CN112072110B - Negative electrode, method for producing same, and lithium ion battery using same - Google Patents

Negative electrode, method for producing same, and lithium ion battery using same Download PDF

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CN112072110B
CN112072110B CN202010973378.5A CN202010973378A CN112072110B CN 112072110 B CN112072110 B CN 112072110B CN 202010973378 A CN202010973378 A CN 202010973378A CN 112072110 B CN112072110 B CN 112072110B
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polymer
negative electrode
electrode
active material
thickener
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CN112072110A (en
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魏迪锋
李�昊
孙化雨
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Vision Power Technology Hubei Co ltd
Envision Power Technology Jiangsu Co Ltd
Envision Ruitai Power Technology Shanghai Co Ltd
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Envision Ruitai Power Technology Shanghai Co Ltd
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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • H01M4/0435—Rolling or calendering
    • H—ELECTRICITY
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    • 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
    • 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
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
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    • 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
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • 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
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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Abstract

The application discloses a negative electrode, a preparation method thereof and a lithium ion battery using the same. In the present application, the negative electrode includes: a current collector and a negative active material layer on the current collector, the negative active material layer including: a binder; a conductive agent; a negative electrode active material; and an electrode thickener comprising: deionized water; a first polymer, and a second polymer; the average molecular weight of the first polymer is larger than that of the second polymer, so that the electrochemical performance, particularly the quick charge performance, of the lithium ion battery using the first polymer is remarkably improved under the same energy density, and the aim of improving the charge efficiency can be fulfilled.

Description

Negative electrode, method for producing same, and lithium ion battery using same
Technical Field
The embodiment of the invention relates to the field of lithium ion batteries, in particular to a negative electrode, a preparation method thereof and a lithium ion battery using the negative electrode.
Background
The trend of miniaturization and convenience of electronic equipment is developing, and the lithium ion battery is taken as a main energy storage device of the electronic equipment, and the problem of improving the energy density and the charging efficiency of the lithium ion battery is urgently needed to be solved in the field.
An electrode for a lithium battery is mainly composed of an active material, a conductive agent, a binder, and a current collector. The energy density of a lithium ion battery is related to the activity of the electrode active material inside the battery. A common way to increase the energy density of lithium batteries is to increase the ratio of active material supported on the electrode.
The inventor finds that at least the following problems exist in the prior art:
with the increase of active materials loaded on the electrode, the dynamic diffusion condition of lithium ions in the electrode is worsened, so that the charge and discharge multiplying power of the battery is reduced, and the quick charge performance of the battery is further influenced. Therefore, it is desirable to provide a method for improving the electrochemical performance, especially the quick charge performance, of a battery at the same energy density.
Disclosure of Invention
The invention aims to provide a negative electrode, which can obviously improve the electrochemical performance, particularly the quick charge performance, of a lithium ion battery using the negative electrode under the same energy density, and realize the aim of improving the charge efficiency.
To solve the above technical problem, a first aspect of the present invention provides an anode including: a current collector and a negative active material layer on the current collector, the negative active material layer including: a binder; a conductive agent; a negative electrode active material; and an electrode thickener comprising: deionized water; a first polymer, and a second polymer; wherein the average molecular weight of the first polymer is greater than the average molecular weight of the second polymer.
Compared with the prior art, the anode provided by the first aspect of the invention comprises the following core components: the method comprises the following steps: a current collector and a negative electrode material layer on the current collector, the negative electrode material layer comprising: a binder; a conductive agent; a negative electrode active material; and an electrode thickener comprising: deionized water; a first polymer, and a second polymer; the average molecular weight of the first polymer is larger than that of the second polymer, the first polymer is dissolved in deionized water to form a network structure, the second polymer with smaller average molecular weight is inserted into the network structure formed by the first polymer to fill up gaps formed by the first polymer, and a more compact network structure is formed, so that the negative active material layer has lower porosity and better conductivity, the electrode dynamic condition is improved, the electrochemical performance, particularly the quick charge performance, of the lithium ion battery using the negative active material layer is remarkably improved under the same energy density, and the aim of improving the charge efficiency is fulfilled. In addition, the lithium ion battery using the lithium ion battery also has higher charge-discharge specific capacity, lower impedance, higher charge-discharge multiplying power and better high-low temperature adaptability.
In one embodiment, the average molecular weight of the first polymer is 5 to 100 times the average molecular weight of the second polymer.
