CN112645314A - Graphene conductive liquid and preparation method and application thereof - Google Patents
Graphene conductive liquid and preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000007788 liquid Substances 0.000 title claims abstract description 53
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 20
- 239000010439 graphite Substances 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 239000000725 suspension Substances 0.000 claims abstract description 3
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 2
- 239000000243 solution Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 7
- 239000006258 conductive agent Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 6
- 239000002482 conductive additive Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229910004786 P-Li Inorganic materials 0.000 description 1
- 229910004796 P—Li Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 238000000875 high-speed ball milling Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/28—Solid content in solvents
-
- 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 belongs to the technical field of preparation of conductive agents, and particularly relates to a graphene conductive liquid and a preparation method and application thereof. The preparation method of the graphene conductive liquid comprises the following steps: step 1, uniformly mixing expanded graphite, a solvent and a dispersing agent to obtain turbid liquid; step 2, introducing protective gas into the suspension obtained in the step 1 in a pressurizing manner to obtain a mixed solution; step 3, performing ball milling treatment on the mixed liquid obtained in the step 2, and step 4, performing ultrasonic treatment on the dispersion liquid obtained in the step 3; and 5, concentrating the dispersion liquid obtained in the step 4 to obtain the graphene conductive liquid. The graphene conductive liquid prepared by the preparation method provided by the invention has about 5-20 graphene layers, good conductivity and excellent low-temperature performance, and has a discharge capacity retention rate of 76-80% at-20 ℃ and 1C and a discharge capacity retention rate of more than 95% at 20℃ rate.
Description
Technical Field
The invention belongs to the technical field of preparation of conductive agents, and particularly relates to a graphene conductive liquid and a preparation method and application thereof.
Background
The lithium ion battery has the advantages of high voltage, large energy density, rapid charge and discharge, long service life, no memory effect and the like, and becomes an important development direction of new energy. The lithium ion battery using the lithium iron phosphate as the anode has the advantages of good thermal stability, high safety, long cycle life, low raw material cost and the like. However, the conductivity of the lithium iron phosphate material is low, so that the excellent conductive additive is added in the preparation process of the lithium iron phosphate anode slurry, the electron transfer rate in the anode material can be obviously improved, and the effects of improving the multiplying power performance and the cycle performance of the battery are achieved. At present, commercial conductive agents are mainly carbon materials, and mainly comprise conductive graphite, acetylene black, Super P-Li and carbon nanotubes.
The graphene is represented by sp2The two-dimensional nano carbon material composed of hybridized carbon atoms has novel material chemical properties and extremely high conductivity. The graphene can be wrapped to form zero-dimensional fullerene, can be curled into one-dimensional carbon nanotubes, can be stacked into three-dimensional graphite, and can be easily wrapped around electrode active material particles like a 'film' to form surface contact to form a three-dimensional conductive network. The graphene conductive additive can improve and improve the low-temperature performance, the cycling stability and the rate performance of the lithium iron phosphate anode.
In the existing methods for preparing the graphene conductive liquid, a chemical vapor deposition method and a chemical synthesis method have the defects of high cost and low yield, and a chemical oxidation-reduction method has the defects of more product defects and serious environmental pollution.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene conductive liquid, aiming at the defects of high preparation cost and serious environmental pollution of the existing graphene.
The invention also provides application of the graphene conductive liquid, and the conductive liquid can be applied to a lithium iron phosphate positive electrode and has good conductivity.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of a graphene conductive liquid comprises the following steps:
step 1, uniformly mixing expanded graphite, a solvent and a dispersing agent to obtain turbid liquid;
step 2, introducing protective gas into the suspension obtained in the step 1 in a pressurizing manner to obtain a mixed solution;
step 3, performing ball milling treatment on the mixed solution obtained in the step 2,
step 4, carrying out ultrasonic treatment on the dispersion liquid obtained in the step 3;
and 5, concentrating the dispersion liquid obtained in the step 4 to obtain the graphene conductive liquid.
Preferably, the mass ratio of the expanded graphite to the solvent in the step 1 is 1:10-1:100, the ratio of the expanded graphite to the dispersant is 100:1-10:1, and the expanded graphite is in a powder shape.
Preferably, the particle size of the expanded graphite is 0.1 μm to 1 mm.
Preferably, the ball milling in the step 3 adopts a high-speed planetary ball mill, the rotating speed of the ball mill is set to be 1000-5000r/min, the ball milling time is 5-30min, and the ball milling times are 1-3.
Preferably, the ultrasonic treatment in the step 4 has ultrasonic power of 500-.
