CN113782837A - Preparation method of high-quality graphene battery - Google Patents
Preparation method of high-quality graphene battery Download PDFInfo
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- CN113782837A CN113782837A CN202110883413.9A CN202110883413A CN113782837A CN 113782837 A CN113782837 A CN 113782837A CN 202110883413 A CN202110883413 A CN 202110883413A CN 113782837 A CN113782837 A CN 113782837A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 31
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011267 electrode slurry Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 37
- 239000010439 graphite Substances 0.000 claims description 37
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000006258 conductive agent Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000007773 negative electrode material Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- IAQLJCYTGRMXMA-UHFFFAOYSA-M lithium;acetate;dihydrate Chemical compound [Li+].O.O.CC([O-])=O IAQLJCYTGRMXMA-UHFFFAOYSA-M 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000010008 shearing Methods 0.000 claims description 4
- 238000007581 slurry coating method Methods 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000006256 anode slurry Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000007774 positive electrode material Substances 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000003980 solgel method Methods 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 239000006255 coating slurry Substances 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
Classifications
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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
- H01M10/058—Construction or manufacture
-
- 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
- H01M4/62—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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a preparation method of a high-quality graphene battery, which comprises the following steps: s10, preparing a graphene material; s20, preparing negative electrode slurry; s30, preparing positive electrode slurry; s40, coating slurry; and S50, assembling the battery. The invention provides a preparation method of a high-quality graphene battery, wherein graphene is a hexagonal honeycomb structure formed by hybridizing carbon atoms based on sp2, is a two-dimensional crystal with the thickness of only one atomic layer, and has excellent performances in the aspects of electricity, optics, thermal mechanics and the like. The lithium titanate battery cathode has poor conductivity, but the graphene and lithium titanate composite material can effectively improve the active substance ratio of the battery material, and more importantly, the rate performance can be improved while the cycle performance can be improved.
Description
Technical Field
The invention relates to the technical field of battery manufacturing, in particular to a preparation method of a high-quality graphene battery.
Background
A lithium ion battery is a type of secondary battery that mainly operates by movement of lithium ions between a positive electrode and a negative electrode. During charging, lithium ions are extracted from the positive electrode and are inserted into the negative electrode through the electrolyte, and the negative electrode is in a lithium-rich state; the opposite is true during discharge. The lithium ion battery has the obvious advantages of high energy density, high output voltage, long cycle life, small environmental pollution and the like, is widely applied to small digital electronic products, and has wide application prospect in the fields of hybrid electric vehicles, aerospace, diving and the like. Graphene is a hexagonal honeycomb structure formed by hybridizing carbon atoms based on sp2, is a two-dimensional crystal with the thickness of only one atomic layer, and has excellent performances in the aspects of electricity, optics, thermal mechanics and the like.
However, the rate performance and cycle performance of the current graphene battery in charge and discharge are still not completely satisfactory, so how to improve the rate performance and cycle performance is a difficult problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a high-quality graphene battery to solve the problems.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-quality graphene battery comprises the following steps:
s10, preparing a graphene material: processing a graphite raw material step by step to obtain graphene powder;
s20, preparing anode slurry: compounding the graphene powder obtained in the step S10 with a lithium titanate negative electrode material by a sol-gel method, adding the prepared graphene powder into a conductive agent, and homogenizing by combining a binder to obtain negative electrode slurry;
s30, preparing positive electrode slurry: homogenizing a lithium manganate positive electrode material, a binder and a conductive agent to obtain positive electrode slurry;
s40, slurry coating: coating the negative electrode slurry prepared in the step S20 on a negative electrode sheet, and coating the positive electrode slurry prepared in the step S30 on a positive electrode sheet;
s50, assembling the battery: and (4) rolling and shearing the negative pole piece and the positive pole piece prepared in the step (S40), and assembling the negative pole piece and the positive pole piece into a battery frame.
