CN110931773A - Preparation method of battery positive electrode material - Google Patents
Preparation method of battery positive electrode material Download PDFInfo
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- CN110931773A CN110931773A CN201911122098.7A CN201911122098A CN110931773A CN 110931773 A CN110931773 A CN 110931773A CN 201911122098 A CN201911122098 A CN 201911122098A CN 110931773 A CN110931773 A CN 110931773A
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a battery anode material, which specifically comprises the following steps: step 1, soaking blue algae in diammonium phosphate; step 2, preparing blue algae powder; step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, and then adding lithium hydroxide, stearic acid and N-methylpyrrolidone to obtain a suspension; step 4, heating the suspension, filtering and drying to obtain filter residue; step 5, putting the filter residue into an ethanol solution, and adding chloroiridic acid; and 6, adding blue algae powder, and calcining to obtain the battery anode material. The anode material prepared by the invention has strong cycle performance, utilizes the unicellular structure of blue-green algae, can utilize wastes and reduce the cost, has simple preparation process, high yield and no pollution, and simultaneously has good conductivity, reversible specific capacity and better cycle stability.
Description
Technical Field
The invention belongs to the technical field of battery preparation, and relates to a preparation method of a battery anode material.
Background
In order to meet the increasing energy demand and avoid global resource exhaustion and long-term damage to the environment, the problem to be solved urgently is to find an energy storage battery with high working voltage, high energy density, long cycle life, small self-discharge and environmental friendliness. Lithium ion batteries are highly desirable as a highly efficient energy storage battery for a wide range of applications. In recent years, lithium ion batteries have shown important application prospects in the fields of portable electronic devices, electric automobiles, aerospace and the like. However, with the increasing demand of people on the performance of energy storage batteries, lithium ion batteries with higher energy density, high specific capacity and good cycling stability are developed, which is a necessary trend for the development of future energy storage batteries, and the key point for developing high-performance lithium ion batteries lies in searching for suitable electrode materials.
Disclosure of Invention
The invention aims to provide a preparation method of a battery anode material, which solves the problem of poor electrode cycle stability in the prior art.
The invention adopts the technical scheme that a preparation method of a battery anode material is specifically carried out according to the following steps:
step 1, taking the dried blue algae, soaking the blue algae in a diamine hydrogen phosphate solution, and taking out and drying the blue algae;
step 2, carbonizing the soaked blue algae, cooling and crushing to obtain blue algae powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, then sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension;
step 4, pouring the suspension into a sealer, heating, taking out after the reaction is finished, filtering and drying to obtain filter residue;
step 5, putting the filter residue into an ethanol solution, adding chloroiridic acid, soaking, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding blue algae powder, stirring, filtering, drying, and calcining to obtain the battery anode material.
In the step 1, the blue algae is any one of nostoc, cyanobacteria and oscillatoria.
In the step 1, the mass concentration of the diammonium hydrogen phosphate solution is 20-30%, and the soaking time is 1-3 h.
In the step 2, the carbonization temperature is 300-500 ℃, the carbonization time is 1-4 h, and the inert gas used in carbonization is argon.
In the step 3, the mass ratio of the manganese dioxide to the sodium pyrophosphate solution is 1: 0.1-0.3, the mass ratio of the manganese dioxide to the lithium hydroxide is 1: 2-3, the mass concentration of stearic acid is 0.1-0.15%, and the mass concentration of N-methylpyrrolidone is 5-8%.
In the step 4, the heating temperature is 150-200 ℃, and the heating time is 10-12 h.
In the step 5, the mass ratio of the filter residue to the ethanol is 1: 5-6, the mass concentration of the iridium element in the solution is 5-10%, and the soaking time is 2-4 h.
In the step 6, the calcination time is 4-5 h, and the calcination temperature is 400-600 ℃.
