CN112436128A - Preparation method of manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode - Google Patents
Preparation method of manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode Download PDFInfo
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- CN112436128A CN112436128A CN202011385930.5A CN202011385930A CN112436128A CN 112436128 A CN112436128 A CN 112436128A CN 202011385930 A CN202011385930 A CN 202011385930A CN 112436128 A CN112436128 A CN 112436128A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 36
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- WSHADMOVDWUXEY-UHFFFAOYSA-N manganese oxocobalt Chemical compound [Co]=O.[Mn] WSHADMOVDWUXEY-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910003164 Mn2CoO4 Inorganic materials 0.000 claims abstract description 13
- 150000001868 cobalt Chemical class 0.000 claims abstract description 13
- 150000002696 manganese Chemical class 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 229920002678 cellulose Polymers 0.000 claims abstract description 4
- 239000001913 cellulose Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000013329 compounding Methods 0.000 claims description 6
- 229920001046 Nanocellulose Polymers 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical group [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000010000 carbonizing Methods 0.000 abstract description 3
- 239000011572 manganese Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000010405 anode material Substances 0.000 abstract description 2
- 230000008859 change Effects 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000006258 conductive agent Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 102000004310 Ion Channels Human genes 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—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
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
-
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- 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
-
- 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
-
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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 manganese-cobalt-oxygen composite two-dimensional carbon material for a lithium ion battery cathode, which comprises the steps of mixing manganese salt and cobalt salt, taking nano-cellulose with high length-diameter ratio as a two-dimensional carbon material template, carbonizing at high temperature and graphitizing under the atmosphere of inert gas to obtain Mn2CoO4A modified two-dimensional carbon material. The two-dimensional structure of the carbon material can increase the conductivity on the one hand and prevent Mn in the cyclic process on the other hand2CoO4The structural change of the lithium ion battery lead to the reduction of the cycle performance, so that the material is used as the anode material of the lithium ion batteryThe charge and discharge performance can be improved.
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery cathode material, in particular to a preparation method of a manganese cobalt oxygen composite two-dimensional carbon material for a lithium ion battery cathode.
Background
With the development of electronic devices and electric vehicles, higher and higher demands are made on the capacity and cycle performance of batteries. The lithium ion battery has the advantages of long cycle life, large specific capacity, high working voltage and the like, and becomes a novel green high-energy chemical power supply with great development potential in the world.
The current commercialized lithium battery negative electrode material is graphite, is limited by theoretical capacity, and has limited energy density promotion space, so that development of a novel high-specific-capacity lithium battery negative electrode material is very important.
The metal oxide is considered to be a next generation high energy density lithium ion battery cathode material with great potential due to the advantages of low lithium removal potential, environmental friendliness, abundant reserves, low cost and the like. However, the large expansion and poor conductivity limit the industrialization of the anode material.
The problem can be solved by carbon coating, so that the invention develops a simple preparation method for realizing the metal oxide modified two-dimensional carbon material, and the two-dimensional material has the advantages of improving the electrical property of the material, having a better ion channel, preventing the material from losing efficacy caused by the expansion of the material and having non-important significance for promoting the industrialization process.
Disclosure of Invention
The invention aims to provide a preparation method of a manganese-cobalt-oxygen composite two-dimensional carbon material for a lithium ion battery cathode.
The purpose of the invention is realized by the following scheme: preparation method of manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode, wherein manganese-cobalt-oxygen is Mn2CoO4Mixing manganese salt and cobalt salt, taking nano-cellulose with high length-diameter ratio as a two-dimensional carbon material template, carbonizing at high temperature and graphitizing in an inert gas atmosphere to obtain Mn2CoO4A modified two-dimensional carbon material comprising the steps of:
the method comprises the following steps: respectively preparing 50mL of manganese salt aqueous solution with the molar concentration of 0.8-1M and cobalt salt aqueous solution with the concentration of 0.4-0.5M, wherein the molar ratio of manganese salt to cobalt salt is 2:1, and mixing the manganese salt aqueous solution and the cobalt salt aqueous solution to obtain mixed solution;
step two: taking 200g of 1wt% nanocellulose aqueous solution, mixing with the mixed solution obtained in the step one, stirring for 30-50 min, freeze-drying to obtain powder, grinding the powder, and performing heat treatment in an inert gas atmosphere to obtain Mn2CoO4And compounding the two-dimensional carbon material.