As a modification of the present invention, in step S10, the graphene material preparation includes the following steps:
s11, pretreatment of graphite raw materials: stirring and mixing a graphite raw material and an organic solvent, filtering, and carrying out high-temperature treatment on a graphite filter cake obtained by filtering under the protection of inert gas;
s12, graphite oxidation treatment: adding the graphite raw material pretreated in the step S11 and an auxiliary oxidant into an alkali solution, placing the mixture into a closed space, introducing oxidation into the closed space to a certain pressure for reaction, and performing solid-liquid separation after the reaction is finished to obtain a solid phase, namely graphene oxide;
s13, reducing graphene oxide: preparing the graphene oxide prepared in the step S12 into a graphene oxide aqueous solution, adjusting the pH, and carrying out reduction reaction on the graphene oxide aqueous solution under the irradiation of ultraviolet light;
s14, post-processing: and (4) filtering and drying the aqueous solution obtained after the reduction in the step S13 to obtain graphene powder.
As an improvement of the present invention, in step S40, when the positive electrode tab and the negative electrode tab are subjected to slurry coating, empty foils are left on both the upper and lower sides of the positive electrode tab and the negative electrode tab.
As an improvement of the invention, in step S11, adding the graphite raw material and the organic solvent N-dimethylformamide solvent into a high-pressure reaction kettle, heating to 170 ℃, and stirring for 4 hours; and after cooling, taking out the graphite raw material, filtering to obtain a graphite filter cake, and treating the graphite filter cake for 2 hours at the temperature of 500 ℃ under the protection of nitrogen.
In step S12, the graphite raw material pretreated in step S11, KOH and NaNO3 are put into a reaction kettle, deionized water is added, and stirring is performed for 15 min; replacing gas in the reaction kettle with oxygen for 3 times under a sealed state, charging oxygen to 5MPa, raising the temperature to 500 ℃, and stirring for 40H; and cooling, mechanically stirring the reactants for 2 hours, carrying out solid-liquid separation, washing the solid product with 5% diluted hydrochloric acid, washing with deionized water to neutrality, and carrying out vacuum drying at 100 ℃ to obtain the graphene oxide solid.
In step S13, the graphene oxide treated in step S12 is prepared as an aqueous solution, the PH of the aqueous solution of graphene oxide is adjusted to 3 with HCL, and the aqueous solution of graphene is placed in an ultraviolet light device for reduction by irradiation for 40 hours.
In step S20, compounding graphene and a lithium titanate negative electrode material by preparing a titanium source dispersion solution from tetrabutyl titanate, graphene, P123, and tert-butyl alcohol, preparing a lithium source solution from lithium acetate dihydrate, deionized water, and tert-butyl alcohol, transferring the mixed titanium source dispersion solution to a microwave reactor, heating to reflux, adding the lithium source solution to react, cooling, removing the solvent, drying to obtain a graphene-based lithium titanate precursor, placing the obtained precursor in a tubular furnace, and calcining under the protection of N2 to obtain the graphene-lithium titanate composite material, wherein the graphene-lithium titanate composite material is the negative electrode slurry.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
A preparation method of a high-quality graphene battery comprises the following steps:
s10, preparing a graphene material: processing a graphite raw material step by step to obtain graphene powder;
s20, preparing anode slurry: compounding the graphene powder obtained in the step S10 with a lithium titanate negative electrode material by a sol-gel method, adding the prepared graphene powder into a conductive agent, and homogenizing by combining a binder to obtain negative electrode slurry;
s30, preparing positive electrode slurry: homogenizing a lithium manganate positive electrode material, a binder and a conductive agent to obtain positive electrode slurry;
s40, slurry coating: coating the negative electrode slurry prepared in the step S20 on a negative electrode sheet, and coating the positive electrode slurry prepared in the step S30 on a positive electrode sheet;
s50, assembling the battery: and (4) rolling and shearing the negative pole piece and the positive pole piece prepared in the step (S40), and assembling the negative pole piece and the positive pole piece into a battery frame.