In one embodiment, the average molecular weight of the first polymer is 10 to 80 times the average molecular weight of the second polymer.
In one embodiment, the average molecular weight of the first polymer is 20 to 50 times the average molecular weight of the second polymer.
In one embodiment, the first polymer is: at least one of carboxymethyl cellulose or its metal salt, polyacrylic acid, sodium alginate, xanthan gum and guar gum.
In one embodiment, the second polymer is: at least one of carboxymethyl cellulose or metal salt thereof, polyacrylic acid, sodium alginate, xanthan gum and guar gum.
In one embodiment, the molecular weight of the first polymer ranges from 800000 to 10000000; the molecular weight range of the second polymer is 10000-500000.
In one embodiment, the first polymer has a molecular weight in the range of 3000000 to 7000000; the molecular weight range of the second polymer is 100000-300000.
In one embodiment, the molecular weight of the first polymer ranges from 4000000 to 6000000; the molecular weight range of the second polymer is 150000-200000.
In one embodiment, the first polymer and/or the second polymer has a carbon and oxygen backbone comprising at least one hydroxyl group and-COOY, wherein Y is an alkali group element.
In one embodiment, the carbon and oxygen composite backbone comprises repeating units according to formula (I):
Figure BDA0002684898320000021
wherein R is 1 、R 2 、R 3 Selected from hydrogen, C 1-4 Alkyl or alkoxy of C 1-8 An alkylene or alkyleneoxy group, -CH2COOY, -CCH3HCOOY or-CCH 3CH3COOY, wherein Y is an alkali metal group element.
In one embodiment, R is 1 、R 2 、R 3 Selected from hydrogen, C 1-4 or-CH 2COOY, wherein Y is lithium.
In one embodiment, the first polymer n has a value ranging from 8500 to 80000, and the second polymer n has a value ranging from 100 to 3500.
In one embodiment, the first polymer n has a value ranging from 10000 to 40000, and the second polymer n has a value ranging from 500 to 2000.
In one embodiment, in the electrode thickener, the mass percentage of the first polymer is: the mass percentage content ratio of the second polymer is 9:1 to 1: 9.
In one embodiment, in the electrode thickener, the mass percentage of the first polymer is: the mass percentage content ratio of the second polymer is 8:2 to 2: 8.
In one embodiment, in the electrode thickener, the mass percentage of the first polymer and the second polymer is 1.0-3.0%.
In one embodiment, in the electrode thickener, the mass percentage of the first polymer and the second polymer is 1.3 to 1.7%.
In one embodiment, in the electrode thickener, the mass percentage of the deionized water is 95.0-98.0%.
In one embodiment, the viscosity range of the electrode thickener is: 6000 to 8000 mPas.
In one embodiment, the viscosity of the electrode thickener is: 7000 mPas.
In one embodiment, the electrode thickener comprises the following components in percentage by mass: 0.5 to 1.0 percent.
In one embodiment, the negative active material is selected from lithium metal; a lithium alloy; a carbon material capable of deintercalating lithium; tin; tin compounds; silicon; a silicon compound; and a lithium titanate compound.
In one embodiment, in the negative electrode active material layer, the negative electrode active material has a mass percentage content range of: 80-99%.
In one embodiment, the current collector is selected from copper foil; a nickel foil; a stainless steel foil; a titanium foil; a nickel foam; a copper foam; and a polymer material coated with a conductive metal.
In one embodiment, the binder is selected from styrene butadiene rubber; nitrile rubber; butadiene rubber; a modified butadiene rubber; carboxyl modified styrene butadiene rubber; and a modified polyorganosiloxane polymer.
In one embodiment, the conductive agent is selected from natural graphite; artificial graphite; carbon black; acetylene black; carbon fibers; a polyphenylene derivative; and at least one of metal powder or metal fiber containing copper, nickel, aluminum, silver.
In one embodiment, the thickness range of the negative electrode is: 0.130-0.150 mm.
The second aspect of the present invention also provides a method for producing the above-described anode, comprising the steps of:
a. homogenizing: mixing and stirring the binder, the conductive agent, the negative electrode active material, and the electrode thickener to make a slurry; and
b. coating: diluting the slurry obtained in the step a by using deionized water, and then coating the slurry on the current collector to obtain a crude product of the negative electrode; and
c. compacting: and c, compacting the crude product of the cathode in the step b to prepare the cathode.
In one embodiment, the coating is a double-sided coating.
