboxymethylcellulose emulsion (solid content 1wt%), be applied to the porous polyethylene membrane surface of 20 micron thickness then, 50 ℃ of vacuumizes 10 hours, do not contained the lithium ion battery negative of current collector layers.
The lithium ion battery negative that makes is assembled into lithium ion battery carries out charge-discharge test, preceding 20 times the circulation capacity-the cycle-index curve as shown in Figure 5.Its first charge-discharge coulombic efficiency is that 36%, 4 reversible capacity after the circulation drops to below the 200mAh/g, and the reversible capacity after 20 circulations decays to 20mAh/g.
Claims (2)
1. lithium ion battery negative is characterized in that coating silicon layer and barrier film by flexible current-collecting body layer, carbon bonds together and constitute;
The thickness of flexible current-collecting body layer is 8～12 microns, form by acetylene black and binding agent, binder content is 6～18wt%, wherein binding agent is butadiene-styrene rubber-sodium carboxymethylcellulose emulsion, its solid content is 0.5wt%～5wt%, the 1-Methyl-2-Pyrrolidone solution of Kynoar, and its concentration is 0.01～0.10g/ml, or acrylic acid aqueous binding agent, its solid content is 1wt%～15wt%;
The thickness that carbon coats silicon layer is 12～25 microns, coating silicon, conductive carbon black and binding agent by carbon forms, conductive carbon black content is 3～6wt%, binder content is 6～12wt%, wherein the particle size range of carbon coating silicon is 60～130 nanometers, the average grain diameter of conductive carbon black is 40 nanometers, binding agent is butadiene-styrene rubber-sodium carboxymethylcellulose emulsion, its solid content is 0.5wt%～5wt%, the 1-Methyl-2-Pyrrolidone solution of Kynoar, its concentration is 0.01～0.10g/ml, or acrylic acid aqueous binding agent, and its solid content is 1wt%～15wt%;
The thickness of barrier film is 18～22 microns, is porous polyethylene, porous polypropylene or porous polyethylene-polypropylene composite film.
2. the preparation method of a kind of lithium ion battery negative as claimed in claim 1 is characterized in that the preparation method is as follows:
(1) the carbon coating silicon with 82～91 weight portions mixes stirring 4～10 hours with conductive carbon black, 6～12 parts by weight of adhesive of 3～6 weight portions, is applied to membrane surface then, 40～50 ℃ of vacuumizes 8～12 hours, obtains carbon and coats silicon layer;
(2) acetylene black of 82～94 weight portions is mixed stirring 4～10 hours with 6～18 parts by weight of adhesive, be coated with or spray to carbon then and coat silicon surface,, obtain a kind of lithium ion battery negative 40～50 ℃ of vacuumizes 8～12 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4068914A3 (en) * | 2009-05-19 | 2022-10-12 | OneD Material, Inc. | Nanostructured materials for battery applications |
| CN102386439B (en) * | 2010-08-31 | 2014-02-12 | 比亚迪股份有限公司 | Lithium ion secondary battery |
| JP6495570B2 (en) * | 2012-03-23 | 2019-04-03 | 株式会社半導体エネルギー研究所 | Power storage device |
| CN104064713A (en) * | 2014-07-10 | 2014-09-24 | 厦门大学 | Composite diaphragm as well as preparation method and application thereof |
| CN105304858B (en) * | 2014-07-10 | 2017-12-12 | 宁德新能源科技有限公司 | Lithium ion battery and its negative plate and preparation method |
| CN104091921A (en) * | 2014-07-22 | 2014-10-08 | 厦门首能科技有限公司 | Porous silicon and carbon mixed anode plate and lithium ion secondary battery comprising same |
| CN104103809B (en) * | 2014-07-31 | 2017-02-01 | 中国科学院上海硅酸盐研究所 | Three-layer electrode structure for alloy anode of lithium ion battery |
| CN105633357B (en) * | 2014-11-11 | 2019-09-17 | 东莞新能源科技有限公司 | Negative electrode active material and preparation method thereof and lithium ion secondary battery |
| CN106025283B (en) * | 2016-05-25 | 2019-05-14 | 华南理工大学 | The aqueous adhesive of lignin-base for negative electrode of lithium ion battery and the electrode slice and lithium ion battery based on it |
| US11081761B2 (en) * | 2016-07-22 | 2021-08-03 | HYDRO-QUéBEC | Flexible electrode-separator elements and processes for their preparation |
| CN106159197A (en) * | 2016-09-30 | 2016-11-23 | 上海空间电源研究所 | A kind of integrated flexible membrane electrode and preparation method thereof |
| CN107069040A (en) * | 2016-12-30 | 2017-08-18 | 深圳市沃特玛电池有限公司 | Electrodes of lithium-ion batteries and preparation method thereof and lithium ion battery |
| CN107565091B (en) * | 2017-08-31 | 2019-12-31 | 浙江大学 | Stretchable electrode of lithium ion battery and preparation method thereof |
| CN108281608A (en) * | 2018-02-07 | 2018-07-13 | 深圳前海优容科技有限公司 | Electrode slice, battery and battery |
| CN111384370B (en) * | 2018-12-29 | 2022-02-25 | 安普瑞斯（南京）有限公司 | High-capacity density lithium ion battery cathode |
| CN112993205B (en) * | 2019-12-14 | 2022-03-08 | 中国科学院大连化学物理研究所 | Elastic electrode constructed by CNT array and preparation and application thereof |
| CN111146428B (en) * | 2020-01-02 | 2021-06-29 | 宁德新能源科技有限公司 | Negative electrode, and electrochemical device and electronic device comprising same |
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