CN110911643B - Diatomite-based lithium ion battery anode material and preparation method thereof - Google Patents
Diatomite-based lithium ion battery anode material and preparation method thereof Download PDFInfo
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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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a diatomite-based lithium ion battery anode material and a preparation method thereof, wherein the anode material is M-SiO formed by filling or coating metal with a porous silicon oxide material by a high-temperature solid-phase self-assembly synthesis method x Composite material, M is one of Sn and Al, siO x Wherein x is more than or equal to 0 and less than or equal to 2, and the lithium ion battery assembled by the negative plate prepared by the negative electrode material has excellent lithium storage performance, cycle life and good rate capability.
Description
Technical Field
The invention relates to the technical field of battery preparation, in particular to a diatomite-based lithium ion battery negative electrode material and a preparation method thereof.
Background
Currently, the lithium ion battery anode materials commercially produced in the market are mainly carbon-based anode materials, including graphite-type and mesophase carbon microsphere-type anode materials. The theoretical capacity of the negative electrode material is about 372 mAh/g, the actual capacity of the negative electrode material reaches 370 mAh/g, and the graphite negative electrode material has almost no lifting space in capacity. Meanwhile, the preparation process of the carbon anode material is slightly complicated. Therefore, it is very necessary to develop a lithium ion battery anode material that has a large theoretical capacity, can be commercialized, and can be mass-produced.
In recent years, a plurality of novel high-capacity and high-rate negative electrode materials are developed and put into production successively, wherein silicon oxide negative electrode materials become hot spots for research because of high theoretical capacity and abundant reserves, wherein the theoretical capacity of SiO is as high as 2800 mAh/g, and the theoretical capacity of SiO is as high as 2800 mAh/g 2 The theoretical capacity of the lithium ion battery anode material is as high as 1965 mAh/g, and the source of the material is wide and the cost is low due to the abundant reserves, so that the silicon oxide material becomes an ideal lithium ion battery anode material.
Some metal elements also possess high theoretical specific capacities, for example Sn can reach 994 mAh/g, al can also reach 2978 mAh/g, and their metallic nature determines that they possess very good electrical conductivity. However, both silicon oxide materials and metal materials have respective disadvantages in the case of being used as negative electrode materials for lithium ion batteries, for example, large volume deformation due to intercalation and deintercalation of lithium ions during charge and discharge, and low conductivity of silicon oxide materials have limited commercial applications.
Patent CN 108075110A discloses preparation of a lithium ion battery anode material of a carbon-coated nano silicon composite anode, and the preparation steps of the composite are complicated, and the obtained target product has larger particles and is not suitable for large-scale commercial production.
Patent CN110165177 a discloses a preparation method of a silicon-based composite anode material of a lithium ion battery, which is to ball-mill silicon and copper oxide to prepare the silicon-based composite anode material, and the material prepared by the method cannot ensure the purity, has low yield and has the defects of poor shape controllability and the like.
Patent CN 108598442A discloses a preparation method of a silicon-based lithium ion battery cathode material, which is to coat graphene oxide with silicon nano particles to form the silicon-based lithium ion battery cathode material, wherein aniline used in the method has toxicity, high production cost and complicated steps, and is not beneficial to large-scale commercial production.
Patent CN 102437318A discloses a silicon-carbon composite lithium ion battery negative electrode material and a preparation method thereof, wherein phenolic resin is coated outside silicon particles, and then the phenolic resin is changed into a coating layer of hard carbon through high-temperature pyrolysis, so that the silicon-carbon negative electrode material with a carbon-coated core-shell structure is obtained. However, the synthetic process of phenolic resin has the defects of high toxicity, high cost and the like, and the carbon hardness obtained by pyrolyzing the resin is high, so that the phenolic resin cannot have good adaptability to the volume change of silicon. Therefore, the cyclic stability of such composites is poor.
Patent CN102983317 a discloses a silicon-carbon composite lithium ion battery anode material and a preparation method thereof, which are characterized in that silicon particles and a precursor of carbon are blended to obtain mixed slurry of the silicon particles and the precursor of carbon, and then high-temperature carbonization is carried out to obtain a silicon-carbon composite. However, the composite obtained by the production process has the defects of uneven silicon distribution, easy agglomeration and the like. Meanwhile, the carbonization temperature is higher, the process difficulty is high, and the production cost is higher.
