CN110911643A - Diatomite-based lithium ion battery negative electrode material and preparation method thereof - Google Patents
Diatomite-based lithium ion battery negative electrode material and preparation method thereof Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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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
- H01M4/134—Electrodes based on metals, Si or alloys
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- 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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a diatomite-based lithium ion battery cathode material and a preparation method thereof, wherein the cathode material is M-SiO formed by filling or coating a porous silicon oxide material with metal by a high-temperature solid-phase self-assembly synthesis methodxM is one of Sn and Al, SiOxAnd x is more than or equal to 0 and less than or equal to 2, and the lithium ion battery assembled by the negative pole pieces prepared by the negative pole material has excellent lithium storage performance, cycle life and good rate performance.
Description
Technical Field
The invention relates to the technical field of battery preparation, in particular to a diatomite-based lithium ion battery cathode material and a preparation method thereof.
Background
Currently, the lithium ion battery cathode materials commercially produced in the market are mainly carbon-based cathode materials, including graphite and mesophase carbon microsphere cathode materials. The theoretical capacity of the cathode material is about 372 mAh/g, actually reaches 370mAh/g, and the capacity of the graphite cathode material is almost not improved. Meanwhile, the preparation process of the carbon cathode material is slightly complicated. Therefore, it is necessary to develop a lithium ion battery cathode material with large theoretical capacity, which can be commercialized and produced in large scale.
In recent years, the technology of the present invention has been developedSince then, a variety of new high-capacity and high-rate negative electrode materials have been developed and put into production in succession, wherein silicon oxide negative electrode materials have been the focus of research due to their high theoretical capacity and abundant reserves, wherein the theoretical capacity of SiO is as high as 2800 mAh/g, and SiO is SiO2The theoretical capacity of the material is as high as 1965 mAh/g, and the abundant reserves ensure that the material has wide sources and low price, so the silicon oxide material becomes an ideal lithium ion battery cathode material.
Some metal elements also have high theoretical specific capacity, for example, Sn can reach 994 mAh/g, Al can also reach 2978 mAh/g, and the metal property of the metal elements determines that the metal elements have very good conductivity. However, both silicon oxide materials and metal materials have their own disadvantages as negative electrode materials for lithium ion batteries, such as large volume deformation caused by intercalation and deintercalation of lithium ions during charge and discharge, low conductivity of silicon oxide materials, and these characteristics restrict their commercial application.
Patent CN 108075110 a discloses a preparation method of a lithium ion battery cathode material with a carbon-coated nano silicon composite cathode, the preparation steps of the composite are complicated, and the obtained target product has large particles, which is not suitable for large-scale commercial production.
Patent CN 110165177A discloses a preparation method of a silicon-based composite negative electrode material of a lithium ion battery, which is to perform ball milling on silicon and copper oxide to prepare the silicon-based composite negative electrode material, and the material prepared by the method can not ensure the purity, and has the defects of low yield, poor morphology controllability and the like.
Patent CN 108598442A discloses a preparation method of a silicon-based lithium ion battery cathode material, in the method, graphene oxide is coated with silicon nanoparticles to form the silicon-based lithium ion battery cathode material, aniline used in the method has toxicity, and the method is high in production cost, complicated in steps and not beneficial to large-scale commercial production.
Patent CN 102437318A discloses a silicon-carbon composite lithium ion battery cathode 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 as to obtain the silicon-carbon cathode material with a carbon-coated core-shell structure. However, the synthetic process of the phenolic resin has the defects of high toxicity, high cost and the like, and the carbon obtained by pyrolyzing the resin has high hardness and cannot be well adapted to the volume change of silicon. Therefore, the cycle stability of this composite material is relatively poor.
Patent CN 102983317A discloses a silicon-carbon composite lithium ion battery cathode material and a preparation method thereof, which comprises blending silicon particles and a precursor of carbon to obtain a mixed slurry of the silicon particles and the precursor of the carbon, and then carbonizing at high temperature to obtain a silicon-carbon composite. However, the composite obtained by the production process has the defects of nonuniform silicon distribution, easy agglomeration and the like. Meanwhile, the carbonization temperature is high, the process difficulty is high, and the production cost is high.
