CN114927677B - Flexible sodium battery anode material and green preparation method and application thereof - Google Patents
Flexible sodium battery anode material and green preparation method and application thereof Download PDFInfo
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- CN114927677B CN114927677B CN202210608710.7A CN202210608710A CN114927677B CN 114927677 B CN114927677 B CN 114927677B CN 202210608710 A CN202210608710 A CN 202210608710A CN 114927677 B CN114927677 B CN 114927677B
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- 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 title claims abstract description 24
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 24
- 239000011734 sodium Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000010405 anode material Substances 0.000 title claims abstract description 17
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000009713 electroplating Methods 0.000 claims abstract description 22
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001509 sodium citrate Substances 0.000 claims abstract description 14
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 14
- 239000011975 tartaric acid Substances 0.000 claims abstract description 14
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 14
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 14
- 238000007600 charging Methods 0.000 claims abstract description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011701 zinc Substances 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- 238000004070 electrodeposition Methods 0.000 claims abstract description 8
- 239000007773 negative electrode material Substances 0.000 claims abstract description 8
- 150000003751 zinc Chemical class 0.000 claims abstract description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 12
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical group [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000010406 cathode material Substances 0.000 claims description 9
- 239000011592 zinc chloride Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 239000011889 copper foil Substances 0.000 claims description 5
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical group Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 238000010277 constant-current charging Methods 0.000 claims description 2
- 239000011888 foil Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 19
- 239000011148 porous material Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 0.000 description 1
- 239000003440 toxic substance Substances 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- 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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
- H01M4/662—Alloys
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention discloses a flexible sodium battery anode material and a preparation method and application thereof, and the preparation method comprises the following steps: placing the flexible current collector in electroplating solution, depositing tin and zinc on the flexible current collector in an electrodeposition mode, and then charging to dissolve the deposited zinc to obtain a flexible porous tin negative electrode material; the electroplating solution comprises zinc salt, tin salt, trisodium citrate and tartaric acid. The invention adopts the integrated technology of electrodeposition alloying-dealloying to prepare the porous tin anode material, the preparation process is simple and feasible, green and environment-friendly, and the invention is expected to realize mass production.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a flexible sodium battery negative electrode material, a green preparation method and application thereof, and the prepared negative electrode material is particularly suitable for sodium batteries.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Among the alloy cathode materials of sodium batteries, the metallic tin cathode has high theoretical specific capacity (847 mAh g -1) and lower reaction potential, so that the alloy cathode material has great application potential. However, in the circulation process, larger volume expansion (420%) can be generated, the structure of the electrode can be damaged, and then the electrode material is pulverized and crushed so as to fall off the current collector; in addition, a large volume change may form an unstable SEI film, thereby consuming electrolyte and sodium ions, resulting in rapid decay of capacity.
The problem can be effectively solved by making the tin material porous, the porous structure has large specific surface area, and the shell increases the contact area of the electrolyte; the pore canal structure can provide a channel for rapid diffusion of sodium ions; in addition, the volume change in the circulation process can be buffered, and the circulation stability of the material is improved. The special porous structure can improve the electrochemical performance of the tin anode to a certain extent.
The existing preparation method of porous tin has the problems of complex process, harsh conditions, requirement for toxic substances and the like.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a flexible sodium battery anode material and a green preparation method and application thereof.
In order to achieve the above object, the present invention is realized by the following technical scheme:
In a first aspect, the invention provides a preparation method of a flexible sodium battery anode material, comprising the following steps:
Placing the flexible current collector in electroplating solution, depositing tin and zinc on the flexible current collector in an electrodeposition mode, and then charging to dissolve the deposited zinc to obtain a flexible porous tin negative electrode material;
The electroplating solution comprises zinc salt, tin salt, trisodium citrate and tartaric acid.
In a second aspect, the invention provides a flexible sodium battery anode material prepared by the preparation method.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
The invention adopts the integrated technology of electrodeposition alloying-dealloying to prepare the porous tin anode material, the preparation process is simple and feasible, green and environment-friendly, and the invention is expected to realize mass production.
The zinc obtained by dealloying can be recycled, so that the utilization rate of materials can be improved, and the production cost is further reduced.
The proportion of different metals in the zinc-tin alloy can be regulated by regulating parameters in the alloying process, so that the pore size and distribution of the porous tin of the product can be regulated.