To date, no research has been seen on the use of metal-filled porous diatomaceous earth as an integral composite system for lithium ion battery anode materials.
Disclosure of Invention
Aiming at the problems in the prior art, the invention discloses a porous silicon oxide negative electrode material formed by uniformly embedding nanoscale metal particles into silicon oxide or coating the metal particles on the surface of the silicon oxide, and a negative electrode plate and a lithium ion battery are prepared based on the porous silicon oxide negative electrode material. According to the invention, the two anode materials which are independently researched before, namely silicon oxide and metal, are firstly placed in a composite system for research, so that the advantages of the two materials are fully exerted, and the defect that the two materials independently form the anode material is overcome.
The technical scheme of the invention is as follows: a lithium ion battery negative electrode material based on diatomite base is M-SiO formed by filling or coating metal with porous silicon oxide material by a high-temperature solid-phase self-assembly synthesis method x Composite material, wherein M is one of Sn and Al, siO x X is more than or equal to 0 and less than or equal to 2.
The preparation method of the diatomite-based lithium ion battery anode material specifically comprises the following steps:
1) Combining a metal source M with porous silicon oxide SiO x Ultrasonic treatment is carried out for 0.5 to 1 h after mixing, so that the mixture is dispersed, and then the mixture is dried in a baking oven at 50 to 80 ℃ to obtain a mixture A;
2) Grinding the mixture A obtained in the step 1 for 10-30 min to ensure that M and SiO in the mixture x Fully contacting to obtain a mixture B;
3) Heating the mixture B obtained in the step 2 to 400-1500 ℃ at a speed of 2-20 ℃/min under the condition of nitrogen, argon or argon-hydrogen mixed gas, preserving heat for 3-10 h, and naturally cooling to obtain a metal-coated silicon oxide anode material C;
in step 1, the metal source is one of simple substance, hydroxide, halide or nitrate compound of Sn, al;
in step 1, the SiO x Refers to a porous silicon oxide material with the grain size of 100 nm-40 um;
in the step (1) of the process,metal source M and porous silicon oxide SiO x The mixed molar ratio of (2) is 1:1 to 10:1.
In step 2, the grinding time is preferably 20 min;
in step 3, the volume content of hydrogen in the argon-hydrogen mixture is 5% -15%, preferably 5%.
The negative plate prepared from the negative material further comprises a conductive agent and a binder, wherein the weight percentage of the negative material is 50-99.5-wt%, the weight percentage of the conductive agent is 0.1-40-wt%, and the weight percentage of the binder is 0.1-40-wt%.
The conductive agent is at least one of carbon black, acetylene black, natural graphite, carbon nano tube, graphene and carbon fiber; the binder is at least one of polytetrafluoroethylene, polyvinylidene fluoride, polyurethane, polyacrylic acid, polyamide, polypropylene, polyvinyl ether, polyimide, styrene-butadiene copolymer and sodium carboxymethyl cellulose.
The lithium ion battery prepared by the negative plate also comprises a positive electrode, a diaphragm and electrolyte.
The positive electrode is a common positive electrode of a lithium battery, and specifically comprises one of lithium cobaltate, lithium manganate, lithium nickelate, lithium iron phosphate, lithium titanate, a nickel-cobalt-manganese ternary system or a lithium composite metal oxide; the membrane comprises one of an aramid membrane, a non-woven membrane, a polyethylene microporous membrane, a polypropylene-polyethylene double-layer or three-layer composite membrane and a ceramic coating membrane; the electrolyte comprises electrolyte and solvent, wherein the electrolyte is LiPF 6 、LiBF 4 、LiClO 4 、LiAsF 6 、LiCF 3 SO 3 、LiN(CF 3 SO 2 ) At least one of LiBOB, liCl, liBr, liI; the solvent comprises at least one of Propylene Carbonate (PC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), 1, 2-Dimethoxyethane (DME), ethylene carbonate, propylene carbonate, butylene carbonate, diethyl carbonate, methyl propyl carbonate, acetonitrile, ethyl acetate and ethylene sulfite.