So far, a composite system taking metal filled porous diatomite as a whole is not seen to be used for the research of lithium ion battery negative electrode 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 nanoscale metal particles on the surface of the silicon oxide, and a negative electrode piece and a lithium ion battery are prepared on the basis of the porous silicon oxide negative electrode material. According to the invention, the silicon oxide and the metal which are independently researched before are put into a composite system for research for the first time, so that the advantages of the silicon oxide and the metal are fully exerted, and the defect that the silicon oxide and the metal independently form the negative electrode material is overcome.
The technical scheme of the invention is as follows: the negative electrode 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 methodxThe composite material is prepared from M, one of Sn and Al, and SiOxIn the formula, x is more than or equal to 0 and less than or equal to 2.
A preparation method of a diatomite-based lithium ion battery negative electrode material specifically comprises the following steps:
1) mixing a metal source M and porous silicon oxide SiOxMixing, and ultrasonic treating for 0.5-1 hDispersing the mixture, and drying the mixture in an oven at the temperature of between 50 and 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 mixturexFully contacting to obtain a mixture B;
3) heating the mixture B obtained in the step 2 to 400-1500 ℃ at the speed of 2-20 ℃/min under the condition of nitrogen, argon or argon-hydrogen mixed gas, preserving the heat for 3-10 h, and naturally cooling to obtain a metal-coated silicon oxide cathode material C;
in step 1, the metal source is one of simple substances, hydroxides, halides or nitrate compounds of Sn and Al;
in step 1, the SiOxThe porous silicon oxide material has the grain size of 100 nm-40 um;
in step 1, a metal source M and porous silica SiOxIs 1:1 to 10: 1.
In step 2, the grinding time is preferably 20 min;
in step 3, the argon-hydrogen mixture has a hydrogen content of 5% to 15% by volume, preferably 5% by volume.
The negative plate prepared from the negative electrode material further comprises a conductive agent and a binder, wherein the weight percentage range of the negative electrode material is 50-99.5 wt%, the weight percentage range of the conductive agent is 0.1-40 wt%, and the weight percentage range of the binder is 0.1-40 wt%.
The conductive agent is at least one of carbon black, acetylene black, natural graphite, carbon nano tubes, 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 carboxymethylcellulose.
The lithium ion battery prepared by the negative plate further comprises a positive electrode, a diaphragm and electrolyte.
The positive electrode is a commonly used lithium battery positive electrode 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 oxideSeed growing; the diaphragm comprises one of an aramid diaphragm, a non-woven fabric diaphragm, a polyethylene microporous film, a polypropylene-polyethylene double-layer or three-layer composite film and a ceramic coating diaphragm thereof; the electrolyte comprises an electrolyte and a solvent, wherein the electrolyte is LiPF6、LiBF4、LiClO4、LiAsF6、LiCF3SO3、LiN(CF3SO2) At least one of LiBOB, LiCl, LiBr and LiI; the solvent comprises at least one of Propylene Carbonate (PC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC), 1, 2-Dimethoxyethane (DME), ethylene carbonate, propylene carbonate, butylene carbonate, diethyl carbonate, methyl propyl carbonate, acetonitrile, ethyl acetate and ethylene sulfite.
The invention has the beneficial effects that:
1. according to the invention, Sn or Al is creatively filled or coated with diatomite (porous silicon oxide) to form a negative active material in a compounding manner, the porous diatomite is used as a framework, the problem of volume expansion of active substances such as Sn, Al and the like in the lithium charging and discharging process can be effectively inhibited, meanwhile, the addition of a metal substance can improve the conductivity of silicon oxide, and the lithium ion battery assembled by the negative plate prepared on the basis of the porous diatomite shows excellent lithium storage performance, cycle life and good rate performance;
2. the invention adopts a high-temperature solid-phase self-assembly synthesis method to complete the preparation of the cathode material, the reaction method is simple and controllable, large-scale production can be realized, and the synthesis process is favorable for controlling the cost and is commercially popularized and applied.