In one embodiment, the coating is performed by a coating machine, and the coating speed is in the range of 0.8-1.2 m/min -1 。
In one embodiment, the compacting is performed by a roller press, and the compacting density is in the range of 1.4-1.8 g/cm -3 The roll-pressing speed is in the range of 0.6-1.0 m/min.
The third aspect of the present invention also provides a lithium battery comprising the above negative electrode, the lithium battery comprising:
the above negative electrode;
a positive electrode;
a diaphragm; and
a non-aqueous electrolyte.
Detailed Description
The embodiment of the invention provides a negative electrode which has lower porosity, better conductivity and better electrode dynamics conditions, and the electrochemical performance, particularly the quick charge performance of a lithium ion battery using the negative electrode is obviously improved under the same energy density, so that the aim of improving the charge efficiency is fulfilled. In addition, the lithium ion battery using the lithium ion battery also has higher charge-discharge specific capacity, lower impedance, higher charge-discharge multiplying power and better high-low temperature adaptability.
A negative electrode provided as a first aspect of the invention includes: a current collector and a negative electrode material layer on the current collector, the negative electrode material layer comprising: a binder; a conductive agent; a negative electrode active material; and an electrode thickener comprising: deionized water; a first polymer; and a second polymer, wherein the average molecular weight of the first polymer is greater than the average molecular weight of the second polymer. The electrode thickener has a more compact cross-linked network structure, the compact cross-linked network structure is formed by dissolving a first polymer and a second polymer in deionized water, and specifically, the second polymer has a shorter skeleton and can be inserted into the network structure formed by the first polymer to fill gaps in the network structure formed by the first polymer, so that the more compact network structure is formed.
Further, in one embodiment, the average molecular weight of the first polymer is 5 to 100 times the average molecular weight of the second polymer.
Further, in one embodiment, the average molecular weight of the first polymer is 10 to 80 times the average molecular weight of the second polymer.
Further, in one embodiment, the average molecular weight of the first polymer is 20 to 50 times the average molecular weight of the second polymer.
In one embodiment, the first polymer is carboxymethyl cellulose or a metal salt thereof, polyacrylic acid (poly (acrylic acid)), Sodium Alginate (Sodium Alginate), Xanthan Gum (Xanthan Gum), Guar Gum (Guar Gum), or a combination thereof; the second polymer is carboxymethyl cellulose or metal salt thereof, polyacrylic acid (poly (acrylic acid)), Sodium Alginate (Sodium Alginate), Xanthan Gum (Xanthan Gum), Guar Gum (Guar Gum) or combination thereof.
Further, in one embodiment, the first polymer and the second polymer are both lithium carboxymethyl cellulose.
Further, in one embodiment, the first polymer and/or the second polymer has a carbon and oxygen backbone comprising at least one hydroxyl group and-COOY, wherein Y is an alkali group element, and in one embodiment, Y is lithium. It is considered that lithium improves lithium ion conduction as compared with other alkali metal elements.
Further, the first polymer has a molecular weight of 800000 to 10000000, and in one embodiment, the first polymer has a molecular weight of 3000000 to 7000000; the second polymer has a molecular weight of 10000 to 500000, and in one embodiment, the second polymer has a molecular weight of 100000 to 300000.
In one embodiment, the carbon and oxygen comprising backbone comprises repeating units according to formula (I):
Figure BDA0002684898320000051
wherein R is 1 、R 2 、R 3 Selected from hydrogen, C 1-4 Alkyl or alkoxy of C 1-8 Alkylene or alkyleneoxy groups of-CH 2COOY, -CCH3HCOOY or-CCH 3CH3COOY, wherein Y is an alkali metal group element; in one embodiment, R 1 、R 2 、R 3 Selected from hydrogen, C 1-4 or-CH 2COOY, wherein Y is lithium. It is considered that lithium improves lithium ion conduction as compared with other alkali metal elements.
In one embodiment, the more dense, inter-linked network structure is chemically inert with respect to lithium ions.
The above is dissolved in deionized water, and it is understood that it is blended in deionized water, and the form of blending may be selected from physical blending.