Preferably, the protective gas in the step 2 is nitrogen, and the pressure is 5-10 MPa.
Preferably, the concentration in step 5 is centrifugation, suction filtration or pressure filtration.
Preferably, the solvent in step 1 is N-methyl pyrrolidone, and the dispersant is a mixture of one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and polyvinylpyrrolidone.
The graphene conductive liquid prepared by the preparation method.
The application of the graphene conductive liquid is characterized in that the graphene conductive liquid can be applied to a lithium iron phosphate anode.
The invention has the advantages of
(1) The raw materials adopted by the invention have rich resources, simple process and good dispersibility;
(2) the graphene conductive liquid prepared by the preparation method provided by the invention has about 5-20 graphene layers, good conductivity and excellent low-temperature performance, and has a discharge capacity retention rate of 76-80% at-20 ℃ and 1C and a discharge capacity retention rate of more than 95% at 20℃ rate.
Drawings
Fig. 1 is a 3C charge-discharge cycle performance curve of the graphene conductive liquid prepared in example 1 for a lithium iron phosphate battery;
fig. 2 is a 1C constant current discharge curve of the graphene conductive liquid prepared in example 1 at-20 ℃ for a lithium iron phosphate battery;
fig. 3 is a constant current discharge curve of the graphene conductive liquid prepared in example 1 for a lithium iron phosphate battery at 20C compared with 1C.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the embodiments are not limited thereto.
Example 1
Step 1, respectively weighing 50g of powdery expanded graphite, 5000g N-methyl pyrrolidone and 5g of sodium dodecyl benzene sulfonate, stirring and mixing N-methyl pyrrolidone and sodium dodecyl benzene sulfonate, and slowly adding the powdery expanded graphite to be uniformly mixed while stirring, wherein the particle size of the expanded graphite is 0.1 mu m-1 mm;
step 2, introducing nitrogen into the mixed liquid obtained in the step 1 in a pressurizing mode, wherein the pressure is 10 Mpa;
step 3, placing the mixed liquor obtained in the step 2 into a high-speed planetary ball mill for ball milling treatment, wherein the rotating speed of the ball mill is 5000r/min, the ball milling time is 30min, and the ball milling times are 3 times;
step 4, placing the dispersion liquid obtained in the step 3 in an ultrasonic instrument for ultrasonic treatment, wherein the ultrasonic power is 2000W, and the time is 5 h;
and 5, centrifuging the dispersion liquid obtained in the step 4 to obtain a concentrated graphene conductive liquid, wherein the mass percent of graphene is between 5% and 99%, and the conductive liquid is suitable for a lithium iron phosphate anode.
Example 2
Step 1, respectively weighing 50g of powdery expanded graphite, 2500g N-methyl pyrrolidone, 0.5g of sodium dodecyl benzene sulfonate and 0.5g of polyvinylpyrrolidone, stirring and mixing N-methyl pyrrolidone, sodium dodecyl benzene sulfonate and polyvinylpyrrolidone, and slowly adding the powdery expanded graphite to be uniformly mixed while stirring, wherein the particle size of the expanded graphite is 0.1 mu m-1 mm;
step 2, introducing nitrogen into the mixed liquid obtained in the step 1 in a pressurizing mode, wherein the pressure is 5 Mpa;
step 3, placing the mixed liquor obtained in the step 2 into a high-speed planetary ball mill for ball milling treatment, wherein the rotating speed of the ball mill is 2500r/min, the ball milling time is 15min, and the ball milling times are 3 times;
step 4, placing the dispersion liquid obtained in the step 3 in an ultrasonic instrument for ultrasonic treatment, wherein the ultrasonic power is 1000W, and the time is 2 h;
and 5, centrifuging the dispersion liquid obtained in the step 4 to obtain a concentrated graphene conductive liquid, wherein the mass percent of graphene is between 5% and 99%, and the conductive liquid is suitable for a lithium iron phosphate anode.
According to the technical methods of the embodiment 1 and the embodiment 2, graphite is mechanically stripped by utilizing the comprehensive actions of high-speed ball milling, high-frequency oscillation and ultrasonic stripping, so that graphene dispersion liquid is obtained, and then the concentrated graphene conductive liquid can be obtained through centrifugation. The method has the advantages of simple process, green and pollution-free preparation process and good dispersibility.
