CN113594438A - Preparation of honeycomb structure micro/nano-sized silicon/carbon composite material used as lithium ion battery cathode material, product and application - Google Patents
Preparation of honeycomb structure micro/nano-sized silicon/carbon composite material used as lithium ion battery cathode material, product and application Download PDFInfo
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- CN113594438A CN113594438A CN202110852311.0A CN202110852311A CN113594438A CN 113594438 A CN113594438 A CN 113594438A CN 202110852311 A CN202110852311 A CN 202110852311A CN 113594438 A CN113594438 A CN 113594438A
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- 239000002131 composite material Substances 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- 239000010406 cathode material Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 title claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 102000002322 Egg Proteins Human genes 0.000 claims description 3
- 108010000912 Egg Proteins Proteins 0.000 claims description 3
- 210000003278 egg shell Anatomy 0.000 claims description 3
- 239000007773 negative electrode material Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims 1
- 239000007772 electrode material Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- 239000002153 silicon-carbon composite material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910021426 porous silicon Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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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
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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 provides a preparation method of a micron/nanometer silicon/carbon composite material with a honeycomb structure used as a lithium ion battery cathode material, and a product and application thereof, wherein commercial micron-sized silicon powder and polyacrylonitrile are used as raw materials, and a Si/PC50 porous composite material is obtained through simple processes of mixing, stirring and the like, and can effectively improve the cycle performance and rate capability of an electrode material. The preparation process is simple and easy to operate.
Description
Technical Field
The invention designs a preparation method of a lithium ion battery cathode material, and particularly relates to a preparation method of a micro/nano silicon/carbon composite material with a honeycomb structure and used as the lithium ion battery cathode material, and a product and application thereof.
Background
A lithium ion battery is an electrochemically rechargeable energy storage system in which lithium ions move between a cathode and an anode through an electrolyte during charge/discharge. Due to the advantages of high energy density, no memory effect, long cycle life and the like, the lithium battery is rapidly developed and widely applied to small electronic equipment such as smart phones, notebook computers, digital cameras, portable tools and the like, and large application fields including public transportation, aerospace engineering, national defense and medical systems. With the development of human society, more advanced lithium ion batteries with high energy density and high power density are required to meet the increasing demand for new and clean energy in the world, which has stimulated intensive research into novel electrode materials with low cost, high capacity, and high capacity. Good environmental benign. In the aspect of a negative electrode, researches mainly focus on carbon-containing materials such as graphite-based carbon, hard carbon and carbon nano tubes and graphene, and non-carbon materials such as transition metal oxides/sulfides, alloys and the like, at present, most reports use the center of gravity for researching nano silicon-carbon composite materials with good cycle performance, but the nano materials have low stacking density, and the huge specific surface area causes more irreversible side reactions, so that the low first efficiency is caused, and the practical application of the nano silicon-carbon composite materials is limited.
To date, a large number of nano/porous silicon-based Si/C composites have been prepared by Chemical Vapor Deposition (CVD), spray drying/pyrolysis, and high energy ball milling. However, the manufacturing processes for nano-silicon and porous silicon are generally complex and expensive.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a micro/nano silicon/carbon composite material with a honeycomb structure, which is used as a lithium ion battery cathode material.
Yet another object of the present invention is to: the micro/nano-sized silicon/carbon composite material product with the honeycomb structure, which is used as the lithium ion battery cathode material, is prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a micro/nano-sized silicon/carbon composite material with a honeycomb structure used as a lithium ion battery cathode material is characterized in that the material has a mixed eggshell and oatmeal-shaped porous structure, and the material shows strong cycling stability when being used as a lithium ion battery cathode, and comprises the following steps:
(1) 2.12g of Na2CO3 (0.02mol) and 2.22g of CaCl2 (0.02mol) were dissolved in 100 mL of distilled water, respectively;
(2) 0.1 g of silicon powder was dispersed in Na2CO3Stirring vigorously for 1 h, performing ultrasonic treatment for 3 h, and then dropwise adding the dispersed solution into CaCl under stirring2Obtaining a mixture in the solution;
(3) the mixture was further stirred for 10 min and filtered to obtain Si @ CaCO3The product, which is washed with water, ethanol and Dimethylformamide (DMF);
(4) the washed Si @ CaCO3Dispersing in 1-2 mL DMF, dissolving 0.30-0.50 g Polyacrylonitrile (PAN) in the solution, stirring for 1 h to obtain a uniform mixture, and vacuum drying at 60 deg.C to obtain Si @ CaCO3A PAN precursor;
(5) pre-oxidizing the precursor in air environment at 280 deg.c for 4 hr, washing with dilute hydrochloric acid and water to eliminate CaCO3And carbonizing the purified precursor at 650 ℃ in a nitrogen atmosphere for 6 h to obtain Si/PC 30-50.
