CN114709393A - Preparation method of negative electrode material for sodium ion battery - Google Patents
Preparation method of negative electrode material for sodium ion battery Download PDFInfo
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- CN114709393A CN114709393A CN202210374215.4A CN202210374215A CN114709393A CN 114709393 A CN114709393 A CN 114709393A CN 202210374215 A CN202210374215 A CN 202210374215A CN 114709393 A CN114709393 A CN 114709393A
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- ion battery
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- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 34
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims description 35
- 239000011847 coal-based material Substances 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 25
- 239000003245 coal Substances 0.000 claims description 22
- 239000010426 asphalt Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052736 halogen Inorganic materials 0.000 claims description 11
- 150000002367 halogens Chemical class 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 150000008282 halocarbons Chemical class 0.000 claims description 10
- 238000010000 carbonizing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 9
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 7
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003830 anthracite Substances 0.000 claims description 6
- 239000002802 bituminous coal Substances 0.000 claims description 6
- 239000003077 lignite Substances 0.000 claims description 6
- 239000003476 subbituminous coal Substances 0.000 claims description 6
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 4
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 4
- 102220043159 rs587780996 Human genes 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 229910003481 amorphous carbon Inorganic materials 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 description 5
- 150000005826 halohydrocarbons Chemical class 0.000 description 5
- 239000002243 precursor Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
-
- 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
Abstract
The invention discloses a preparation method of a negative electrode material for a sodium ion battery. According to the method, a purification process is inserted under the condition that common preparation steps are not reduced, so that the purification cost can be greatly reduced, in addition, a plurality of holes are caused in the obtained material due to the volatilization of impurities in the carbonization process, the holes provide great convenience for the diffusion and migration of sodium ions, so that the large-current charge-discharge performance is favorably improved, meanwhile, the surface is coated with amorphous carbon, the specific surface area can be reduced, the interface is improved, the inner part is porous, the surface is compact, and the capacity, the first-time efficiency and the power performance of the graphite cathode can be greatly improved; moreover, the preparation method has the advantages of simple process, convenient operation and less production equipment, thereby further reducing the cost, being convenient for popularization and application and being suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a preparation method of a negative electrode material for a sodium ion battery.
Background
With the advance of human industrialization, the consumption of traditional fossil energy is gradually increased, the problems of environmental pollution and energy shortage are increasingly highlighted, and the development of clean energy such as wind energy, solar energy, tidal energy and the like becomes one of effective ways for solving the problems. However, the clean energy has the characteristics of randomness and intermittency, and cannot be directly connected to a power grid, so that the development of a large-scale energy storage system with low cost and high performance becomes the key for efficiently utilizing the clean energy.
The sodium ion battery becomes one of candidates of large-scale energy storage devices by virtue of the advantages of abundant sodium resource reserves and low price. The electrode material directly influences the performance of the battery as a core component of the sodium ion battery, and the main challenge of commercialization of the sodium ion battery is to find a positive and negative electrode material with high performance and low cost. Meanwhile, the carbon material is one of the cathode materials with great potential by virtue of the advantages of low price, good chemical stability, controllable structure and the like. The coal-based material represented by sub-bituminous coal, bituminous coal and anthracite has the characteristics of abundant resources, low price, easy obtainment and high carbon yield, and the sodium-ion battery cathode material prepared by adopting the coal-based precursor is the most cost-effective sodium-ion battery carbon-based cathode material at present. However, the existing materials such as coal-based carbon are doped with impurities such as metal oxides and other non-carbon materials in the process of forming the precursor of the materials. The presence of these impurities directly affects the cell performance, and the presence of impurities such as silica, alumina, magnesia, etc. reduces the conductivity of the material, most of which do not promote the storage of sodium ions, which in turn reduces the energy density of the cell. Therefore, the purification of the coal-based precursor is urgently needed, and the sodium storage capacity and the cycle performance of the coal-based precursor are improved so as to meet the performance requirements of the sodium ion battery with high energy density, long cycle life and low cost.
