CN112615004A - Cellulose @ graphene composite carbon aerogel and preparation method and application thereof - Google Patents
Cellulose @ graphene composite carbon aerogel and preparation method and application thereof Download PDFInfo
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- CN112615004A CN112615004A CN202011492805.4A CN202011492805A CN112615004A CN 112615004 A CN112615004 A CN 112615004A CN 202011492805 A CN202011492805 A CN 202011492805A CN 112615004 A CN112615004 A CN 112615004A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/626—Metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a cellulose @ graphene composite carbon aerogel and a preparation method and application thereof, wherein cotton cellulose is added into a sodium hydroxide solution; placing the mixed solution at a low temperature, mixing the mixed solution with the graphene oxide solution at a low temperature, and stirring to obtain a cellulose @ graphene oxide mixed solution; pouring the mixed solution of the cellulose and the graphene oxide into a mold, and standing at room temperature to obtain cellulose and graphene oxide hydrogel; freezing and drying the cellulose @ graphene oxide hydrogel to obtain cellulose @ graphene oxide aerogel; and carrying out high-temperature pyrolysis on the cellulose @ graphene oxide aerogel to obtain the cellulose @ graphene composite carbon aerogel. The cellulose @ graphene composite carbon aerogel is used in an electrode structure for inducing the directional growth of lithium dendrites, so that the battery diaphragm is protected.
Description
Technical Field
The invention relates to the field of lithium metal batteries, relates to a strategy for directional growth of lithium dendrites by inducing current distribution, and particularly relates to cellulose @ graphene composite carbon aerogel and a preparation method and application thereof.
Background
The rapid growth in the electric vehicle market has led to a wide research interest in next generation batteries to meet the ever-increasing demands for high power performance, high energy density and long cycle life. Lithium metal is due to its higher theoretical capacity (3860mAh g)-1) Lower electrochemical potential (-3.040V vs standard hydrogen electrode) and 0.534g cm-3And is often selected as the negative electrode material. However, metal lithium electrodes present serious safety concerns. The culprit of these problems appears to be due primarily to uncontrolled growth of lithium dendrites, which can lead to internal short circuits, thermal runaway, etc., leading to serious safety concerns.
In recent years, researchers have made many strategies focused on improving the separator/anode interface to inhibit the growth of lithium dendrites and protect the separator. Such as artificial SEI films, electrolyte additives, lithium/carbon composite electrodes, and the like. However, these strategies still do not change the dendrite upward growth direction of the separator/electrolyte interface, and as cycling proceeds, the battery separator still presents a safety hazard.
Disclosure of Invention
The invention aims to provide a cellulose @ graphene composite carbon aerogel and a preparation method and application thereof, and aims to overcome the defect that lithium dendrites grow upwards at an electrode/electrolyte interface.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of cellulose @ graphene composite carbon aerogel comprises the following steps:
step 1, adding cotton cellulose into a sodium hydroxide solution;
step 2, placing the mixed solution obtained in the step 1 at a low temperature, mixing the mixed solution with a graphene oxide solution at a low temperature, and stirring to obtain a cellulose @ graphene oxide mixed solution;
step 3, pouring the cellulose @ graphene oxide mixed solution obtained in the step 2 into a mold, and standing at room temperature to obtain cellulose @ graphene oxide hydrogel;
step 4, freezing and drying the cellulose @ graphene oxide hydrogel obtained in the step 3 to obtain cellulose @ graphene oxide aerogel;
and 5, performing high-temperature pyrolysis on the cellulose @ graphene oxide aerogel obtained in the step 4 to obtain cellulose @ graphene composite carbon aerogel, namely CCA.
Further, the sodium hydroxide solution in step 1 is specifically: 7.6g of NaOH is added into 32.4mL of water, and the mass ratio of the cotton cellulose to the NaOH in the sodium hydroxide solution in the step 1 is 1: 7.6.