Drawings
FIG. 1 is a graph comparing electrochemical impedance of electrodes prepared in example 1 and comparative example 1;
FIG. 2 is a graph showing charge and discharge curves of the electrode prepared in example 1;
FIG. 3 is a schematic diagram of a negative electrode material formed of metal-coated porous silica;
FIG. 4 is a graph comparing rate performance of tin-filled silica with silica;
FIG. 5 is a graph comparing the cycling performance of tin-filled silica with silica.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
Example 1
6 mmol of diatomite (the diatomite component is porous silica) and 4 mmol of tin powder are put into ethanol for 30 minutes of ultrasonic treatment, and then dried in a 50 ℃ oven to obtain a mixture of the silica and the tin powder. And then grinding the mixture in a grinding body for 20 minutes to enable the mixture to be fully contacted, transferring the ground product into a tubular furnace, introducing argon-hydrogen mixed gas (argon gas 95 percent and hydrogen gas 5 percent) into the tubular furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, preserving heat for 3 hours, and naturally cooling to obtain the tin-coated silicon oxide cathode material.
The invention adopts a high-temperature solid-phase self-assembly synthesis method to prepare a metal-filled or coated porous silicon oxide composite material (M-SiO)x) The solid-phase synthesis method has the advantages of simplicity, large-scale production and the like, so that the diatomite-based silicon oxide negative electrode material prepared by the method is favorable for being effectively popularized in future commercial application.
Meanwhile, metal can be spontaneously self-assembled 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 lithium charging and discharging process can be effectively solved, and meanwhile, the conductivity of silicon oxide can be improved by adding a metal substance, so that the metal and the silicon oxide are mutually cooperated to improve the electrochemical energy storage characteristic of a composite system.
The prepared tin-coated silicon oxide active substance, conductive carbon black and a binder polyvinylidene fluoride are mixed according to the weight ratio of 8: 1:1, preparing a negative electrode slurry by using 1-methyl-2-pyrrolidone as a solvent, coating the negative electrode slurry on a copper foil to prepare a negative electrode sheet, and drying at 50 ℃ overnight. The electrochemical test is carried out by using a CR2025 type button cell, the counter electrode is an analytically pure metal lithium sheet, and the electrolyte is 1M LiPF6The volume ratio of Ethylene Carbonate (EC) to ethylmethyl carbonate (DEC) is 1:1, and the battery diaphragm is Celgard-2320 (microporous polypropylene film). The cell assembly was performed in a glove box filled with argon.
Comparative example 1
For comparison with the product from example 1, a comparative 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. After that, the silicon oxide negative electrode material was ground in a grinding body for 20 minutes, and the ground product was transferred to a tube furnace, and then argon-hydrogen mixed gas (argon 95%, hydrogen 5%) was introduced into the tube furnace, and the temperature was raised to 500 ℃ at a temperature rising rate of 10 ℃/min, and then the tube furnace was kept warm for 3 hours, and was naturally cooled to obtain a silicon oxide negative electrode material, and then, the cell assembly was performed under the same conditions as in example 1.
Example two: characterization of the Anode materials
The electrochemical impedance test of the electrodes prepared in example 1 and comparative example 1 is performed, and the result is shown in fig. 1, wherein the result shows that the resistance of the tin-coated silicon oxide is obviously improved, and compared with the resistance of the original silicon oxide of 400 Ω, the resistance of the composite material is reduced to about 200 Ω, and the resistance is greatly improved.
Fig. 2 is a charge-discharge cycle diagram of the electrode prepared in example one, and it can be seen from the figure that the first discharge of the electrode after the porous silica is coated with tin metal can reach about 380 mAh/g, while the first charge-discharge of the silica is only 150 mAh/g, which is improved compared with the performance of the electrode made of silica alone.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.