As an embodiment of the present invention, in step S10, the graphene material preparation includes the following steps:
s11, pretreatment of graphite raw materials: stirring and mixing a graphite raw material and an organic solvent, filtering, and carrying out high-temperature treatment on a graphite filter cake obtained by filtering under the protection of inert gas;
s12, graphite oxidation treatment: adding the graphite raw material pretreated in the step S11 and an auxiliary oxidant into an alkali solution, placing the mixture into a closed space, introducing oxidation into the closed space to a certain pressure for reaction, and performing solid-liquid separation after the reaction is finished to obtain a solid phase, namely graphene oxide;
s13, reducing graphene oxide: preparing the graphene oxide prepared in the step S12 into a graphene oxide aqueous solution, adjusting the pH, and carrying out reduction reaction on the graphene oxide aqueous solution under the irradiation of ultraviolet light;
s14, post-processing: and (4) filtering and drying the aqueous solution obtained after the reduction in the step S13 to obtain graphene powder.
In step S40, when the positive electrode tab and the negative electrode tab are coated with the slurry, empty foils are left on both the upper and lower sides of the positive electrode tab and the negative electrode tab.
As an embodiment of the present invention, in step S11, adding the graphite raw material and the organic solvent N-dimethylformamide solvent into a high pressure reaction kettle, raising the temperature to 170 ℃, and stirring for 4 hours; and after cooling, taking out the graphite raw material, filtering to obtain a graphite filter cake, and treating the graphite filter cake for 2 hours at the temperature of 500 ℃ under the protection of nitrogen.
As an embodiment of the present invention, in step S12, the graphite raw material pretreated in step S11, KOH and NaNO3 are placed in a reaction kettle, deionized water is added, and stirring is performed for 15 min; replacing gas in the reaction kettle with oxygen for 3 times under a sealed state, charging oxygen to 5MPa, raising the temperature to 500 ℃, and stirring for 40H; and cooling, mechanically stirring the reactants for 2 hours, carrying out solid-liquid separation, washing the solid product with 5% diluted hydrochloric acid, washing with deionized water to neutrality, and carrying out vacuum drying at 100 ℃ to obtain the graphene oxide solid.
In step S13, the graphene oxide treated in step S12 is prepared as an aqueous solution, the PH of the aqueous solution of graphene oxide is adjusted to 3 with HCL, and the aqueous solution of graphene is placed in an ultraviolet light device for reduction by irradiation for 40 hours.
As an embodiment of the present invention, in step S20, graphene and lithium titanate negative electrode material are compounded, where tetrabutyl titanate, graphene, P123, and tert-butyl alcohol are prepared into a titanium source dispersion solution, lithium acetate dihydrate, deionized water, and tert-butyl alcohol are prepared into a lithium source solution, the mixed titanium source dispersion solution is transferred to a microwave reactor and heated to reflux, a lithium source solution is added to react and cool, a solvent is removed and dried to obtain a graphene-based lithium titanate precursor, the obtained precursor is placed in a tubular furnace and calcined under the protection of N2 to obtain a graphene-lithium titanate composite material, and the graphene-lithium titanate composite material is negative electrode slurry.
The working principle and the beneficial effects of the technical scheme are as follows:
the specific implementation operation is as follows:
weighing 0.5g of 500-mesh graphite, weighing 10ml of N, N-dimethylformamide solvent, adding into a high-pressure reaction kettle, heating to 170 ℃, and stirring for 4H. After cooling, the graphite filter cake is taken out for filtration, and the graphite filter cake is treated for 2H at 500 ℃ under the protection of N2. 0.3g of pretreated graphite, 4Gkoh and 0.3g of NaNO3 are weighed and placed in a reaction kettle, 30ml of deionized water is added, and stirring is carried out for 15 mins. Sealing, replacing gas in the reaction kettle with oxygen for 3 times, introducing oxygen to 5MPa, heating to 500 deg.C, and stirring for 40H. And cooling, mechanically stirring the reactants for 2 hours, carrying out solid-liquid separation, washing the solid product with 5% diluted hydrochloric acid, washing with deionized water to neutrality, and carrying out vacuum drying at 100 ℃ to obtain the graphene oxide solid. Weighing 0.1g of graphene oxide to prepare an aqueous solution, adjusting the pH value of the aqueous solution of graphene oxide to 3 by using HCL, measuring 3ML of the aqueous solution of graphene into a 5ML small glass bottle, horizontally placing the small glass bottle into an ultraviolet analyzer, adjusting the wavelength to 245nm and carrying out irradiation reduction for 40 hours at a position 5cm away from a fluorescent lamp. And finally, filtering the graphene aqueous solution reduced by the reaction, and drying in vacuum to obtain high-quality graphene powder.