Further, the n value of the first polymer ranges from 8500 to 80000, and in one embodiment, the n value of the first polymer ranges from 10000 to 40000; the second polymer n has a value ranging from 100 to 3500, and in one embodiment, the second polymer n has a value ranging from 500 to 2000. When the n value of the first polymer is within the range of 8500-80000, the formed network is larger and moderate in viscosity, if the n value of the first polymer exceeds 80000, the material is easy to generate a gel or aggregation phenomenon, and if the n value of the first polymer is less than 8500, a large network structure is difficult to form, and the viscosity is insufficient; when the n value range of the second polymer is 100-3500, the second polymer can better fill up the gaps in the large network structure formed by the first polymer, and is beneficial to forming a more compact mutually-crosslinked network structure, so that the negative electrode active material layer has lower porosity and better conductivity.
Further, the above-mentioned first polymer: the mass percentage of the second polymer is 9:1 to 1:9, and in one embodiment, the ratio of the first polymer: the mass percentage ratio of the second polymer is 8:2 to 2:8, and it is considered that the electrode thickener prepared by the first polymer and the second polymer in the mass percentage range can form a dense and mutually cross-linked network structure relative to the total weight of the electrode thickener, and is helpful for improving the electrochemical performance.
Further, the mass percentage of the first polymer and the second polymer is 1.0 to 3.0% with respect to the total weight of the electrode thickener, and in one embodiment, the mass percentage of the first polymer and the second polymer is 1.3 to 1.7%, and it is considered that the electrode thickener prepared in the mass ratio range of the first polymer and the second polymer can exert a good dispersion thickening effect with respect to the total weight of the electrode thickener, and that when the mass percentage of the first polymer and the second polymer exceeds 3%, the polymer is less dispersed, and when the mass percentage of the first polymer and the second polymer is less than 1%, the dispersion thickening effect is not exerted.
Further, in one embodiment, the deionized water is 95.0 to 98.0% by mass based on the total weight of the electrode thickener.
As the electrode thickener of the present invention, the electrode thickener may be included in a range of 0.5 to 1.0 wt% with respect to the total weight of the negative electrode active material layer, and in one embodiment, the electrode thickener may be included in a range of 0.7 to 0.9 wt% with respect to the total weight of the negative electrode active material layer.
The negative electrode active material of the negative electrode of the present invention is a material capable of inserting and extracting lithium. Including, but not limited to, carbon materials such as crystalline carbon (natural graphite, artificial graphite, and the like), amorphous carbon, carbon-coated graphite, and resin-coated graphite, and oxide materials such as indium oxide, silicon oxide, tin oxide, lithium titanate, zinc oxide, and lithium oxide. The negative electrode active material may also be lithium metal or a metal material that can form an alloy with lithium. Specific examples of metals that can be alloyed with lithium include Cu, Sn, Si, Co, Mn, Fe, Sb, and Ag. Binary or ternary alloys containing these metals and lithium may also be used as the negative electrode active material. These negative electrode active materials may be used alone, or two or more of them may be used in combination. From the viewpoint of high energy density, a carbon material such as graphite and an Si-based active material such as Si, an Si alloy, and an Si oxide may be combined as the negative electrode active material. From the viewpoint of both cycle characteristics and high energy density, graphite and an Si-based active material may be combined as the negative electrode active material. In the combination, the ratio of the mass of the Si-based active material to the total mass of the carbon material and the Si-based active material may be 0.5% to 95%, 1% to 50%, or 2% to 40%. In various embodiments, the negative electrode active material is dispersed in the above-described dense inter-crosslinked network structure.
The content of the negative active material as the negative electrode of the present invention may include 80 to 99 wt% of the negative active material with respect to the total weight of the negative active material layer, and in one embodiment, may include 80 to 96 wt% of the negative active material with respect to the total weight of the negative active material layer. It is considered that when the amount of the anode active material is less than 80 wt%, the negative high capacity cannot be achieved, and when it is more than 99 wt%, the amount of the binder in the anode is insufficient to provide appropriate binding strength between the anode active material and the current collector.
The binder of the negative electrode of the present invention may be at least one selected from styrene-butadiene rubber, nitrile rubber, butadiene rubber, modified butadiene rubber, carboxyl-modified styrene-butadiene rubber, and modified polyorganosiloxane-based polymer.
The conductive agent of the negative electrode of the present invention is a conductive material that does not cause chemical changes, and may be selected from at least one of natural graphite, artificial graphite, carbon black, acetylene black, carbon fiber, polyphenylene derivatives, metal powder containing copper, nickel, aluminum, silver, and metal fiber.
As the current collector of the negative electrode of the present invention, at least one selected from the group consisting of copper foil, nickel foil, stainless steel foil, titanium foil, nickel foam, copper foam, and polymer material coated with conductive metal may be selected.