Claims (10)
1. The diatomite-based lithium ion battery negative electrode material is characterized in that the negative electrode material is a high-temperature solid-phase self-assembled materialThe assembly synthesis method is to form M-SiO after filling or coating the porous silicon oxide material with metalxThe composite material is prepared from M, one of Sn and Al, and SiOxIn the formula, x is more than or equal to 0 and less than or equal to 2.
2. The preparation method of the diatomite-based lithium ion battery negative electrode material according to claim 1, which is characterized by comprising the following steps:
1) mixing a metal source M and porous silicon oxide SiOxUltrasonic treatment for 0.5-1 h after mixing to disperse the mixture, and then drying in a drying oven at 50-80 ℃ 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 mixturexFully contacting to obtain a mixture B;
3) and (3) heating the mixture B obtained in the step (2) to 400-1500 ℃ at the speed of 2-20 ℃/min under the condition of nitrogen, argon or argon-hydrogen mixed gas, preserving the heat for 3-10 h, and naturally cooling to obtain the metal-coated silicon oxide cathode material C.
3. The method for preparing the negative electrode material of the diatomite-based lithium ion battery according to claim 2, wherein in the step 1, the metal source is one of simple substances, hydroxides, halides or nitrate compounds of Sn, Al.
4. The preparation method of the diatomite-based lithium ion battery negative electrode material as claimed in claim 2, wherein in the step 1, the porous silicon oxide SiO is preparedxThe particle size of (A) is 100 nm-40 um.
5. The preparation method of the negative electrode material of the lithium ion battery based on the diatomite base as claimed in claim 2, wherein in the step 1, the metal source M and the porous silicon oxide SiO are usedxIs 1:1 to 10: 1.
6. The preparation method of the negative electrode material of the lithium ion battery based on the diatomite base as claimed in claim 2, wherein in the step 3, the hydrogen volume content in the argon-hydrogen mixed gas is 5% -15%.
7. The negative electrode sheet prepared from the negative electrode material of the diatomite-based lithium ion battery according to any one of claims 1-6, further comprising a conductive agent and a binder, wherein the weight percentage of the negative electrode 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%.
8. The negative electrode sheet according to claim 7, 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 carboxymethylcellulose.
9. The lithium ion battery prepared from the negative electrode sheet according to claim 7, further comprising a positive electrode, a separator and an electrolyte.
10. The lithium ion battery of claim 9, wherein the positive electrode material comprises one of lithium cobaltate, lithium manganate, lithium nickelate, lithium iron phosphate, lithium titanate, nickel-cobalt-manganese ternary system, or lithium composite metal oxide; the diaphragm comprises one of an aramid diaphragm, a non-woven fabric diaphragm, a polyethylene microporous film, a polypropylene-polyethylene double-layer or three-layer composite film and a ceramic coating diaphragm thereof; the electrolyte comprises an electrolyte and a solvent, wherein the electrolyte is LiPF6、LiBF4、LiClO4、LiAsF6、LiCF3SO3、LiN(CF3SO2) At least one of LiBOB, LiCl, LiBr and LiI; the solvent comprises propylene carbonate, dimethyl carbonate, ethyl methyl carbonate, 1, 2-dimethoxyethane, ethylene carbonate, propylene carbonate, butylene carbonate, and carbonAt least one of diethyl carbonate, methyl propyl carbonate, acetonitrile, ethyl acetate and ethylene sulfite.
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| CN112133898A (en) * | 2020-09-21 | 2020-12-25 | 陕西煤业化工技术研究院有限责任公司 | Silicon-based negative electrode material and preparation method thereof |
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| CN112133898A (en) * | 2020-09-21 | 2020-12-25 | 陕西煤业化工技术研究院有限责任公司 | Silicon-based negative electrode material and preparation method thereof |
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