The positive electrode material prepared by the method has the beneficial effects that the cycle performance is strong, the unicellular structure of blue-green algae is utilized, strong alkali is not needed for pore forming, the preparation steps are few, waste can be utilized, the cost can be reduced, the preparation process is simple, the yield is high, no pollution is caused, the product structure is amorphous, the safety performance is high, and meanwhile, the positive electrode material has good conductivity, reversible specific capacity and better cycle stability.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
A preparation method of a battery positive electrode material specifically comprises the following steps:
step 1, taking the dried blue algae, soaking the blue algae in a diamine hydrogen phosphate solution, and taking out and drying the blue algae;
step 2, carbonizing the soaked blue algae, cooling and crushing to obtain blue algae powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, then sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension;
step 4, pouring the suspension into a sealer, heating, taking out after the reaction is finished, filtering and drying to obtain filter residue;
step 5, putting the filter residue into an ethanol solution, adding chloroiridic acid, soaking, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding blue algae powder, stirring, filtering, drying, and calcining to obtain the battery anode material.
In the step 1, the blue algae is any one of nostoc, cyanobacteria and oscillatoria.
In the step 1, the mass concentration of the diammonium hydrogen phosphate solution is 20-30%, and the soaking time is 1-3 h.
In the step 2, the carbonization temperature is 300-500 ℃, the carbonization time is 1-4 h, and the inert gas used in carbonization is argon.
In the step 3, the mass ratio of the manganese dioxide to the sodium pyrophosphate solution is 1: 0.1-0.3, the mass ratio of the manganese dioxide to the lithium hydroxide is 1: 2-3, the mass concentration of stearic acid is 0.1-0.15%, and the mass concentration of N-methylpyrrolidone is 5-8%.
In the step 4, the heating temperature is 150-200 ℃, and the heating time is 10-12 h.
In the step 5, the mass ratio of the filter residue to the ethanol is 1: 5-6, the mass concentration of the iridium element in the solution is 5-10%, and the soaking time is 2-4 h.
In the step 6, the calcination time is 4-5 h, and the calcination temperature is 400-600 ℃.
The lithium battery is a rechargeable battery and mainly works by moving lithium ions between a positive electrode and a negative electrode, when the lithium battery is charged, the lithium ions are extracted from crystal lattices of a positive electrode material and inserted into the crystal lattices of a negative electrode material after passing through an electrolyte, so that the negative electrode is rich in lithium, the positive electrode is poor in lithium, when the lithium battery is discharged, the lithium ions are extracted from the crystal lattices of the negative electrode material and inserted into the crystal lattices of the positive electrode material after passing through the electrolyte, so that the positive electrode is rich in lithium, and the negative electrode is poor in lithium. Thus, the difference of the potentials of the anode and cathode materials relative to the metallic lithium during the insertion and extraction of lithium ions is the working voltage of the battery.
The positive electrode is the end with higher potential in the power supply, the positive electrode generally contains lithium ions, has variable-valence transition metal and is suitable for a space structure of a lithium ion extraction ground, the positive electrode material has higher oxidation-reduction potential, so that the battery has higher output voltage, the lithium ions can be greatly and reversibly inserted into and extracted from the positive electrode material, so that the battery has high capacity, the structure of the positive electrode material does not change in the lithium ion insertion/extraction process, the good cycle performance of the battery is ensured, the oxidation-reduction potential of the positive electrode changes slightly in the lithium ion insertion/extraction process, the voltage of the battery does not change significantly, so that the battery is ensured to be charged and discharged smoothly, the conductivity of the positive electrode material is higher, and the battery is charged and discharged in a large-current mode;
the negative electrode is the end with lower potential in the power supply, in the primary battery, it is the electrode with oxidation action, written on the left side in the battery reaction, from the physical point of view, it is the electrode from which the electrons flow out in the circuit, and the negative electrode material is the raw material of the negative electrode in the battery, the negative electrode of the lithium ion battery is made up by mixing the negative electrode active material carbon material or non-carbon material, adhesive and additive to make paste adhesive, evenly smearing on the two sides of the copper foil, drying and rolling.