As a second aspect of the present invention, there is provided a method for producing the anode according to the first aspect of the present invention, comprising the steps of:
a. homogenizing: mixing and stirring the binder, the conductive agent, the negative electrode active material, and the electrode thickener to make a slurry;
b. coating: and diluting the slurry with deionized water, coating the slurry on the current collector, and compacting to prepare the negative electrode.
In one embodiment, the coating is a double-sided coating.
In one embodiment, the coating is performed by a coater at a coating speed ranging from 0.8 to 1.2m/min -1 。
In one embodiment, the compacting is performed by a roller press, and the compacting density is in the range of 1.4 to 1.8g/cm -3 The rolling speed is in the range of 0.6-1.0 m/min.
In one embodiment, the binder is Styrene Butadiene Rubber (SBR), the negative electrode active material is graphite, and the conductive agent is conductive carbon black (Super P).
In one embodiment, the binder, the conductive agent, the negative electrode active material, and the electrode thickener are contained in an amount of 1.8%, 0.8%, 96.6%, and 0.8% by mass, respectively.
A lithium ion battery provided as a third aspect of the invention includes the negative electrode described in the first aspect of the invention; a positive electrode; a diaphragm; and a nonaqueous electrolyte solution.
The positive electrode of the lithium ion battery of the present invention includes a positive electrode active material, and the positive electrode active material may be a lithium-containing composite oxide. Specific examples of the lithium-containing composite oxide include LiMnO 2 、LiFeO 2 、LiMn 2 O 4 、Li 2 FeSiO 4 LiNi 1/3 Co 1/3 Mn 1/3 O 2 、LiNi 5 CO 2 Mn 3 O 2 、Li z Ni (1-x-y) Co x M y O 2 (x, y and z are values satisfying 0.01. ltoreq. x.ltoreq.0.20, 0. ltoreq. y.ltoreq.0.20, and 0.97. ltoreq. z.ltoreq.1.20, M represents at least one element selected from Mn, V, Mg, Mo, Nb and Al), LiFePO 4 And Li z CO (1-x) M x O 2 (x and z are values satisfying 0. ltoreq. x.ltoreq.0.1 and 0.97. ltoreq. z.ltoreq.1.20, M represents at least one element selected from the group consisting of Mn, Ni, V, Mg, Mo, Nb, and Al). Active anodeThe substance may also be Li z Ni (1-x-y) Co x M y O 2 (x, y and z are values satisfying 0.01. ltoreq. x.ltoreq.0.15, 0. ltoreq. y.ltoreq.0.15, and 0.97. ltoreq. z.ltoreq.1.20, M represents at least one element selected from the group consisting of Mn, Ni, V, Mg, Mo, Nb and Al) or Li z CO (1-x) M x O 2 (x and z are values satisfying 0. ltoreq. x.ltoreq.0.1 and 0.97. ltoreq. z.ltoreq.1.20, and M represents at least one element selected from Mn, V, Mg, Mo, Nb, and Al).
The separator of the lithium ion battery of the present invention is not particularly limited, and a single-layer or laminated microporous film, woven fabric, nonwoven fabric, or the like of polyolefin such as polypropylene or polyethylene can be used.
The nonaqueous electrolyte solution for the lithium ion battery of the present invention is not particularly limited, and an electrolyte solution formulation commonly used in the art may be used, and will not be described in detail herein.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be described in detail with reference to experimental examples. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present application in various embodiments of the present invention. However, the technical solution claimed in the present application can be implemented without these technical details and various changes and modifications based on the following embodiments.
[ PREPARATION EXAMPLES ] preparation of electrode thickener
Preparation of lithium carboxymethyl cellulose (Mw 1000000):
the method comprises the following steps: taking cellulose raw materials (refined cotton, wood pulp and the like) with the molecular weight range of 1000000, adding sodium hydroxide for alkalization, adding monochloroacetic acid for reaction, adding an acetic acid solution, reacting in a mixed solution of ethanol and water for 2 hours at 35 ℃, filtering, repeatedly washing by using the mixed solvent to obtain purified carboxymethyl cellulose, placing the prepared carboxymethyl cellulose in a mixed solution of ethanol and water, reacting with 7 wt% of LiOH for 2 hours at 50 ℃, adding acetic acid for regulating the pH value to x, and obtaining the carboxymethyl cellulose lithium with the molecular weight of 1000000.
