CN116885146B - Battery negative electrode active material, preparation method and application thereof - Google Patents
Battery negative electrode active material, preparation method and application thereof Download PDFInfo
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- CN116885146B CN116885146B CN202311058111.3A CN202311058111A CN116885146B CN 116885146 B CN116885146 B CN 116885146B CN 202311058111 A CN202311058111 A CN 202311058111A CN 116885146 B CN116885146 B CN 116885146B
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- sulfur compound
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- 239000007773 negative electrode material Substances 0.000 title claims description 10
- 238000002360 preparation method Methods 0.000 title abstract description 15
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 102000005298 Iron-Sulfur Proteins Human genes 0.000 claims abstract description 27
- 108010081409 Iron-Sulfur Proteins Proteins 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000011149 active material Substances 0.000 claims abstract description 13
- 239000006183 anode active material Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 70
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 claims description 8
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000006258 conductive agent Substances 0.000 claims description 5
- 239000010405 anode material Substances 0.000 claims description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 3
- 229910001416 lithium ion Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000006182 cathode active material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229960004887 ferric hydroxide Drugs 0.000 abstract description 13
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 abstract description 13
- 239000011247 coating layer Substances 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000011056 performance test Methods 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 239000006230 acetylene black Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
Classifications
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 relates to a battery anode active material, a preparation method and application thereof. The method comprises the steps of in-situ generation of ferric hydroxide on the surface of an iron-sulfur compound by wet ball milling, forming of a ferric hydroxide coated iron-sulfur compound active material, and the preparation process comprises the steps of feeding, ball milling, drying and the like. According to the invention, through a wet ball milling mode, the coating layer ferric hydroxide can be formed on the surface of the iron-sulfur compound in situ, the method is simple to operate, the preparation efficiency is higher, the ferric hydroxide coating layer can be formed rapidly, the preparation period is shortened, and through an electrochemical performance test, the battery taking the ferric hydroxide as the anode active material has better electrochemical performance, and the circulation stability and the multiplying power performance are improved.
Description
Technical Field
The invention relates to the technical field of battery cathode materials.
Background
Pyrite is abundant in the surface, and has the advantages of low price, convenient exploitation, environmental protection and the like. When pyrite is used as electrode material, it has higher charge-discharge specific capacity, long storage time and wider temp. range, but its volume change is larger in the course of circulation, so that it can solve the defects of poor rate performance and circulation stability and low coulombic efficiency, and can solve the problems of poor circulation stability and poor storage of iron-sulfur compound negative electrode in the prior artThe problem of low efficiency is mainly that a carbon coating method is adopted, for example, a hydrothermal method is adopted to prepare the reduced graphene oxide coated FeS 2 (FeS 2 rGO), but the preparation period of the hydrothermal method is long, so that large-scale or large-batch production is difficult to realize, and the coating material has high cost and severe process conditions, and is not beneficial to industrialization.
Disclosure of Invention
The invention provides a battery anode active material, a preparation method and application thereof, and aims to solve the technical problems that a carbon coating method is not beneficial to industrialization and has poor conductive effect in the prior art.
The technical scheme adopted by the invention for achieving the purpose is as follows: a battery negative electrode active material comprises ferric hydroxide and an iron-sulfur compound, wherein the ferric hydroxide is uniformly coated on the surface of the iron-sulfur compound.
The iron-sulfur compound is FeS, fe 2 S 3 、FeS 2 One or more of them.
The invention also provides a preparation method of the battery anode active material, which comprises the following steps:
s1: putting iron-sulfur compound powder, zirconia balls and deionized water into a ball milling tank;
s2: starting the ball mill, and performing ball milling.
S3: after ball milling is completed, the obtained iron-sulfur compound powder coated by the iron oxyhydroxide is put into a blast drying oven for drying;
s4: and (5) drying to obtain iron-sulfur compound powder coated by the iron oxyhydroxide.
The iron-sulfur compound in the step S1 is FeS, fe 2 S 3 、FeS 2 One or more of the iron-sulfur compounds has a particle size of 0.1-100 μm.
In the step S1, the mass ratio of the iron-sulfur compound, the deionized water and the zirconia balls is as follows: 1:10-20:10-70.
The zirconia balls in the step S2 comprise 10-millimeter-diameter zirconia balls and 5-millimeter-diameter zirconia balls, and the mass ratio of the 10-millimeter-diameter zirconia balls to the 5-millimeter-diameter zirconia balls is as follows: 2-5:1.
The ball milling time in the step S4 is 30-60 minutes, and the rotating speed of the ball mill is 300-600rpm.
In the step S6, the drying temperature is 70-90 ℃ and the drying time is 6-12 hours.