The beneficial effects of the invention are as follows:
1. according to the invention, sn or Al is creatively filled or coated with diatomite (porous silicon oxide) and then is compounded to form a negative electrode active material, the porous diatomite is taken as a framework, so that the problem of volume expansion of active substances such as Sn, al and the like in the process of charging and discharging lithium can be effectively inhibited, meanwhile, the addition of metal substances can improve the conductivity of the silicon oxide, and the lithium ion battery assembled by the negative electrode plate prepared on the basis of the metal substances has excellent lithium storage performance, cycle life and good multiplying power performance;
2. the preparation of the anode material is completed by adopting a high-temperature solid-phase self-assembly synthesis method, the reaction method is simple and controllable, and the large-scale production can be realized, and the synthesis process is favorable for controlling the cost and commercialized popularization and application.
Drawings
FIG. 1 is a graph showing the electrochemical impedance contrast of the electrodes prepared in example 1 and comparative example 1;
fig. 2 is a charge-discharge curve of the electrode prepared in example 1;
FIG. 3 is a schematic diagram of a negative electrode material formed of metal-clad porous silica;
FIG. 4 is a graph of the ratio performance comparison of tin-filled silica to silica;
fig. 5 is a graph comparing the cycle performance of tin-filled silica to that of silica.
Detailed Description
The following examples further illustrate the invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the present invention without departing from the spirit of the invention are intended to be within the scope of the present invention.
Example 1
6 mmol of diatomite (the diatomite component is porous silicon oxide) and 4 mmol of tin powder are put into ethanol for ultrasonic treatment for 30 minutes, and then the mixture of the silicon oxide and the tin powder is obtained by drying in a 50 ℃ oven. And grinding the mixture in a grinding body for 20 minutes to fully contact the mixture, transferring the ground product into a tube furnace, introducing argon-hydrogen mixed gas (argon 95% and hydrogen 5%) into the tube furnace, heating to 500 ℃ at a heating rate of 10 ℃ per minute, preserving heat for 3 hours, and naturally cooling to obtain the tin-coated silicon oxide anode material.
The invention adopts a high-temperature solid-phase self-assembly synthesis method to prepare the metal-filled or coated porous silicon oxide composite material (M-SiO) x ) The solid phase synthesis method has the advantages of simplicity, mass production and the like, so that the diatomite-based silicon oxide anode material prepared by the method is effectively popularized in future commercial application.
Meanwhile, the metal can automatically perform self-assembly in a high-temperature solid-phase reaction, effective filling is realized in porous diatomite, the porous diatomite is used as a framework, the problem of volume expansion of Sn in the process of charging and discharging lithium can be effectively inhibited, and meanwhile, the addition of a metal substance can improve the conductivity of silicon oxide, so that the mutual cooperation of the metal and the silicon oxide is formed, and the electrochemical energy storage property of a composite system is improved.
The prepared tin-coated silicon oxide active substance, conductive carbon black and adhesive polyvinylidene fluoride are mixed according to the proportion of 8:1:1, and uniformly mixing, preparing negative electrode slurry by taking 1-methyl-2-pyrrolidone as a solvent, coating the negative electrode slurry on copper foil to prepare a negative electrode plate, and drying the negative electrode plate at 50 ℃ overnight. Electrochemical testing was performed using a CR2025 coin cell with an analytically pure metallic lithium sheet as the counter electrode and 1M LiPF as the electrolyte 6 The battery separator was Celgard-2320 (microporous polypropylene film). The assembly of the cell was performed in an argon filled glove box.
Comparative example 1
For comparison with the product of example 1, a comparison test was carried out. In this experiment, the diatomaceous earth used in example 1 was sonicated in ethanol for 30 minutes and dried in a 50 ℃ oven to give silica powder. And then grinding the silicon oxide cathode material in a grinding body for 20 minutes, transferring the ground product into a tube furnace, introducing argon-hydrogen mixed gas (argon 95 percent and hydrogen 5 percent) into the tube furnace, heating to 500 ℃ at the heating rate of 10 ℃ per minute, preserving heat for 3 hours, naturally cooling to obtain the silicon oxide cathode material, and then assembling the battery under the same conditions as in the example 1.
Embodiment two: characterization of negative electrode materials
The electrochemical impedance test is performed on the electrodes prepared in example 1 and comparative example 1, and the results are shown in fig. 1, in which the resistance of the tin-coated silicon oxide is obviously improved, and compared with the resistance of the original silicon oxide, the resistance of the composite material is reduced to about 200Ω, and the resistance is greatly improved.
