CN111509202A - Composite cathode material and preparation method and application thereof - Google Patents
Composite cathode material and preparation method and application thereof Download PDFInfo
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- CN111509202A CN111509202A CN202010301086.7A CN202010301086A CN111509202A CN 111509202 A CN111509202 A CN 111509202A CN 202010301086 A CN202010301086 A CN 202010301086A CN 111509202 A CN111509202 A CN 111509202A
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- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 239000010406 cathode material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 59
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 49
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000007774 positive electrode material Substances 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000013329 compounding Methods 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000000463 material Substances 0.000 abstract description 7
- 238000007599 discharging Methods 0.000 abstract description 6
- 239000010405 anode material Substances 0.000 abstract description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 229910032387 LiCoO2 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 238000012916 structural analysis Methods 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
-
- 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
-
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
-
- 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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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention belongs to the field of battery materials, and provides a composite cathode material and a preparation method and application thereof. The composite anode material is prepared by dispersing graphene into a dispersing agent, adding lithium iron phosphate, removing the dispersing agent, and applying the composite anode material to a power battery system. According to the invention, graphene and lithium iron phosphate are compounded, and isolated lithium iron phosphate nano particles can be linked in the electrode by the graphene, so that a high-efficiency conductive network is constructed, and the rapid charging and discharging performance is better improved.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to a composite cathode material and a preparation method and application thereof.
Background
The lithium ion battery is a secondary battery, and is relatively to the traditional secondary batteryThe lithium ion battery consists of a positive electrode, a negative electrode, a diaphragm, electrolyte and a battery shell, wherein the positive electrode material occupies an important position in the aspects of the cost and the performance of the battery2、LiCoO2、LiFePO4And ternary materials, etc., wherein L iNiO2、LiCoO2And ternary materials although high in energy density, generally suffer from poor safety ratio lithium iron phosphate (L iFePO)4L FP) is obviously better in safety, and has the advantages of higher energy density and theoretical capacity, rich reserve, environmental protection, stable cycle performance and the like, so the lithium iron phosphate is gradually used in power batteries2+Is oxidized. However, the carbon-coated lithium iron phosphate material is relatively loose and uneven, so that the conductivity is improved to a limited extent.
Disclosure of Invention
The invention aims to provide a composite cathode material, a preparation method and application thereof, and the composite cathode material has better rapid charging and discharging performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a composite anode material, which comprises the following preparation steps:
and dispersing graphene into a dispersing agent, adding lithium iron phosphate, and removing the dispersing agent to obtain the composite cathode material.
Preferably, the iron content in the graphene is less than 100ppm, and the conductivity of the graphene is 1300-1500S/cm.
Preferably, the graphene is obtained by calcining graphene oxide at a temperature of 2200 ℃ or higher.
Preferably, the dispersant is methanol, ethanol or acetone.
Preferably, the amount of the graphene is 1-5% of the total mass of the lithium iron phosphate and the graphene.
Preferably, the lithium iron phosphate is a nano-scale particle.
Preferably, the method for removing the dispersant is heating.
Preferably, the heating temperature is 50-80 ℃.
The invention also provides a composite cathode material, which is obtained by compounding graphene and lithium iron phosphate, wherein the graphene is of a two-dimensional film structure, the lithium iron phosphate is of a nanoparticle structure, and the graphene is distributed in the middle of the lithium iron phosphate.
The invention also provides application of the composite cathode material in a power battery system.
According to the composite cathode material and the preparation method and application thereof, graphene and lithium iron phosphate are compounded, so that the graphene is uniformly distributed among lithium iron phosphate nano-particles, the graphene can link isolated lithium iron phosphate nano-particles in an electrode, a high-efficiency conductive network is constructed, and the quick charging and discharging performance of a battery is improved.
Drawings
Fig. 1 is an SEM image of graphene;
FIG. 2 is a Raman spectrum of graphene;
FIG. 3 is an SEM image of lithium iron phosphate and a composite cathode material, FIG. 3a is an SEM image of lithium iron phosphate, and FIG. 3b is an SEM image of a composite cathode material;
FIG. 4 is an XRD pattern of lithium iron phosphate and the composite anode material;
FIG. 5 shows the cycling performance of 18650 cells with composite positive electrode material as the positive electrode;
fig. 6 shows the cycle performance of the soft package power battery with the composite positive electrode material as the positive electrode.