The invention also provides a battery anode material which comprises the active material, a conductive agent and a binder, wherein the mass ratio of the active material to the conductive agent to the binder is 8-9:1-0.5:1-0.5.
The invention also provides a lithium ion battery, which comprises the battery anode material.
The method has the advantages that the coating layer ferric hydroxide can be formed on the surface of the iron-sulfur compound in situ by a wet ball milling method, the method is simple to operate, the preparation efficiency is higher, the ferric hydroxide coating layer can be formed rapidly, the preparation period is shortened, and the electrochemical performance test shows that the battery taking the ferric hydroxide as the anode active material has better electrochemical performance, and the cycle stability and the multiplying power performance are improved.
Drawings
Fig. 1 is an X-ray diffraction pattern of the active material in example 1, a method of preparing a battery anode active material according to the present invention.
Fig. 2 is an SEM and elemental distribution diagram of the active material in example 1 of the preparation method of the battery anode active material of the present invention.
Fig. 3 is a graph showing electrochemical cycle performance of the active material of example 1 according to the preparation method of the battery anode active material of the present invention.
Fig. 4 is a graph showing electrochemical cycle performance of the active material in example 2, which is a preparation method of the negative electrode active material for a battery according to the present invention.
FIG. 5 is a graph showing electrochemical cycle performance of the active material of example 3 according to the preparation method of the negative electrode active material of the battery of the present invention
Detailed Description
The embodiment provides a battery anode active material, which comprises ferric hydroxide and an iron-sulfur compound, wherein the ferric hydroxide is uniformly coated on the surface of the iron-sulfur compound, and the iron-sulfur compound is FeS or Fe 2 S 3 、FeS 2 One or more of them；
A method for preparing a battery anode active material, comprising the steps of:
example 1: s1: feS is carried out 2 Placing the powder, zirconia balls and deionized water into a ball milling tank, and FeS 2 Has a particle size of 0.1-100 μm, feS 2 The mass ratio of deionized water to zirconia balls is as follows: the zirconia balls comprise 10-millimeter-diameter zirconia balls and 5-millimeter-diameter zirconia balls, and the mass ratio of the 10-millimeter-diameter zirconia balls to the 5-millimeter-diameter zirconia balls is as follows: 2:1;
s2: the ball mill was started and ball milling was carried out for 30 minutes at 600rpm.
S3: after ball milling, putting the iron-sulfur compound powder coated by the obtained iron oxyhydroxide into a blast drying oven for drying at 70-90 ℃ for 6-12 hours;
s4: drying is completed, and iron-sulfur compound powder coated by iron oxyhydroxide is obtained;
electrochemical performance test:
mixing the prepared active material with acetylene black and polyvinylidene fluoride according to the mass ratio of 8:1:1 to prepare slurry, uniformly coating the slurry on aluminum foil, vacuum drying at 90 ℃ for 10 hours, and stamping the slurry into a round electrode plate with the diameter of 12 mm, wherein a lithium metal plate is used as an anode, and 1mol/LLiPF is used as a cathode 6 The electrolyte/(EC+DEC) (volume ratio 1:1) is electrolyte, celgard 2300 is diaphragm, CR2032 button cell is assembled in a glove box filled with argon, electrochemical test is carried out at room temperature after the cell is taken out, and the charging and discharging voltage range of the cell is 1-2.7V, and the current density is 1000mA.g -1 Under the condition (figure 3), the specific capacity of the first-turn discharge is 341.26mAh.g -1 The specific charge capacity is 335.80mAh.g -1 The reversible specific capacity after 300 times of circulation is 369.45mAh.g -1 The coulombic efficiency was 99.78%.
Example 2: the present example is similar to example 1, except that in S1, feS, zirconia balls and deionized water are placed in a ball milling tank, and the mass ratio of FeS, deionized water and zirconia balls is: 1:20:70, wherein the zirconia balls comprise 10-millimeter-diameter zirconia balls and 5-millimeter-diameter zirconia balls, and the mass ratio of the 10-millimeter-diameter zirconia balls to the 5-millimeter-diameter zirconia balls is as follows: 3:1, ball milling time in S2 is 40 minutes, and the rotation speed of the ball mill is 500rpm.
Mixing the prepared active material with acetylene black and polyacrylic acid according to the mass ratio of 9:0.5:0.5 to prepare slurry, uniformly coating the slurry on aluminum foil, vacuum drying at 70 ℃ for 12 hours, stamping the slurry into a round electrode plate with the diameter of 12 mm, and taking a lithium metal plate as a positive electrode and 1mol/L LiClO (LiClO) 4 And (2) assembling a CR2025 button cell by using an (EC+DMC) electrolyte (volume ratio of 1:1) as an electrolyte and Celgard 2300 as a diaphragm in a glove box filled with argon, taking out, performing electrochemical test at room temperature, wherein the charge-discharge voltage range of the cell is 1-2.7V, and the current density is 1000mA g -1 Under the condition (figure 4), the specific capacity of the first-turn discharge is 238.40mAh.g -1 The specific charge capacity is 231mAh.g -1 The reversible capacity after 300 times of circulation is 255.08mAh.g -1 The coulombic efficiency was 100.16%.