Fig. 2 is a charge-discharge cycle chart of the electrode prepared in the first embodiment, and it can be seen from the chart that after the porous silica is coated by the metal tin, the first discharge can reach about 380 mAh/g, and the first charge-discharge of the silica is only 150 mAh/g, so that the performance is improved compared with the single silica electrode.
The foregoing has outlined and described the basic principles, features, and advantages of the present invention. However, the foregoing is merely specific examples of the present invention, and the technical features of the present invention are not limited thereto, and any other embodiments that are derived by those skilled in the art without departing from the technical solution of the present invention are included in the scope of the present invention.
Claims (6)
1. A preparation method of a diatomite-based lithium ion battery anode material is characterized in that the anode material is M-SiO formed by filling or coating metal with a porous diatomite material by a high-temperature solid-phase self-assembly synthesis method x Composite material, wherein M is Sn, siO x X is more than or equal to 0 and less than or equal to 2;
the preparation process comprises the following steps:
1) Combining a metal source M with porous silicon oxide SiO x Ultrasonic treatment is carried out for 0.5 to 1 h after mixing, so that the mixture is dispersed, and then the mixture is dried in a baking oven at 50 to 80 ℃ to obtain a mixture A;
2) Grinding the mixture A obtained in the step 1) for 10-30 min to ensure that M and SiO in the mixture x Fully contacting to obtain a mixture B;
3) Heating the mixture B obtained in the step 2) to 500 ℃ at a speed of 10 ℃/min under the condition of argon-hydrogen mixed gas, preserving heat for 3 h, and naturally cooling to obtain a metal-coated silicon oxide anode material C;
the porous silica SiO x Is diatomite;
the porous silica SiO x The particle size of (2) is 100 nm-40 um;
metal source M and porous silicon oxide SiO x The mixed molar ratio of (2) to (3);
the metal source is Sn powder.
2. The preparation method of the diatomite-based lithium ion battery anode material as claimed in claim 1, wherein in the step 3, the hydrogen gas volume content in the argon-hydrogen mixture is 5% -15%.
3. The negative plate prepared from the diatomite-based lithium ion battery negative material is characterized by being prepared from the preparation method of the diatomite-based lithium ion battery negative material according to any one of claims 1-2, and further comprises a conductive agent and a binder, wherein the weight percentage of the negative plate is 50-99.5 wt%, the weight percentage of the conductive agent is 0.1-40 wt%, and the weight percentage of the binder is 0.1-40 wt%.
4. The negative electrode sheet prepared from the diatomite-based lithium ion battery negative electrode material according to claim 3, wherein the conductive agent is at least one of carbon black, acetylene black, natural graphite, carbon nanotubes, graphene, and carbon fibers; the binder is at least one of polytetrafluoroethylene, polyvinylidene fluoride, polyurethane, polyacrylic acid, polyamide, polypropylene, polyvinyl ether, polyimide, styrene-butadiene copolymer and sodium carboxymethyl cellulose.
5. A lithium ion battery is characterized in that the lithium ion battery is prepared based on the negative electrode sheet according to claim 4, and further comprises a positive electrode, a separator and electrolyte.
6. The lithium ion of claim 5A sub-battery characterized in that the positive electrode material comprises one of lithium cobaltate, lithium manganate, lithium nickelate, lithium iron phosphate, lithium titanate, a nickel-cobalt-manganese ternary system, or a composite metal oxide of lithium; the membrane comprises one of an aramid membrane, a non-woven membrane, a polyethylene microporous membrane, a polypropylene-polyethylene double-layer or three-layer composite membrane and a ceramic coating membrane; the electrolyte comprises electrolyte and solvent, wherein the electrolyte is LiPF 6 、LiBF 4 、LiClO 4 、LiAsF 6 、LiCF 3 SO 3 、LiN(CF 3 SO 2 ) At least one of LiBOB, liCl, liBr, liI; the solvent comprises at least one of propylene carbonate, dimethyl carbonate, methyl ethyl carbonate, 1, 2-dimethoxyethane, ethylene carbonate, propylene carbonate, butylene carbonate, diethyl carbonate, methyl propyl carbonate, acetonitrile, ethyl acetate and ethylene sulfite.
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