Preparing a graphene battery: performing a homogenate procedure of slurry required by coating a battery positive pole piece through a lithium manganate positive pole, a binder and a conductive agent, and preparing coating preparation after preparing the slurry; then compounding the prepared graphene and a lithium titanate negative electrode material, adding the graphene into a conductive agent, and combining a binder to perform a slurry homogenizing process of coating slurry required by a battery negative electrode plate, wherein the prepared slurry is prepared for coating; compounding graphene and a lithium titanate negative electrode material, namely preparing titanium source dispersion liquid from tetrabutyl titanate, graphene, P123 and tert-butyl alcohol, preparing lithium source solution from lithium acetate dihydrate, deionized water and tert-butyl alcohol, transferring the mixed titanium source dispersion liquid into a microwave reactor, heating to reflux, adding the lithium source solution, reacting for a certain time, cooling, removing a solvent, and drying to obtain a graphene-based lithium titanate precursor. Placing the obtained precursor in a tubular furnace, and calcining under the protection of N2 to obtain the graphene/lithium titanate composite material; and performing positive and negative electrode coating procedures on the prepared slurry, reserving empty foils on two sides of the pole piece, performing rolling and shearing procedures on the pole piece, and finally assembling to obtain the graphene battery.
The invention provides a preparation method of a high-quality graphene battery, wherein graphene is a hexagonal honeycomb structure formed by hybridizing carbon atoms based on sp2, is a two-dimensional crystal with the thickness of only one atomic layer, and has excellent performances in the aspects of electricity, optics, thermal mechanics and the like. The lithium titanate battery cathode has poor conductivity, but the graphene and lithium titanate composite material can effectively improve the active substance ratio of the battery material, and more importantly, the rate performance can be improved while the cycle performance can be improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of a high-quality graphene battery is characterized by comprising the following steps:
s10, preparing a graphene material: processing a graphite raw material step by step to obtain graphene powder;
s20, preparing anode slurry: compounding the graphene powder obtained in the step S10 with a lithium titanate negative electrode material by a sol-gel method, adding the prepared graphene powder into a conductive agent, and homogenizing by combining a binder to obtain negative electrode slurry;
s30, preparing positive electrode slurry: homogenizing a lithium manganate positive electrode material, a binder and a conductive agent to obtain positive electrode slurry;
s40, slurry coating: coating the negative electrode slurry prepared in the step S20 on a negative electrode sheet, and coating the positive electrode slurry prepared in the step S30 on a positive electrode sheet;
s50, assembling the battery: and (4) rolling and shearing the negative pole piece and the positive pole piece prepared in the step (S40), and assembling the negative pole piece and the positive pole piece into a battery frame.
2. The method for preparing a high-quality graphene battery according to claim 1, wherein the method comprises the following steps: in step S10, the graphene material preparation includes the following steps:
s11, pretreatment of graphite raw materials: stirring and mixing a graphite raw material and an organic solvent, filtering, and carrying out high-temperature treatment on a graphite filter cake obtained by filtering under the protection of inert gas;
s12, graphite oxidation treatment: adding the graphite raw material pretreated in the step S11 and an auxiliary oxidant into an alkali solution, placing the mixture into a closed space, introducing oxidation into the closed space to a certain pressure for reaction, and performing solid-liquid separation after the reaction is finished to obtain a solid phase, namely graphene oxide;
s13, reducing graphene oxide: preparing the graphene oxide prepared in the step S12 into a graphene oxide aqueous solution, adjusting the pH, and carrying out reduction reaction on the graphene oxide aqueous solution under the irradiation of ultraviolet light;
s14, post-processing: and (4) filtering and drying the aqueous solution obtained after the reduction in the step S13 to obtain graphene powder.