Example 1
A preparation method of a battery positive electrode material specifically comprises the following steps:
step 1, soaking sun-dried nostoc into a 25% diammonium hydrogen phosphate solution for 2 hours, and then taking out and drying;
step 2, carbonizing the soaked nostoc for 2 hours at 400 ℃, and cooling and crushing to obtain nostoc powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension, wherein the mass ratio of the manganese dioxide to the lithium hydroxide is 1:2.5, the mass concentration of the stearic acid is 0.12%, and the mass concentration of the N-methylpyrrolidone is 7%;
step 4, pouring the suspension into a sealer, heating at 180 ℃ for 11 hours, taking out after the reaction is finished, filtering and drying to obtain filter residues;
step 5, putting the filter residue into an ethanol solution, adding chloroiridic acid into the solution, wherein the mass ratio of the filter residue to the ethanol is 1:5.5, the mass concentration of iridium in the solution is 7%, soaking the solution for 3 hours, putting the solution into a vacuum box, vacuumizing the vacuum box until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding nostoc powder, stirring, filtering, drying and then calcining for 4.5 hours at the calcining temperature of 500 ℃ to obtain the battery anode material.
In the step 1, the blue algae is any one of blue algae and oscillatoria.
Example 2
A preparation method of a battery positive electrode material specifically comprises the following steps:
step 1, taking sun-dried cyanobacteria, soaking the cyanobacteria in a 30% diammonium hydrogen phosphate solution for 1 hour, and taking out and drying the cyanobacteria;
step 2, carbonizing the soaked cyanobacteria at 500 ℃ for 1h, cooling and crushing to obtain cyanobacteria powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension, wherein the mass ratio of the manganese dioxide to the lithium hydroxide is 1:2, the mass concentration of the stearic acid is 0.15%, and the mass concentration of the N-methylpyrrolidone is 5%;
step 4, pouring the suspension into a sealer, heating at 200 ℃ for 10 hours, taking out after the reaction is finished, filtering and drying to obtain filter residues;
step 5, putting the filter residue into an ethanol solution, wherein the mass ratio of the filter residue to the ethanol is 1:6, adding chloroiridic acid, the mass concentration of iridium in the solution is 5%, soaking for 4h, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding the blue-green algae powder, stirring, filtering, drying and then calcining for 4 hours at 600 ℃ to obtain the battery anode material.
Example 3
A preparation method of a battery positive electrode material specifically comprises the following steps:
step 1, soaking dried nostoc into 20% diammonium hydrogen phosphate solution for 3 hours, and then taking out and drying;
step 2, carbonizing the soaked nostoc for 4 hours at the carbonization temperature of 300 ℃, and cooling and crushing to obtain nostoc powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension, wherein the mass ratio of the manganese dioxide to the lithium hydroxide is 1:3, the mass concentration of the stearic acid is 0.1%, and the mass concentration of the N-methylpyrrolidone is 8%;
step 4, pouring the suspension into a sealer, heating at 150 ℃ for 12 hours, taking out after the reaction is finished, filtering and drying to obtain filter residues;
step 5, putting the filter residue into an ethanol solution, wherein the mass ratio of the filter residue to the ethanol is 1:5, adding chloroiridic acid, the mass concentration of iridium in the solution is 10%, soaking for 2h, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding nostoc powder, stirring, filtering, drying and then calcining for 5 hours at 400 ℃ to obtain the battery anode material.
Example 4
A preparation method of a battery positive electrode material specifically comprises the following steps:
step 1, soaking sun-dried nostoc into a 30% diammonium hydrogen phosphate solution for 2 hours, and then taking out and drying;
step 2, carbonizing the soaked nostoc for 2 hours at the carbonization temperature of 300 ℃, and crushing after cooling to obtain nostoc powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension, wherein the mass ratio of the manganese dioxide to the lithium hydroxide is 1:2, the mass concentration of the stearic acid is 0.1%, and the mass concentration of the N-methylpyrrolidone is 8%;
step 4, pouring the suspension into a sealer, heating at 175 ℃ for 12 hours, taking out after the reaction is finished, filtering and drying to obtain filter residues;
step 5, putting the filter residue into an ethanol solution, wherein the mass ratio of the filter residue to the ethanol is 1:5, adding chloroiridic acid, the mass concentration of iridium in the solution is 10%, soaking for 3h, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding nostoc powder, stirring, filtering, drying and then calcining for 4 hours at 600 ℃ to obtain the battery anode material.