Disclosure of Invention
In view of the above, the present invention is directed to a method for preparing a negative electrode material for a sodium ion battery, wherein the prepared negative electrode material has excellent sodium storage capacity and cycle performance, and can meet the performance requirements of a sodium ion battery with high energy density, long cycle life and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a negative electrode material for a sodium-ion battery comprises the following steps:
(1) mixing materials:
mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material;
(2) carbonizing:
and (2) putting the mixture material obtained in the step (1) into a protective furnace filled with halogen or halogenated hydrocarbon atmosphere for carbonization, raising the temperature to 1100-1600 ℃ at the heating rate of 2-25 ℃/min, preserving the temperature for 4-11h, crushing and screening to obtain the cathode material for the sodium-ion battery.
Preferably, the coal-based material in step (1) is pulverized coal with particle edges and corners, and the pulverized coal is obtained by crushing one or more of sub-bituminous coal, lignite, bituminous coal and anthracite, and D50 is 7-16 μm.
Preferably, the binder in the step (1) is one or a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
As a preferable scheme, the mass ratio of the coal-based material to the binder in the step (1) is 1 (0.03-0.1).
As a preferable mode, the halogen or halogenated hydrocarbon in the step (2) is F2、Cl2、Br2、CCl4、CH3Cl、CH2Cl2、CHCl3、C2H5Br、C3H7I and C4H7Cl3At least one of (1).
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that: according to the method, a purification process is inserted under the condition that common preparation steps are not reduced, so that the purification cost can be greatly reduced, in addition, a plurality of holes are caused in the obtained material due to the volatilization of impurities in the carbonization process, the holes provide great convenience for the diffusion and migration of sodium ions, so that the large-current charge-discharge performance is favorably improved, meanwhile, the surface is coated with amorphous carbon, the specific surface area can be reduced, the interface is improved, the inner part is porous, the surface is compact, and the capacity, the first-time efficiency and the power performance of the graphite cathode can be greatly improved; moreover, the preparation method has the advantages of simple process, convenient operation and less production equipment, thereby further reducing the cost, being convenient for popularization and application and being suitable for large-scale production.
To more clearly illustrate the features and efficacy of the present invention, the present invention will be described in detail with reference to the following specific examples.
Detailed Description
The invention discloses a preparation method of a negative electrode material for a sodium ion battery, which comprises the following steps:
(1) mixing materials:
mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1 (0.03-0.1), the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing one or more of subbituminous coal, lignite, bituminous coal and anthracite, D50 is 7-16 mu m, the binder is one or mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
placing the mixture material obtained in the step (1) in a protective furnace filled with halogen or halohydrocarbon atmosphere for carbonization, raising the temperature to 1100-1600 ℃ at the temperature rise rate of 2-25 ℃/min, preserving the heat for 4-11h, crushing and screening to obtain the cathode material for the sodium-ion battery; the halogen or halogenated hydrocarbon is F2、Cl2、Br2、CCl4、CH3Cl、CH2Cl2、CHCl3、C2H5Br、C3H7I and C4H7Cl3At least one of (1).
The present invention will be described in detail with reference to the following examples.
Example 1
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.03, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing sub-bituminous coal, D50 is 7-16 mu m, the binder is coal-series asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halogen atmosphere for carbonization, heating to 1100 ℃ at a heating rate of 2 ℃/min, preserving heat for 11 hours, crushing and screening to obtain a negative electrode material for a sodium-ion battery; the halogen is F2。
Example 2
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.1, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing lignite, D50 is 7-16 mu m, the binder is oil-based asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halohydrocarbon atmosphere for carbonization, heating to 1600 ℃ at a heating rate of 25 ℃/min, preserving heat for 4 hours, crushing and screening to obtain a negative electrode material for the sodium-ion battery; the halogenated hydrocarbon is CCl4、CH3Cl、CH2Cl2And CHCl3A mixture of (a).
Example 3
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.06, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing bituminous coal, D50 is 7-16 mu m, the binder is a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halogen atmosphere for carbonization, heating to 1300 ℃ at a heating rate of 20 ℃/min, preserving heat for 8 hours, crushing and screening to obtain a negative electrode material for a sodium-ion battery; the halogen is Cl2And Br2A mixture of (a).