The porosity of the porous tin can be adjusted by adjusting parameters in the dealloying process.
The flexible porous tin material prepared by the invention has good mechanical properties, can effectively buffer volume change in the circulation process, keeps the stability of the structure and obtains good circulation performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
Figure 1 is an XRD pattern of porous tin of the product of example 1.
Fig. 2 is a cyclic voltammogram of the product porous tin of example 1 as the negative electrode material for a sodium ion battery.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In a first aspect, the invention provides a preparation method of a flexible sodium battery anode material, comprising the following steps:
Placing the flexible current collector in electroplating solution, depositing tin and zinc on the flexible current collector in an electrodeposition mode, and then charging to dissolve the deposited zinc to obtain a flexible porous tin negative electrode material;
The electroplating solution comprises zinc salt, tin salt, trisodium citrate and tartaric acid.
Trisodium citrate is used as a conductive salt to improve the conductivity of the electrolyte, and tartaric acid is used for stabilizing the pH value of the electroplating solution.
In some embodiments, the flexible current collector is selected from copper foil, aluminum foil, carbon-based material, or Mxenes.
In some embodiments, the zinc salt is zinc chloride or zinc sulfate.
Preferably, the concentration of zinc salt is 0.01 to 0.5mol L -1.
In some embodiments, the tin salt is tin chloride.
Preferably, the concentration of tin chloride is 0.01 to 0.5mol L -1.
Preferably, the concentration of trisodium citrate is 0.2 to 1.0mol L -1.
Preferably, the concentration of tartaric acid is 0.05 to 0.5mol L -1.
Too large concentrations of zinc and tin salts can cause too large and uneven electrodeposited particles, too small concentrations, and too small amounts of electrodeposited active material. Too low a concentration of trisodium citrate can result in too low a conductivity of the electrolyte and too high a concentration can exceed its solubility. Too high a concentration of tartaric acid results in a meta-acidity of the electrolyte, and too low a concentration can cause the solution to be meta-alkaline.
In some embodiments, the solvent of the plating solution is a mixed solution of water and ethylene glycol.
Preferably, the volume ratio of water to glycol is 3:1-1:3.
In some embodiments, the electrodeposition is a constant current discharge with a current density of 10 to 50mA cm -2 for a period of 30s to 2 hours.
Preferably, the charging is constant-current charging, the current density is 1-20 mA cm -2, and the time is 300s-6h.
In a second aspect, the invention provides a flexible porous tin anode material, which is prepared by the preparation method.
The invention is further illustrated below with reference to examples.
Example 1
A flexible sodium battery cathode material and a preparation method thereof are provided:
electroplating solution: 0.2M SnCl 4+0.2M ZnCl2 +0.12M trisodium citrate+0.15M tartaric acid.
Placing copper foil in the electroplating solution, wherein the constant-current discharge current is 10mA cm -2, and the time is 3min; and then charging for 32min under the current density of 1mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 500-600nm.
FIG. 1 is an XRD pattern of porous tin of the product of example 1, and characteristic peaks of tin are observed, and other impurity peaks are not present, thus indicating that a high-purity porous tin material is synthesized.
Fig. 2 is a cyclic voltammogram of the product porous tin of example 1 as the negative electrode material for a sodium ion battery. The characteristic peaks of the tin material when sodium is stored are shown, and in addition, the overlapped curves further illustrate that the synthesized porous tin material has good cycle performance.
Example 2
A flexible sodium battery cathode material and a preparation method thereof are provided:
electroplating solution: 0.15M SnCl 4+0.15M ZnCl2 +0.12M trisodium citrate+0.11M tartaric acid
Placing copper foil in the electroplating solution, wherein the constant-current discharge current is 15mA cm -2, and the time is 2min; and then charging for 17min under the current density of 2mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 800-900nm.
Example 3
A flexible sodium battery cathode material and a preparation method thereof are provided:
Electroplating solution: 0.08M SnCl 4+0.08M ZnCl2 +0.12M trisodium citrate+0.15M tartaric acid
Placing copper foil in the electroplating solution, wherein the constant-current discharge current is 18mA cm -2, and the time is 2min; and then charging for 40min under the current density of 1mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 900-950nm.