3. The method for preparing a high-quality graphene battery according to claim 1, wherein the method comprises the following steps: in step S40, when the positive electrode tab and the negative electrode tab are coated with the slurry, empty foils are left on both the upper and lower sides of the positive electrode tab and the negative electrode tab.
4. The method for preparing a high-quality graphene battery according to claim 2, wherein the method comprises the following steps: in step S11, adding a graphite raw material and an organic solvent N-dimethylformamide solvent into a high-pressure reaction kettle, heating to 170 ℃, and stirring for 4 hours; and after cooling, taking out the graphite raw material, filtering to obtain a graphite filter cake, and treating the graphite filter cake for 2 hours at the temperature of 500 ℃ under the protection of nitrogen.
5. The method for preparing a high-quality graphene battery according to claim 2, wherein the method comprises the following steps: in step S12, the graphite raw material pretreated in step S11, KOH and NaNO3 are placed in a reaction kettle, deionized water is added, and stirring is performed for 15 min; replacing gas in the reaction kettle with oxygen for 3 times under a sealed state, charging oxygen to 5MPa, raising the temperature to 500 ℃, and stirring for 40H; and cooling, mechanically stirring the reactants for 2 hours, carrying out solid-liquid separation, washing the solid product with 5% diluted hydrochloric acid, washing with deionized water to neutrality, and carrying out vacuum drying at 100 ℃ to obtain the graphene oxide solid.
6. The method for preparing a high-quality graphene battery according to claim 2, wherein the method comprises the following steps: in step S13, the graphene oxide treated in step S12 is prepared as an aqueous solution, the PH of the aqueous solution of graphene oxide is adjusted to 3 with HCL, and the aqueous solution of graphene is placed in an ultraviolet light device for reduction by irradiation for 40 hours.
7. The method for preparing a high-quality graphene battery according to claim 2, wherein the method comprises the following steps: in step S20, compounding graphene and a lithium titanate negative electrode material by preparing a titanium source dispersion solution from tetrabutyl titanate, graphene, P123, and tert-butyl alcohol, preparing a lithium source solution from lithium acetate dihydrate, deionized water, and tert-butyl alcohol, transferring the mixed titanium source dispersion solution to a microwave reactor, heating to reflux, adding the lithium source solution to react, cooling, removing the solvent, drying to obtain a graphene-based lithium titanate precursor, placing the obtained precursor in a tubular furnace, and calcining under the protection of N2 to obtain the graphene-lithium titanate composite material, wherein the graphene-lithium titanate composite material is a negative electrode slurry.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451925A (en) * | 2014-11-21 | 2015-03-25 | 东华大学 | Water-soluble polymer/graphene composite fiber as well as preparation method and application thereof |
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| CN104451925A (en) * | 2014-11-21 | 2015-03-25 | 东华大学 | Water-soluble polymer/graphene composite fiber as well as preparation method and application thereof |
| CN105347340A (en) * | 2015-12-14 | 2016-02-24 | 太原理工大学 | Preparation method of graphene oxide |
| CN105703012A (en) * | 2016-01-25 | 2016-06-22 | 张博 | Preparation method of graphene quick rechargeable battery |
| CN105977469A (en) * | 2016-07-01 | 2016-09-28 | 天津普兰能源科技有限公司 | High-performance lithium titanate battery |
| CN111584866A (en) * | 2020-05-27 | 2020-08-25 | 安徽科达新材料有限公司 | Preparation method of high-rate artificial graphite negative electrode material |
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