Further, the concentration of the graphene oxide solution in the step 2 is 2mg/mL, and the volume ratio of the mixed solution obtained in the step 1 to the graphene oxide solution is 1: 1.
Further, the temperature of the low-temperature placement in the step 2 is-15 ℃, and the time is 12 h.
Further, the standing time in step 3 was 48 hours.
Further, the high-temperature pyrolysis in the step 5 specifically comprises: heating to 800 ℃ at the heating rate of 2 ℃/min under the Ar atmosphere, and pyrolyzing for 2 h.
The cellulose @ graphene composite carbon aerogel is prepared by the preparation method of the cellulose @ graphene composite carbon aerogel.
The application of the cellulose @ graphene composite carbon aerogel in an electrode structure for inducing the directional growth of lithium dendrites is characterized in that the cellulose @ graphene composite carbon aerogel is placed between a lithium metal negative electrode and a current collector to obtain a CCA-Li composite electrode.
The application of the cellulose @ graphene composite carbon aerogel in an electrode structure for inducing the directional growth of lithium dendrites is characterized in that the cellulose @ graphene composite carbon aerogel is used as an interlayer and is placed between a battery diaphragm and a lithium metal negative electrode to obtain a Li-CCA electrode.
The application of cellulose @ graphene composite carbon aerogel in an electrode structure for inducing directional growth of lithium dendrites is characterized in that the cellulose @ graphene composite carbon aerogel is soaked in 40mg/mL zinc acetate aqueous solution and then soaked in N2Under atmosphere, 600Obtaining CCA @ ZnO composite material by pyrolysis, heating metal lithium to 350 ℃, melting and pouring the metal lithium into the CCA @ ZnO composite material to obtain a CCA @ Li composite electrode, wherein the content of lithium metal is 50mg/cm-2。
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation material has low cost and abundant reserves, is simple to operate and easy to realize when used for protecting lithium metal, has obvious effect, and can greatly improve the long-cycle stability of the lithium metal battery.
The invention relates to a new strategy for protecting a lithium metal negative electrode, which induces the distribution of current density by changing the structure of a CCA/Li composite electrode, thereby changing the deposition place of lithium dendrite and achieving the purpose of protecting a battery diaphragm. The strategy may be at 10mA cm-2The cycle life is as long as 1000 times under the high current density.
Furthermore, the cellulose @ graphene Composite Carbon Aerogel (CCA) is placed between the lithium metal negative electrode and the current collector, so that the CCA layer at the bottom bears high current density, and a main deposition site is induced to migrate from an electrode/electrolyte interface to the electrode/current collector interface, so that the battery diaphragm is protected.
Furthermore, the CCA is placed between the battery diaphragm and the lithium metal cathode to obtain the Li-CCA electrode, so that local high current distribution on the surface of the lithium metal can be effectively reduced, the lithium metal is uniformly deposited on the surface of the lithium metal, and the cycle life of the battery is prolonged.
Further, the method comprises the steps of soaking the cellulose @ graphene composite carbon aerogel in a zinc acetate aqueous solution and adding the zinc acetate aqueous solution into N2In the atmosphere, the CCA @ ZnO composite material is obtained through pyrolysis, and the CCA @ ZnO composite material is filled with the molten metal lithium to obtain the CCA @ Li composite electrode, so that a continuous conductive network and a plurality of nucleation sites are provided, and the cycle life of the electrode is prolonged.
Drawings
Fig. 1 is an SEM image of a CCA prepared by an embodiment of the present invention;
FIG. 2 is a TEM image of a CCA prepared by an embodiment of the present invention;
fig. 3 is a graph of battery performance data obtained for application examples of the present invention and comparative examples.
Detailed Description
The present invention will be described in more detail with reference to examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
In the present invention, all the devices and materials are commercially available or commonly used in the industry, if not specifically mentioned. The methods in the following examples are conventional in the art unless otherwise specified.