Example 4
A flexible sodium battery cathode material and a preparation method thereof are provided:
Electroplating solution: 0.2M SnCl 4+0.2M ZnCl2 +0.12M trisodium citrate+0.15M tartaric acid
Placing a Ti 3C2 film in the electroplating solution, wherein the constant-current discharge current is 10mA cm -2, and the time is 3min; and then charging for 32min under the current density of 1mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 600-650nm.
Example 5
A flexible sodium battery cathode material and a preparation method thereof are provided:
electroplating solution: 0.15M SnCl 4+0.15M ZnCl2 +0.12M trisodium citrate+0.11M tartaric acid
Disposing carbon in the electroplating solution, wherein the constant current discharge current is 15mA cm -2, and the time is 2min; and then charging for 17min under the current density of 2mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 750-900nm.
Example 6
A flexible sodium battery cathode material and a preparation method thereof are provided:
Electroplating solution: 0.08M SnCl 4+0.08M ZnCl2 +0.12M trisodium citrate+0.15M tartaric acid
Placing a carbon net in the electroplating solution, wherein the constant-current discharge current is 18mA cm ~2, and the time is 2min; and then charging for 40min under the current density of 1mA cm -2, washing and drying to obtain the flexible porous tin material, wherein the pore size distribution of the porous tin material is 900-950nm.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a flexible sodium battery anode material is characterized by comprising the following steps: the method comprises the following steps:
Placing the flexible current collector in electroplating solution, depositing tin and zinc on the flexible current collector in an electrodeposition mode, and then charging to dissolve the deposited zinc to obtain a flexible porous tin negative electrode material;
The electroplating solution comprises zinc salt, tin salt, trisodium citrate and tartaric acid;
The electrodeposition is constant-current discharge, the current density is 10-50 mA cm -2, and the time is 30 s-2 h;
The charging is constant-current charging, the current density is 1-20 mA cm -2, and the time is 300s-6h.
2. The method for preparing the flexible sodium battery anode material according to claim 1, wherein: the flexible current collector is selected from copper foil, aluminum foil, carbon-based material or Mxenes.
3. The method for preparing the flexible sodium battery anode material according to claim 1, wherein: the zinc salt is zinc chloride or zinc sulfate; the concentration of the zinc salt is 0.01-0.5 mol L -1.
4. The method for preparing the flexible sodium battery anode material according to claim 1, wherein: the tin salt is tin chloride; the concentration of the stannic chloride is 0.01-0.5 mol L -1.
5. The method for preparing the flexible sodium battery anode material according to claim 1, wherein: the concentration of the trisodium citrate is 0.2-1.0 mol L -1; the concentration of tartaric acid is 0.05-0.5 mol L -1.
6. The method for preparing the flexible sodium battery anode material according to claim 1, wherein: the solvent of the electroplating solution is a mixed solution of water and glycol.
7. The method for producing a battery anode material according to claim 6, characterized in that: the volume ratio of water to glycol is 3:1-1:3.
8. A flexible sodium battery cathode material is characterized in that: the preparation method according to any one of claims 1 to 7.
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CN114927677B true CN114927677B (en) | 2024-05-24 |
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Citations (3)
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---|---|---|---|---|
CN101001982A (en) * | 2004-08-10 | 2007-07-18 | 迪普索尔化学株式会社 | Tin-zinc alloy electroplating method |
CN101752554A (en) * | 2010-01-04 | 2010-06-23 | 北京航空航天大学 | Method for preparing Sn-Zn alloy cathode material of lithium ion battery |
CN108441911A (en) * | 2018-03-20 | 2018-08-24 | 中南大学 | The method that cathodic electrodeposition prepares manganese cobalt composite material |
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Patent Citations (3)
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CN101001982A (en) * | 2004-08-10 | 2007-07-18 | 迪普索尔化学株式会社 | Tin-zinc alloy electroplating method |
CN101752554A (en) * | 2010-01-04 | 2010-06-23 | 北京航空航天大学 | Method for preparing Sn-Zn alloy cathode material of lithium ion battery |
CN108441911A (en) * | 2018-03-20 | 2018-08-24 | 中南大学 | The method that cathodic electrodeposition prepares manganese cobalt composite material |
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Title |
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Dealloying: An effective method for scalable fabrication of 0D, 1D, 2D, 3D materials and its application in energy storage;Yongling An等;《Nano Today》;第1-53页 * |
Sn-Zn无铅钎料的电沉积工艺研究;陈可茂;《工程科技Ⅰ辑》;B015-33 * |
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