Example 3: this example is substantially the same as example 1, except that FeS is used in S1 2 Placing the mixture of FeS, zirconia balls and deionized water into a ball milling tank, and FeS 2 The mass ratio of the FeS mixture, the deionized water and the zirconia balls is as follows: the zirconia balls comprise 10 mm diameter zirconia balls and 5 mm diameter zirconia balls, and the mass ratio of the 10 mm diameter zirconia balls to the 5 mm diameter zirconia balls is as follows: ball milling time in S2 is 60 minutes in 5:1, and ball mill rotating speed is 300rpm
Mixing the prepared iron-sulfur compound coated with the ferric hydroxide, acetylene black and polyacrylic acid (PAA) according to the mass ratio of 8:1:1 to prepare slurry, uniformly coating the slurry on aluminum foil, vacuum drying the slurry at 70 ℃ for 6 hours, stamping the slurry into a round electrode plate with the diameter of 12 mm, and taking a lithium metal plate as an anode and 1mol/LF 2 LiNO 4 S 2 the/(DOL+DEC) electrolyte (volume ratio 1:1) is electrolyte, celgard 2300 is diaphragm, and the CR2025 button cell is assembled in a glove box filled with argon, taken out and subjected to electrochemical test at room temperature. The charge-discharge voltage range of the battery is 1-2.7V, and the current density is 2000mA.g -1 Under the condition (figure 5), the specific capacity of the first-turn discharge is 182.04mAh.g -1 The specific charge capacity was 173.14mAh.g -1 The reversible capacity after 300 times of circulation is 183.22mAh.g -1 The coulombic efficiency was 99.82%.
A battery cathode material comprises the active material, a conductive agent and a binder.
A lithium ion battery comprises the negative electrode material.
The present invention has been described in terms of embodiments, and it will be appreciated by those of skill in the art that various changes can be made to the features and embodiments, or equivalents can be substituted, without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The battery cathode active material is characterized by comprising iron oxyhydroxide and an iron sulfur compound, wherein the iron oxyhydroxide is uniformly coated on the surface of the iron sulfur compound.
2. The negative electrode active material for a battery according to claim 1, wherein the iron-sulfur compound is FeS, fe 2 S 3 、FeS 2 One or more of them.
3. A method for preparing a battery anode active material, comprising the steps of:
s1: putting iron-sulfur compound powder, zirconia balls and deionized water into a ball milling tank;
s2: starting the ball mill, and performing ball milling;
s3: after ball milling is completed, the obtained iron-sulfur compound powder coated by the iron oxyhydroxide is put into a blast drying oven for drying;
s4: and (5) drying to obtain iron-sulfur compound powder coated by the iron oxyhydroxide.
4. The method for preparing a negative electrode active material for a battery according to claim 3, wherein the iron-sulfur compound in step S1 is FeS or Fe 2 S 3 、FeS 2 One or more of the iron-sulfur compounds has a particle size of 0.1-100 μm.
5. The method for preparing a battery anode active material according to claim 3, wherein in the step S1, the mass ratio of the iron-sulfur compound, deionized water, and zirconia balls is: 1:10-20:10-70.
6. The method for producing a battery anode active material according to claim 3, wherein the zirconia balls in step S2 comprise 10 mm diameter zirconia balls and 5 mm diameter zirconia balls, and the mass ratio of the 10 mm diameter zirconia balls to the 5 mm diameter zirconia balls is: 2-5:1.
7. The method for preparing a negative electrode active material for a battery according to claim 3, wherein the ball milling time in the step S4 is 30 to 60 minutes, and the rotational speed of the ball mill is 300 to 600rpm.
8. The method for preparing a negative electrode active material for a battery according to claim 3, wherein the drying temperature in step S6 is 70 ℃ to 90 ℃ and the drying time is 6 to 12 hours.
9. A battery anode material, which is characterized by comprising the active material of claim 1, and further comprising a conductive agent and a binder, wherein the mass ratio of the active material, the conductive agent and the binder is 8-9:1-0.5:1-0.5.
10. A lithium ion battery comprising the battery anode material of claim 9.
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| CN111129469A (en) * | 2019-12-31 | 2020-05-08 | 天目湖先进储能技术研究院有限公司 | FexOy-FeS2-zComposite material and preparation method and application thereof |
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