Detailed Description
The invention provides a composite cathode material, a preparation method and application thereof, and the composite cathode material has better rapid charging and discharging performance.
The invention provides a preparation method of a composite anode battery, which comprises the following steps:
and dispersing graphene into a dispersing agent, adding lithium iron phosphate, and removing the dispersing agent to obtain the composite cathode material.
In the invention, the iron content in the graphene is less than 100ppm, more preferably less than 50ppm, and the conductivity of the graphene is preferably 1300-1500S/cm, more preferably 1500S/cm.
The preparation method of the graphene is preferably obtained by calcining graphene oxide, the calcining temperature is preferably 2200 ℃ or above, further preferably 2600 ℃ or above, and the calcining time is preferably 1-3 h, further preferably 2 h.
In the present invention, the dispersant is preferably methanol, ethanol or acetone, and more preferably ethanol, and the dispersant may be uniformly dispersed without any special requirement for the amount of the dispersant used.
The invention preferably adopts an ultrasonic mode for dispersion, has no special requirement on the ultrasonic condition, and can disperse to obtain suspension.
After the suspension is prepared, lithium iron phosphate is added into the suspension.
In the invention, the dosage of the graphene is preferably 1-5% of the total mass of the lithium iron phosphate and the graphene, more preferably 2-4%, and even more preferably 2%.
In the invention, the lithium iron phosphate is preferably nano-sized particles, and the nano size of the lithium iron phosphate is preferably 10-500 nm, and more preferably 100-200 nm.
In the invention, the lithium iron phosphate is preferably fully stirred after being added.
In the present invention, the method for removing the dispersant is preferably heating
In the present invention, the heating temperature is preferably 50 to 80 ℃, and more preferably 60 ℃.
The invention also provides a composite cathode material, which is obtained by compounding graphene and lithium iron phosphate, wherein the graphene is of a two-dimensional film structure, the lithium iron phosphate is of a nanoparticle structure, and the graphene is uniformly distributed in the middle of the lithium iron phosphate.
The invention also provides application of the composite cathode material in a power battery system.
The composite positive electrode material provided by the present invention, the preparation method and the application thereof are described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
And calcining the graphene oxide at the temperature of over 2200 ℃ for 2 hours to obtain the graphene provided by the invention, wherein the graphene provided by the invention has high purity and high conductivity. The Fe content in the graphene is less than 50ppm, and the conductivity is 1300-1500S/cm.
Example 2
According to the mass fraction, taking 2 parts of graphene and 98 parts of lithium iron phosphate, firstly adding the graphene into ethanol, forming uniform turbid liquid through ultrasonic dispersion, then adding the lithium iron phosphate, fully stirring, and finally heating at 60 ℃ to evaporate the ethanol to dryness, thus obtaining the composite cathode material of the embodiment.
Example 3
According to the weight parts, 1 part of graphene and 99 parts of lithium iron phosphate are taken, the graphene is added into methanol, uniform turbid liquid is formed through ultrasonic dispersion, then the lithium iron phosphate is added, sufficient stirring is carried out, and finally the ethanol is heated and evaporated at 50 ℃, so that the composite cathode material is obtained.
Example 4
According to the weight parts, 5 parts of graphene and 95 parts of lithium iron phosphate are taken, the graphene is added into ethanol, uniform turbid liquid is formed through ultrasonic dispersion, then the lithium iron phosphate is added, the mixture is fully stirred, and finally the ethanol is heated and evaporated at the temperature of 80 ℃, so that the composite cathode material is obtained.
Experimental example 1
As shown in fig. 1, the result of performing electron microscope scanning on the graphene prepared in example 1 of the present invention is shown in fig. 1, and it can be observed from fig. 1 that the graphene exhibits a typical two-dimensional thin-film structure characteristic.