The method 2 comprises the following steps: taking a cellulose raw material (refined cotton, wood pulp and the like) with the molecular weight range of 1000000, dispersing the cellulose raw material in a mixed solution of isopropanol and distilled water, adding lithium hydroxide, stirring overnight, dropwise adding monochloroacetic acid, heating at 55 ℃ for 5 hours, and cooling to room temperature. Filtered, washed with distilled water, dissolved in distilled water and neutralized with acetic acid. Adding isopropanol, filtering to separate precipitate, and oven drying at 55 deg.C overnight to obtain purified lithium carboxymethylcellulose with molecular weight of 1000000.
Preparation of lithium carboxymethyl cellulose (Mw 400000):
taking cellulose raw material (refined cotton, wood pulp and the like) with the molecular weight range of 40000, adding sodium hydroxide for alkalization, adding monochloroacetic acid for reaction, and then adding 20 wt% HCl solution or 50 wt% H 2 SO 4 Reacting the mixed solution of ethanol and water for 2 hours at 35 ℃, repeatedly washing the mixed solution of ethanol and water, filtering the precipitate, placing the precipitate in the mixed solution of ethanol and water, reacting the precipitate with 7 wt% of LiOH at 50 ℃ for 2 hours, and adjusting the pH value of the solution by using acetic acid to obtain the carboxymethyl cellulose lithium with the molecular weight of 400000.
Preparation of electrode thickener:
the electrode thickener is prepared by blending and uniformly stirring carboxymethyl cellulose lithium with the molecular weight of 1000000, carboxymethyl cellulose lithium with the molecular weight of 400000 and deionized water, and the mass percentages of the carboxymethyl cellulose lithium with the molecular weight of 1000000, the carboxymethyl cellulose lithium with the molecular weight of 400000 and the deionized water in each example and comparative example are shown in table 1.
TABLE 1
Figure BDA0002684898320000091
[ COMPARATIVE EXAMPLES ]
Mixing carboxymethyl cellulose lithium with the molecular weight of 1000000, carboxymethyl cellulose lithium with the molecular weight of 400000 and carboxymethyl cellulose lithium with the molecular weight of 400000 with deionized water according to the proportion in the table 2, and uniformly stirring.
TABLE 2
Figure BDA0002684898320000092
[ PREPARATION EXAMPLES ] preparation of negative electrode
Example 6
a. Homogenizing: 571 parts of the electrode thickening agent prepared in example 1 and 8 parts of the conductive agent are dispersed and mixed to form 579 parts of conductive adhesive, 579 parts of conductive adhesive and 966 parts of graphite are mixed and stirred for 60min (revolution 20rpm and rotation 800rpm) to form slurry, 300 parts of deionized water is added to adjust the solid content to about 53%, the mixture is continuously stirred for 90min (revolution 35rpm, rotation 2500rpm and vacuum degree of-90 kPa), and finally 45 parts of SBR emulsion is added and stirred for 30min (revolution 20rpm, rotation 800rpm and vacuum degree of-90 kPa), so that the homogenizing process is completed.
b. Coating: coating the slurry on a copper foil by a coating machine, wherein the foil is coated on two sides, the density of the coated side is controlled to be about 10mg cm < -2 >, the coating speed is 1m/min < -1 >, and the temperature of two sections of drying ovens is maintained to be about 65 ℃ and 80 ℃.
c. Compacting: the rolling is carried out by a rolling machine, the rolling speed is 0.8m/min, the rolling tonnage is continuously changed, the rolled thickness of the pole piece is about 0.142mm, and the compaction density is controlled to be 1.6g/cm -3 。
In other examples and comparative examples, negative electrodes were prepared in the same manner as in example 6, except that electrode thickeners were used differently, as specified in table 3 below:
TABLE 3
Source of electrode thickener
Example 6 Example 1
Example 7 Example 2
Example 8 Example 3
Example 9 Example 4
Example 10 Example 5
Comparative example 4 Comparative example 1
Comparative example 5 Comparative example 2
Comparative example 6 Comparative example 3
[ test examples ] to test
Slurry viscosity test
The slurries prepared in the homogenization procedure of example 6, example 7, example 8, example 9, example 10, comparative example 4, comparative example 5, and comparative example 6, step a were placed in a Brookfield rotational viscometer for viscosity measurement (63# spindle, 12r/min) and the results are shown in Table 4.