The graphene conductive liquid prepared in the embodiment 1 is applied to the preparation of lithium iron phosphate anode slurry, and the addition amount of the graphene conductive liquid is 0.5-10% (mass percentage content) of the lithium iron phosphate anode. Dissolving polyvinylidene fluoride (PVDF) binder in N-methyl pyrrolidone, adding graphene conductive liquid, uniformly stirring, adding lithium iron phosphate positive active material, and stirring and dispersing to obtain lithium iron phosphate positive slurry. The 3C charge-discharge cycle performance of the graphene conductive liquid prepared by the preparation method for the lithium iron phosphate battery is shown in figure 1, and the 1C constant current discharge performance of the graphene conductive liquid at-20 ℃ for the lithium iron phosphate battery is shown in figure 2; the constant-current discharge performance of the graphene conductive liquid for the lithium iron phosphate battery 20C compared with that of the graphene conductive liquid for the lithium iron phosphate battery 1C is shown in fig. 3. According to the pictures, the graphene conductive liquid serving as the conductive additive of the lithium iron phosphate anode is superior to the traditional conductive additive, the cycle stability, the low-temperature performance and the rate capability of the lithium iron phosphate battery can be obviously improved and promoted, the capacity retention rate is more than or equal to 87% after 4000 times of 3C cycle, the 1C discharge capacity retention rate at minus 20 ℃ is 76% -80%, and the 20℃ rate discharge capacity retention rate is more than 95%.
Claims (10)
1. A preparation method of a graphene conductive liquid is characterized by comprising the following steps:
step 1, uniformly mixing expanded graphite, a solvent and a dispersing agent to obtain turbid liquid;
step 2, introducing protective gas into the suspension obtained in the step 1 in a pressurizing manner to obtain a mixed solution;
step 3, performing ball milling treatment on the mixed solution obtained in the step 2;
step 4, carrying out ultrasonic treatment on the dispersion liquid obtained in the step 3;
and 5, concentrating the dispersion liquid obtained in the step 4 to obtain the graphene conductive liquid.
2. The preparation method according to claim 1, wherein the mass ratio of the expanded graphite to the solvent in the step 1 is 1:10 to 1:100, the ratio of the expanded graphite to the dispersant is 100:1 to 10:1, and the expanded graphite is in a powder form.
3. The production method according to claim 2, wherein the particle size of the expanded graphite is 0.1 μm to 1 mm.
4. The method as claimed in claim 1, wherein the ball milling in step 3 is performed by a high-speed planetary ball mill, the rotation speed of the ball mill is set to 1000-.
5. The method as claimed in claim 1, wherein the ultrasonic treatment in step 4 has an ultrasonic power of 500-2000W and a time of 2-5 h.
6. The method according to claim 1, wherein the shielding gas in step 2 is nitrogen and the pressure is 5 to 10 Mpa.
7. Centrifuging, filtering or press filtering.
8. The method according to claim 1, wherein the solvent in step 1 is N-methyl pyrrolidone, and the dispersant is a mixture of one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and polyvinylpyrrolidone.
9. The graphene conductive liquid prepared by the preparation method of any one of claims 1 to 8.
10. The application of the graphene conductive solution according to claim 9, wherein the graphene conductive solution can be applied to a lithium iron phosphate positive electrode.
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| CN202110095408.1A CN112645314A (en) | 2021-01-25 | 2021-01-25 | Graphene conductive liquid and preparation method and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104993137A (en) * | 2015-04-24 | 2015-10-21 | 深圳市德方纳米科技股份有限公司 | Graphene conductive solution, and preparation method and application thereof |
| WO2015196853A1 (en) * | 2014-06-26 | 2015-12-30 | 江苏华东锂电技术研究院有限公司 | Preparation method for lithium iron phosphate |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
| CN109167016A (en) * | 2018-09-05 | 2019-01-08 | 盐城市新能源化学储能与动力电源研究中心 | A kind of anode material for lithium-ion batteries and its preparation method and application |
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- 2021-01-25 CN CN202110095408.1A patent/CN112645314A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015196853A1 (en) * | 2014-06-26 | 2015-12-30 | 江苏华东锂电技术研究院有限公司 | Preparation method for lithium iron phosphate |
| CN104993137A (en) * | 2015-04-24 | 2015-10-21 | 深圳市德方纳米科技股份有限公司 | Graphene conductive solution, and preparation method and application thereof |
| CN107628610A (en) * | 2017-10-30 | 2018-01-26 | 北京万源工业有限公司 | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid |
| CN109167016A (en) * | 2018-09-05 | 2019-01-08 | 盐城市新能源化学储能与动力电源研究中心 | A kind of anode material for lithium-ion batteries and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 陈玉华: "《新型清洁能源技术》", 31 January 2019, 知识产权出版社, pages: 211 - 213 * |
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