In the first step, the manganese salt is at least one of manganese acetate and manganese chloride; the cobalt salt is cobalt acetate.
And in the second step, the inert gas atmosphere is high-purity argon, the heat treatment temperature is 850-950 ℃, the heat preservation time is 2 hours, the heat preservation time is 1100-1200 ℃, and the temperature rise speed is 15-20 ℃/min.
The invention provides a simple method for realizing Mn2CoO4The method for compounding the two-dimensional carbon material has the advantages of simple preparation process, low preparation cost and simple operation, and has great value for further promoting the practical application of the two-dimensional carbon material. The two-dimensional structure of the carbon material can increase the conductivity on the one hand and prevent Mn in the cyclic process on the other hand2CoO4The cycle performance is reduced due to the structural change, so that the charge and discharge performance of the material can be improved when the material is used as a lithium ion battery cathode material. The material prepared by the method can be used in the fields of lithium ion battery cathode materials, gas detection, gas catalytic treatment and the like.
Drawings
FIG. 1 shows example 2Mn of (2)2CoO4And (3) a cycle chart of the composite two-dimensional carbon material.
Detailed Description
Example 1:
manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode, wherein manganese-cobalt-oxygen is Mn2CoO4Mixing manganese salt and cobalt salt, taking nano-cellulose with high length-diameter ratio as a two-dimensional carbon material template, carbonizing at high temperature and graphitizing in an inert gas atmosphere to obtain Mn2CoO4A modified two-dimensional carbon material is prepared by the following steps:
the method comprises the following steps: respectively preparing 50mL of manganese acetate aqueous solution with the molar concentration of 1M and cobalt acetate aqueous solution with the concentration of 0.5M, and mixing the two solutions to obtain a mixed solution;
step two: taking 200g of 1wt% nanocellulose aqueous solution, mixing with the mixed solution obtained in the first step, stirring for 30-50 min, freeze-drying the obtained solution to obtain powder, grinding the obtained powder, performing heat treatment in an inert gas atmosphere at the temperature of 900 ℃ for 2 hours, at the temperature of 1100 ℃ for 2 hours at the temperature rise speed of 15 ℃/min to obtain Mn2CoO4And compounding the two-dimensional carbon material.
The sample prepared in this example was mixed with a binder (CMC), a conductive agent (SP) and SBR in a mass ratio of 8: 0.5: 1: 0.5, preparing the working electrode into slurry, assembling the working electrode into a button battery, standing for more than 10 hours, and performing charge and discharge tests at the ambient temperature of 25 ℃, wherein the capacity retention rate is 73.3 percent after the circulation for 100 weeks.
Example 2:
a manganese-cobalt-oxygen composite two-dimensional carbon material for a negative electrode of a lithium ion battery is prepared by the following steps similar to example 1:
the method comprises the following steps: respectively preparing 50mL of manganese acetate aqueous solution with the molar concentration of 0.8M and cobalt acetate aqueous solution with the concentration of 0.4M, and mixing the two solutions to obtain a mixed solution;
step two: mixing 200g of 1wt% nanocellulose aqueous solution with the mixed solution obtained in the first step, stirring for 30min, freeze-drying to obtain powder, grinding the powder, and heating in inert gas atmosphereTreating at 950 deg.C for 2 hr, at 1100 deg.C for 2 hr, at a temperature rise rate of 15 deg.C/min to obtain Mn2CoO4And compounding the two-dimensional carbon material.