Polyacrylonitrile as carbon and nitrogen source.
CaCO3As a structural template, it was finally removed with dilute hydrochloric acid.
The starting material is 5-10 μm low-cost micrometer silicon powder.
About 5-10 μm micron sized silicon powder was sanded for 4 hours.
The invention provides a micro/nano-sized silicon/carbon composite material with a honeycomb structure for serving as a lithium ion battery cathode material, which is prepared by any one of the methods.
The invention provides an application of a micro/nano-sized silicon/carbon composite material with a honeycomb structure as a lithium ion battery cathode material.
According to the invention, micron-sized silicon powder is used as a silicon source, a preparation method of the silicon-carbon composite material capable of meeting the industrial requirement is developed, and the silicon-carbon porous composite material with excellent electrochemical performance is obtained. The Si/PC50 porous composite material is obtained by taking commercial micron-sized silicon powder and polyacrylonitrile as raw materials through simple processes of mixing, stirring and the like, and the composite material can effectively improve the cycle performance and rate capability of an electrode material. The preparation process is simple and easy to operate.
Drawings
FIG. 1 is a cycle performance test chart of a negative pole piece made of a Si/C50 composite material.
Detailed Description
Example 1
A silicon/carbon composite material with a cellular structure and micro/nano-size used as a lithium ion battery cathode material is a Si/C composite material, and is characterized in that the material has a mixed eggshell and oatmeal-shaped porous structure, and the material shows strong cycling stability when being used as a lithium ion battery cathode, and is prepared by the following steps:
(1) 2.12g of Na2CO3 (0.02mol) and 2.22g of CaCl2 (0.02mol) were dissolved in 100 mL of distilled water, respectively;
(2) 0.1 g of silicon powder was dispersed in Na2CO3Stirring vigorously for 1 h, performing ultrasonic treatment for 3 h, and then dropwise adding the dispersed solution into CaCl under stirring2Obtaining a mixture in the solution;
(3) the mixture was further stirred for 10 min and filtered to obtain Si @ CaCO3The product, after washing several times with water, is washed with ethanol and dimethylformamideWashing with amine (DMF);
(4) the washed Si @ CaCO3Dispersing in 1-2 mL DMF, dissolving 0.30 g Polyacrylonitrile (PAN) in the solution, stirring for 1 h to obtain a uniform mixture, and vacuum drying at 60 deg.C to obtain Si @ CaCO3A PAN precursor;
(5) pre-oxidizing the precursor in air environment at 280 deg.c for 4 hr, washing with dilute hydrochloric acid and water to eliminate CaCO3And carbonizing the purified precursor at 650 ℃ in a nitrogen atmosphere for 6 h to obtain Si/PC 30.
The beneficial effects of the material obtained by the embodiment are as follows: Si/PC30 showed a first coulombic efficiency of 78% and 1245 mAh g-1The charge specific capacity and the capacity retention rate after 200 cycles are 82%, and the good industrial application prospect is shown.