TABLE 4
viscosity/m.Pa.s
Example 6 7000
Example 7 7123
Example 8 7098
Example 9 6867
Example 10 6990
Comparative example 4 13407
Comparative example 5 8703
Comparative example 6 4348
Slurry fineness test
The slurries prepared in the homogenization process of step a of example 6, example 7, example 8, example 9, example 10, comparative example 4, comparative example 5 and comparative example 6 were taken and placed in a fineness tester to measure the particle size, and the results are shown in table 5.
TABLE 5
Fineness/um
Example 6 20
Example 7 20
Example 8 20
Example 9 20
Example 10 20
Comparative example 4 35
Comparative example 5 30
Comparative example 6 30
Analysis of the above experimental data shows that the electrode thickener of the present invention has lower fineness and is more favorable for uniform slurry distribution than slurry prepared from an electrode thickener prepared from lithium carboxymethylcellulose having a molecular weight of 400000, a molecular weight of 700000, and a molecular weight of 1000000 under the same conditions.
[ test examples ] evaluation of Battery Performance
Specific charge-discharge capacity and first coulombic efficiency test
The negative electrodes of example 6, example 7, example 8, example 9, example 10, comparative example 4, comparative example 5 and comparative example 6 were assembled with a positive electrode, a separator and a nonaqueous electrolytic solution according to a method known to those skilled in the art to form a battery (a small pouch battery using a 1Ah lamination process), and the specific discharge capacity and specific charge capacity of the battery were measured to calculate the first coulombic efficiency, and the results are shown in table 6.
TABLE 6
Specific discharge capacity/mAh g-1 Specific charging capacity/mAh g-1 First coulombic efficiency
Example 6 380.6 353 92.77％
Example 7 382.7 355 92.76％
Example 8 381.6 352.8 92.45％
Example 9 380.3 353.9 93.06％
Example 10 377.1 349.5 92.68％
Comparative example 4 366.8 339.1 92.45％
Comparative example 5 370.3 338.75 91.48％
Comparative example 6 379.3 341.5 90.03％
Analysis of the above experimental data shows that the first coulombic efficiency of the electrode thickener according to the present invention is higher than that of a slurry prepared from an electrode thickener prepared from lithium carboxymethylcellulose having a molecular weight of 400000, a molecular weight of 700000, and a molecular weight of 1000000 under the same conditions.
DC internal resistance test
The negative electrodes of example 6, example 7, example 8, example 9, example 10, comparative example 4, comparative example 5, and comparative example 6 were assembled with a positive electrode, a separator, and a nonaqueous electrolytic solution to form a battery according to a method known to those skilled in the art, and the aforementioned battery was subjected to a direct current internal resistance test (1Ah laminate process small pouch battery, 4C discharge at 50% SOC for 30s), and the results are shown in table 7.
TABLE 7
DC internal resistance/m omega
Example 6 90.3
Example 7 91.1
Example 8 90.4
Example 9 89.7
Example 10 90.9
Comparative example 4 111.3
Comparative example 5 98.8
Comparative example 6 97.9
Analysis of the above experimental data shows that the electrode thickener of the present invention has lower direct current resistance than a slurry prepared using an electrode thickener prepared using lithium carboxymethylcellulose having a comparative molecular weight of 400000, a molecular weight of 700000, and a molecular weight of 1000000 under the same conditions.
Rate charge capacity retention rate test
The negative electrodes of examples 6, 7, 8, 9, 10, 4, 5 and 6 were assembled with a positive electrode, a separator and a nonaqueous electrolytic solution to form a battery according to a method known to those skilled in the art, and the battery was subjected to a rate charge capacity retention rate test, and the results are shown in table 8.
TABLE 8
Figure BDA0002684898320000131
Analysis of the experimental data shows that the electrode thickener of the present invention has a higher rate charge capacity retention rate and better fast charge performance than a slurry prepared from an electrode thickener prepared from lithium carboxymethylcellulose having a comparative molecular weight of 400000, a molecular weight of 700000, and a molecular weight of 1000000 under the same conditions.
High and Low temperature Performance test
The negative electrodes of examples 6, 7, 8, 9, 10, 4, 5 and 6 were assembled with a positive electrode, a separator and a nonaqueous electrolytic solution to form a battery according to a method known to those skilled in the art, and the battery was subjected to high and low temperature performance tests (retention rate of discharge capacity of the battery at different temperatures when discharged at 0.33C with respect to the normal temperature) and the results are shown in table 9.