The sample prepared in this example was mixed with a binder (CMC), a conductive agent (SP) and SBR in a mass ratio of 8: 0.5: 1: 0.5, preparing the working electrode into slurry, assembling the working electrode into a button battery, standing for more than 10 hours, and performing charge and discharge tests at the ambient temperature of 25 ℃, wherein the capacity retention rate is 74.5 percent after the circulation for 100 weeks.
FIG. 1 shows Mn according to the present invention2CoO4The cycle diagram of the composite two-dimensional carbon material can be seen from the diagram, after the composite two-dimensional carbon material is formed, the discharge capacity is 692.3mAh/g from the second circle, and after the composite two-dimensional carbon material is used as a lithium ion battery cathode to be cycled for 100 weeks, the capacity retention rate is 74.5%, the composite two-dimensional carbon material has very good cycle performance, and the capacity is greatly improved compared with a graphite material.
Example 3:
a manganese-cobalt-oxygen composite two-dimensional carbon material for a negative electrode of a lithium ion battery is prepared by the following steps similar to example 1:
the method comprises the following steps: respectively preparing 50mL of manganese salt aqueous solution with the molar concentration of 0.9M and cobalt salt aqueous solution with the concentration of 0.45M, and mixing the two solutions to obtain mixed solution;
step two: taking 200g of 1wt% nanocellulose aqueous solution, mixing with the mixed solution obtained in the first step, stirring for 30-50 min, freeze-drying to obtain powder, grinding the powder, performing heat treatment in an inert gas atmosphere at 850 ℃, keeping the temperature for 2 hours, keeping the temperature at 1200 ℃ for 2 hours, and keeping the temperature at the rate of 15 ℃/min to obtain Mn2CoO4And compounding the two-dimensional carbon material.
The sample prepared in this example was mixed with a binder (CMC), a conductive agent (SP) and SBR in a mass ratio of 8: 0.5: 1: 0.5, preparing the working electrode into slurry, assembling the working electrode into a button battery, standing for more than 10 hours, and performing charge and discharge tests at the ambient temperature of 25 ℃, wherein the capacity retention rate is 70.9% after 100 weeks of circulation.
The embodiments described above are described to facilitate an understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications to the present invention based on the disclosure of the present invention within the protection scope of the present invention.
Claims (3)
1. Preparation method of manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode, wherein manganese-cobalt-oxygen is Mn2CoO4The method is characterized in that manganese salt and cobalt salt are mixed, nano-cellulose with high length-diameter ratio is used as a two-dimensional carbon material template, and the two-dimensional carbon material template is carbonized and graphitized at high temperature in an inert gas atmosphere to obtain Mn2CoO4A modified two-dimensional carbon material comprising the steps of:
the method comprises the following steps: respectively preparing 50mL of manganese salt aqueous solution with the molar concentration of 0.8-1M and cobalt salt aqueous solution with the concentration of 0.4-0.5M, wherein the molar ratio of manganese salt to cobalt salt is 2:1, and mixing the manganese salt aqueous solution and the cobalt salt aqueous solution to obtain mixed solution;
step two: taking 200g of 1wt% nanocellulose aqueous solution, mixing with the mixed solution obtained in the step one, stirring for 30-50 min, freeze-drying to obtain powder, grinding the powder, and performing heat treatment in an inert gas atmosphere to obtain Mn2CoO4And compounding the two-dimensional carbon material.
2. The method for preparing a manganese-cobalt-oxygen composite two-dimensional carbon material for a negative electrode of a lithium ion battery according to claim 1, wherein: in the first step, the manganese salt is at least one of manganese acetate and manganese chloride; the cobalt salt is cobalt acetate.
3. The method for preparing a manganese-cobalt-oxygen composite two-dimensional carbon material for a negative electrode of a lithium ion battery according to claim 1, wherein: and in the second step, the inert gas atmosphere is high-purity argon, the heat treatment temperature is 850-950 ℃, the heat preservation time is 2 hours, the heat preservation time is 1100-1200 ℃, and the temperature rise speed is 15-20 ℃/min.
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Cited By (1)
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Application publication date: 20210302 |