Example 2:
a silicon/carbon composite material with a honeycomb structure used as a negative electrode material of a lithium ion battery, which is prepared by the following steps similar to the steps of the example 1:
(1) 2.12g of Na2CO3 (0.02mol) and 2.22g of CaCl2 (0.02mol) were dissolved in 100 mL of distilled water, respectively;
(2) 0.1 g of silicon powder was dispersed in Na2CO3Stirring vigorously for 1 h, performing ultrasonic treatment for 3 h, and then dropwise adding the dispersed solution into CaCl under stirring2Obtaining a mixture in the solution;
(3) the mixture was further stirred for 10 min and filtered to obtain Si @ CaCO3The product, which is washed several times with water, then with ethanol and Dimethylformamide (DMF);
(4) the washed Si @ CaCO3Dispersing in 1-2 mL DMF, dissolving 0.50 g Polyacrylonitrile (PAN) in the solution, stirring for 1 h to obtain a uniform mixture, and vacuum drying at 60 deg.C to obtain Si @ CaCO3A PAN precursor;
(5) pre-oxidizing the precursor in air environment at 280 deg.c for 4 hr, washing with dilute hydrochloric acid and water to eliminate CaCO3Carbonizing the purified precursor at 650 ℃ in a nitrogen atmosphere for 6 h to obtain the product Si/PC50。
The beneficial effects of the material obtained by the embodiment are as follows: Si/PC24 showed a first coulombic efficiency of 82% and 1295 mAh g-1The capacity, 200 cycles capacity retention rate is 85%.
The cycle performance test chart of the negative pole piece made of the Si/C50 composite material is shown in figure 1.
The embodiments described above are described to facilitate an understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications to the present invention based on the disclosure of the present invention within the protection scope of the present invention.
Claims (7)
1. A preparation method of a micro/nano-sized silicon/carbon composite material with a honeycomb structure used as a lithium ion battery cathode material is characterized in that the material has a mixed eggshell and oatmeal-shaped porous structure and comprises the following steps:
(1) 2.12g of Na2CO3 (0.02mol) and 2.22g of CaCl2 (0.02mol) were dissolved in 100 mL of distilled water, respectively;
(2) 0.1 g of silicon powder was dispersed in Na2CO3Stirring vigorously for 1 h, performing ultrasonic treatment for 3 h, and then dropwise adding the dispersed solution into CaCl under stirring2Obtaining a mixture in the solution;
(3) the mixture was further stirred for 10 min and filtered to obtain Si @ CaCO3The product, which is washed with water, ethanol and Dimethylformamide (DMF);
(4) the washed Si @ CaCO3Dispersing in 1-2 mL DMF, dissolving 0.30-0.50 g Polyacrylonitrile (PAN) in the solution, stirring for 1 h to obtain a uniform mixture, and vacuum drying at 60 deg.C to obtain Si @ CaCO3A PAN precursor;
(5) pre-oxidizing the precursor in air environment at 280 deg.c for 4 hr, washing with dilute hydrochloric acid and water to eliminate CaCO3And carbonizing the purified precursor at 650 ℃ in a nitrogen atmosphere for 6 h to obtain Si/PC 30-50.
2. The method according to claim 1, wherein acrylonitrile is used as a carbon source and a nitrogen source.
3. The method of claim 1, wherein the process comprises the steps of3As a structural template and is finally removed with dilute hydrochloric acid.
4. The preparation method according to claim 1, characterized in that the starting material is 5-10 μm low-cost micron-sized silicon powder.
5. The method according to claim 1 or 4, characterized in that the silicon powder of 5-10 μm micron size is sanded for 4 hours.
6. A silicon/carbon composite material with a honeycomb structure for use as a negative electrode material of a lithium ion battery, characterized in that it is prepared by the method according to any one of claims 1 to 5.
7. Use of the micro/nano-sized silicon/carbon composite having a honeycomb structure according to claim 6 as a negative electrode material for lithium ion batteries.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337613A (en) * | 2013-07-04 | 2013-10-02 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material and preparation method thereof, and lithium ion battery |
| CN111816852A (en) * | 2020-06-29 | 2020-10-23 | 瑞声科技（南京）有限公司 | Preparation method of silicon-based composite negative electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103337613A (en) * | 2013-07-04 | 2013-10-02 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material and preparation method thereof, and lithium ion battery |
| CN111816852A (en) * | 2020-06-29 | 2020-10-23 | 瑞声科技（南京）有限公司 | Preparation method of silicon-based composite negative electrode material |
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Application publication date: 20211102 |