TABLE 9
-25℃ -20℃ 0℃ 25℃ 50℃
Example 6 70.1％ 74.3％ 91.2％ 100％ 99.5％
Example 7 70.3％ 74.5％ 90.9％ 100％ 100.2％
Example 8 69.8％ 75％ 90.7％ 100％ 100.1％
Example 9 70.5％ 74.7％ 90.3％ 100％ 99.6％
Example 10 70.2％ 74.9％ 90.8％ 100％ 99.8％
Comparative example 4 65.9％ 71.1％ 90％ 100％ 101.5％
Comparative example 5 66.6％ 70.7％ 89％ 100％ 102％
Comparative example 6 67％ 70.9％ 90.2％ 100％ 101.3％
Analysis of the above experimental data shows that the electrode thickener of the present invention has better high and low temperature performance than the slurry prepared from the electrode thickener prepared from lithium carboxymethylcellulose having a molecular weight of 400000, a molecular weight of 700000, and a molecular weight of 1000000 under the same conditions.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.

Claims (18)

1. An anode, comprising: a current collector and a negative active material layer on the current collector, the negative active material layer including: a binder; a conductive agent; a negative electrode active material; and an electrode thickener comprising:
deionized water;
a first polymer; and
a second polymer;
wherein the average molecular weight of the first polymer is larger than that of the second polymer, and the molecular weight of the first polymer ranges from 800000 to 1000000; the molecular weight range of the second polymer is 400000-500000;
the first polymer and the second polymer are both lithium carboxymethyl cellulose;
the first polymer: the mass percentage content ratio of the second polymer is 1: 2.5-2: 8.
2. The negative electrode according to claim 1, wherein the mass of the first polymer and the second polymer in the electrode thickener is 1.0 to 3.0% of the total mass of the electrode thickener.
3. The negative electrode according to claim 1, wherein the mass of the first polymer and the second polymer in the electrode thickener is 1.3 to 1.7% of the total mass of the electrode thickener.
4. The negative electrode of claim 1, wherein the deionized water is present in the electrode thickener in an amount of 95.0 to 98.0% by mass.
5. The anode of claim 1, wherein the electrode thickener has a viscosity in the range of: 6000 to 8000mPa s.
6. The anode of claim 1, wherein the electrode thickener has a viscosity of: 7000 mPas.
7. The negative electrode of claim 1, wherein the electrode thickener is present in the following range in percentage by mass: 0.5 to 1.0 percent.
8. The anode according to claim 1, wherein the anode active material is selected from the group consisting of lithium metal; a lithium alloy; a carbon material capable of lithium deintercalation; tin; tin compounds; silicon; a silicon compound; and a lithium titanate compound.
9. The negative electrode according to claim 1, wherein the negative electrode active material layer contains the negative electrode active material in the following range in percentage by mass: 80-99%.
10. The negative electrode of claim 1, wherein the current collector is selected from the group consisting of copper foil; a nickel foil; a stainless steel foil; a titanium foil; a nickel foam; a copper foam; and a polymer material coated with a conductive metal.
11. The negative electrode of claim 1, wherein the binder is selected from styrene butadiene rubber; nitrile rubber; butadiene rubber; a modified butadiene rubber; carboxyl modified styrene-butadiene rubber; and a modified polyorganosiloxane polymer.
12. The negative electrode of claim 1, wherein the conductive agent is selected from natural graphite; artificial graphite; carbon black; carbon fibers; a polyphenylene derivative.
13. The anode of claim 1, wherein the anode has a thickness in a range of: 0.130-0.150 mm.
14. A method of preparing the anode of any one of claims 1 to 13, comprising the steps of:
a. homogenizing: mixing and stirring the binder, the conductive agent, the negative electrode active material, and the electrode thickener to make a slurry; and
b. coating: diluting the slurry obtained in the step a by using deionized water, and then coating the slurry on the current collector to obtain a crude product of the negative electrode; and
c. compacting: and c, compacting the crude product of the cathode in the step b to prepare the cathode.
15. The method of claim 14, wherein the coating is a double-sided coating.
16. The method of claim 14, wherein the coating is performed by a coater at a speed ranging from 0.8 to 1.2m/min -1 。
17. The method of claim 14, wherein the compacting is performed by a roller press and the compaction density is in the range of 1.4 to 1.8g/cm -3 The rolling speed range is 0.6-1.0 m/min.
18. A lithium battery, characterized in that the lithium battery comprises:
the negative electrode according to any one of claims 1 to 13;
a positive electrode;
a diaphragm; and
a non-aqueous electrolyte.
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