Example 4
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.08, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing anthracite, D50 is 7-16 mu m, the binder is oil-based asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halohydrocarbon atmosphere for carbonization, raising the temperature to 1400 ℃ at a heating rate of 15 ℃/min, preserving the temperature for 5 hours, crushing and screening to obtain a negative electrode material for the sodium-ion battery; the halogenated hydrocarbon is C4H7Cl3。
Example 5
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.04, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing sub-bituminous coal and lignite, D50 is 7-16 mu m, and the binder is coal-based asphalt or has a softening point of 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halohydrocarbon atmosphere for carbonization, raising the temperature to 1200 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 7 hours, crushing and screening to obtain a negative electrode material for the sodium-ion battery; the halogenated hydrocarbon is C2H5Br。
Example 6
Mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material; the mass ratio of the coal-based material to the binder is 1:0.09, the coal-based material is pulverized coal with particle edges and corners, the pulverized coal is formed by crushing lignite, bituminous coal and anthracite, D50 is 7-16 mu m, the binder is a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
(2) Carbonizing:
putting the mixture material obtained in the step (1) into a protective furnace filled with halohydrocarbon atmosphere for carbonization, heating to 1400 ℃ at a heating rate of 16 ℃/min, preserving heat for 10 hours, and crushing and screening to obtain a negative electrode material for a sodium-ion battery; the halogenated hydrocarbon is C3H 7I.
Comparative example 1: the halogen or halogenated hydrocarbon atmosphere in the step (2) is replaced by a nitrogen atmosphere, and other conditions are the same as those in example 1.
The following performance tests were conducted on each of the examples and comparative examples, and the test results are shown in Table 1.
TABLE 1 comparison of performances of anode materials in various examples and comparative examples
As can be seen from Table 1, the prepared sodium ion battery negative electrode material has excellent capacity performance, cycle performance, first charge-discharge efficiency and rate performance. The special internal porous surface compact structure constructed by the low-cost purification and carbonization integrated process plays a very critical role, reduces the diffusion and migration resistance of sodium ions, and improves the performances in all aspects.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (5)
1. A preparation method of a negative electrode material for a sodium ion battery is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing materials:
mixing a coal-based material and a binder according to a certain mass ratio to obtain a mixture material;
(2) carbonizing:
and (2) putting the mixture material obtained in the step (1) into a protective furnace filled with halogen or halogenated hydrocarbon atmosphere for carbonization, raising the temperature to 1100-1600 ℃ at the heating rate of 2-25 ℃/min, preserving the temperature for 4-11h, and crushing and screening to obtain the negative electrode material for the sodium-ion battery.
2. The method for preparing the negative electrode material for a sodium-ion battery according to claim 1, characterized in that: the coal-based material in the step (1) is pulverized coal with particle edges and corners, and is formed by crushing one or more of sub-bituminous coal, lignite, bituminous coal and anthracite, and D50=7-16 μm.
3. The method for preparing the negative electrode material for a sodium-ion battery according to claim 1, characterized in that: the binder in the step (1) is one or a mixture of coal-series asphalt and oil-series asphalt, and the softening point of the binder is 50-200 ℃.
4. The method for preparing the negative electrode material for a sodium-ion battery according to claim 1, characterized in that: the mass ratio of the coal-based material to the binder in the step (1) is 1 (0.03-0.1).
5. The method for preparing the negative electrode material for the sodium-ion battery according to claim 1, characterized in that: the halogen or halogenated hydrocarbon in the step (2) is F2、Cl2、Br2、CCl4、CH3Cl、CH2Cl2 、CHCl3、C2H5Br、C3H7I and C4H7Cl3At least one of (1).
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| CN108054357A (en) * | 2017-12-06 | 2018-05-18 | 宁夏博尔特科技有限公司 | Power lithium-ion battery coal base composite negative pole material and preparation method thereof |
| CN108807876A (en) * | 2018-04-28 | 2018-11-13 | 福建翔丰华新能源材料有限公司 | Preparation method of modified carbon negative electrode material for lithium ion battery |
| CN111293309A (en) * | 2020-03-04 | 2020-06-16 | 溧阳中科海钠科技有限责任公司 | Performance improvement method and application of coal-based sodium ion battery negative electrode material |
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