Claims (8)
1. The preparation method of the battery positive electrode material is characterized by comprising the following steps:
step 1, taking the dried blue algae, soaking the blue algae in a diamine hydrogen phosphate solution, and taking out and drying the blue algae;
step 2, carbonizing the soaked blue algae, cooling and crushing to obtain blue algae powder;
step 3, weighing manganese dioxide, putting the manganese dioxide into a sodium pyrophosphate solution, uniformly stirring, then sequentially adding lithium hydroxide, stearic acid and N-methylpyrrolidone, and continuously stirring during the adding process to obtain a suspension;
step 4, pouring the suspension into a sealer, heating, taking out after the reaction is finished, filtering and drying to obtain filter residue;
step 5, putting the filter residue into an ethanol solution, adding chloroiridic acid, soaking, putting the solution into a vacuum box, vacuumizing until no bubbles are generated, and taking out the filter residue;
and 6, putting the filter residue obtained in the step 5 into an ethanol solution, adding blue algae powder, stirring, filtering, drying, and calcining to obtain the battery anode material.
2. The method for preparing a battery cathode material according to claim 1, wherein in the step 1, the blue-green algae is any one of nostoc, cyanobacteria and oscillatoria.
3. The method for preparing the battery cathode material according to claim 1, wherein in the step 1, the mass concentration of the diammonium phosphate solution is 20-30%, and the soaking time is 1-3 h.
4. The method for preparing the battery cathode material according to claim 1, wherein in the step 2, the carbonization temperature is 300-500 ℃, the carbonization time is 1-4 h, and the inert gas used in carbonization is argon.
5. The method for preparing the battery cathode material according to claim 1, wherein in the step 3, the mass ratio of the manganese dioxide to the sodium pyrophosphate solution is 1: 0.1-0.3, the mass ratio of the manganese dioxide to the lithium hydroxide is 1: 2-3, the mass concentration of stearic acid is 0.1-0.15%, and the mass concentration of N-methylpyrrolidone is 5-8%.
6. The method for preparing the battery cathode material according to claim 1, wherein in the step 4, the heating temperature is 150-200 ℃ and the heating time is 10-12 h.
7. The preparation method of the battery cathode material according to claim 1, wherein in the step 5, the mass ratio of the filter residue to the ethanol is 1: 5-6, the mass concentration of the iridium element in the solution is 5-10%, and the soaking time is 2-4 h.
8. The method for preparing the battery cathode material according to claim 1, wherein in the step 6, the calcination time is 4-5 h, and the calcination temperature is 400-600 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102983334A (en) * | 2012-12-18 | 2013-03-20 | 中国科学院宁波材料技术与工程研究所 | Positive pole material of lithium ion battery and preparation method of material |
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| CN109920999A (en) * | 2019-03-22 | 2019-06-21 | 广西师范大学 | A kind of cyanobacteria base anode material and preparation method thereof for lithium-sulfur cell |
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2019
- 2019-11-15 CN CN201911122098.7A patent/CN110931773A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102983334A (en) * | 2012-12-18 | 2013-03-20 | 中国科学院宁波材料技术与工程研究所 | Positive pole material of lithium ion battery and preparation method of material |
| CN103413943A (en) * | 2013-08-14 | 2013-11-27 | 宁波奈克斯特新材料科技有限公司 | Lithium manganese phosphate positive electrode material and preparation method thereof |
| CN109888276A (en) * | 2019-03-05 | 2019-06-14 | 江西省灿辉新能源科技有限公司 | A kind of preparation method of lithium manganate cell positive electrode material |
| CN109920999A (en) * | 2019-03-22 | 2019-06-21 | 广西师范大学 | A kind of cyanobacteria base anode material and preparation method thereof for lithium-sulfur cell |
Non-Patent Citations (1)
| Title |
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Application publication date: 20200327 |