The raman spectrum analysis of the graphene prepared in example 1 of the present invention is shown in fig. 2, and as can be observed from fig. 2, no D peak is observed, indicating that sp of the high-purity graphene is present2Very high degree of graphitization with almost defect-free sp3。
Experimental example 2
The composite material prepared in the embodiment 2 of the present invention and the lithium iron phosphate material are subjected to electron microscope scanning. The results are shown in FIG. 3. From fig. 3a, it can be seen that lithium iron phosphate is uniform nanoparticles, and in fig. 3b, it can be observed that graphene having a two-dimensional thin film structure is uniformly distributed in the middle of the lithium iron phosphate nanoparticles. The graphene can link isolated lithium iron phosphate nanoparticles in the electrode to construct a high-efficiency conductive network, so that the quick charging and discharging performance of the battery is improved.
Experimental example 3
Structural analysis is performed on the composite cathode material and the lithium iron phosphate material prepared in embodiment 2 of the present invention, fig. 4 is an XRD chart of the composite cathode material and the lithium iron phosphate, and it can be seen from the XRD chart that the lithium iron phosphate and the composite cathode material both exhibit a complete olivine structure and have a high degree of crystallinity compared with a standard card, and in addition, no diffraction peak of graphene is found in the composite cathode material, possibly due to a small content of graphene in the composite material.
Experimental example 4
When the composite cathode material prepared in example 2 of the present invention is used as the cathode of 18650 battery, the battery performance test is performed, and as shown in fig. 5, it can be seen from the figure that the corresponding 18650 battery has excellent cycle performance, and the capacity retention rate after 2000 cycles is 85.2%.
When the composite cathode material prepared in example 2 of the invention is used as the cathode of a soft package power battery, a battery performance test is performed, and as shown in fig. 6, it can be seen from the figure that the corresponding soft package power battery has excellent cycle performance, and the capacity retention rate after 3000 cycles is 87.5%.
According to the embodiment, the composite cathode material provided by the invention is compounded by adopting graphene and lithium iron phosphate, so that the graphene with a two-dimensional film structure is uniformly distributed in the lithium iron phosphate nanoparticles, the graphene can link isolated lithium iron phosphate nanoparticles in an electrode, a high-efficiency conductive network is constructed, and the quick charging and discharging performance of a battery is improved. And has good electrochemical performance when being applied to a power battery system.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the composite cathode material is characterized by comprising the following preparation steps:
and dispersing graphene into a dispersing agent, adding lithium iron phosphate, and removing the dispersing agent to obtain the composite cathode material.
2. The preparation method of the composite cathode material according to claim 1, wherein the content of iron in the graphene is less than 100ppm, and the conductivity of the graphene is 1300-1500S/cm.
3. The method for producing a composite positive electrode material according to claim 1 or 2, wherein the graphene is obtained by calcining graphene oxide at a temperature of 2200 ℃ or higher.
4. The method for producing a composite positive electrode material according to claim 1, wherein the dispersant is methanol, ethanol, or acetone.
5. The preparation method of the composite cathode material according to claim 1, wherein the amount of the graphene is 1-5% of the total mass of the lithium iron phosphate and the graphene.
6. The method for preparing the composite positive electrode material according to claim 1 or 5, wherein the lithium iron phosphate is a nano-sized particle.
7. The method for producing a composite positive electrode material according to claim 1, wherein the method for removing the dispersant is heating.
8. The method for preparing a composite positive electrode material according to claim 6, wherein the heating temperature is 50 to 80 ℃.
9. The composite cathode material prepared by the preparation method of the composite cathode material according to any one of claims 1 to 8, wherein the composite cathode material is obtained by compounding graphene and lithium iron phosphate, the graphene is of a two-dimensional film structure, the lithium iron phosphate is of a nanoparticle structure, and the graphene is distributed in the middle of the lithium iron phosphate.
10. Use of the composite positive electrode material of claim 9 in a power battery system.
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Citations (5)
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|---|---|---|---|---|
| CN101599543A (en) * | 2009-07-10 | 2009-12-09 | 浙江振龙电源股份有限公司 | A kind of lithium iron (II) phosphate anode of lithium ion battery and preparation method thereof |
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| CN106299251A (en) * | 2015-05-25 | 2017-01-04 | 深圳市沃特玛电池有限公司 | A kind of preparation method of electrokinetic cell composite positive pole |
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-
2020
- 2020-04-16 CN CN202010301086.7A patent/CN111509202A/en active Pending
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Application publication date: 20200807 |