Examples
The first step is as follows: preparation of Cotton cellulose/NaOH/H2O (1.0g/7.6g/32.4ml) mixed solution; standing at-15 deg.C for 12 h;
the second step is that: placing the mixed solution at a low temperature of-15 ℃ for 12 hours, then mixing the mixed solution with a graphene oxide solution (2mg/ml) at a low temperature, and violently and mechanically stirring to obtain a cellulose @ graphene oxide mixed solution;
the third step: pouring the mixed solution of the cellulose @ graphene oxide into a mold, and standing for 48 hours at room temperature to obtain cellulose @ graphene oxide hydrogel;
the fourth step: the cellulose @ graphene oxide hydrogel is subjected to freeze drying to obtain cellulose @ graphene oxide aerogel;
the fifth step: and heating the cellulose @ graphene oxide aerogel to 800 ℃ at a heating rate of 2 ℃/min in an Ar atmosphere, and pyrolyzing for 2h to obtain the cellulose @ graphene Composite Carbon Aerogel (CCA).
Application example 1
The CCA prepared in example was placed between a lithium metal negative electrode and a current collector to obtain a CCA-Li composite electrode. This strategy allows the bottom CCA layer to carry high current densities, allowing the main site of lithium metal deposition to migrate from the diaphragm/electrode interface to the bottom CCA layer, thus ensuring long cycling stability of the diaphragm to protect the battery diaphragm.
Application example 2
The CCA obtained in the example was placed between a battery separator and a lithium metal negative electrode as an interlayer to obtain a Li-CCA electrode. The strategy can effectively reduce local high current distribution on the surface of the lithium metal, so that the lithium metal is uniformly deposited on the surface of the lithium metal, and the cycle life of the battery is prolonged.
Application example 3
The CCA obtained in example was immersed in an aqueous zinc acetate solution (40mg/ml) and dissolved in N2And carrying out pyrolysis at 600 ℃ in the atmosphere to obtain the CCA @ ZnO composite material. Heating metal lithium to 350 ℃, melting and pouring the metal lithium into the CCA @ ZnO composite material to obtain the CCA @ Li composite electrode, wherein the content of lithium metal is 50mg/cm-2. This strategy provides a continuous conductive network and multiple nucleation sites, increasing the cycle life of the electrode.
Comparative example
A metallic lithium electrode was used as a comparative sample.
TEM and SEM analysis, as shown in fig. 1 and 2, indicate that the three-dimensional porosity of CCA is a result of the double structure of the carbon network, in which two-dimensional graphene sheets are closely attached to the surface of one-dimensional nanofibers. FIG. 3 shows the results of overpotential testing for four different examples of applications. Application example 1: the CCA is placed between the lithium metal anode and the current collector. Application example 2: placing a diaphragm and metal lithium by taking CCA as an intermediate layer; application example 3: melting and pouring lithium metal into the CCA @ ZnO composite material; comparative example: two lithium metal symmetrical batteries without CCA; as can be seen from fig. 3, application example 1 shows the most stable cycle performance and the lowest hysteresis voltage. At 10mA cm-2At a high current density of (2), the overpotential of application example 1 was about 118mV, a higher level, after 1000 cycles. The cycle life of the comparative and application example 2 cells were less than 223 and 530 times, respectively. The structure of application example 3 is slightly better than that of the comparative example and application example 2, and the overpotential after 578 cycles is as high as 617 mV.
Claims (10)
1. A preparation method of cellulose @ graphene composite carbon aerogel is characterized by comprising the following steps:
step 1, adding cotton cellulose into a sodium hydroxide solution;
step 2, placing the mixed solution obtained in the step 1 at a low temperature, mixing the mixed solution with a graphene oxide solution at a low temperature, and stirring to obtain a cellulose @ graphene oxide mixed solution;
step 3, pouring the cellulose @ graphene oxide mixed solution obtained in the step 2 into a mold, and standing at room temperature to obtain cellulose @ graphene oxide hydrogel;
step 4, freezing and drying the cellulose @ graphene oxide hydrogel obtained in the step 3 to obtain cellulose @ graphene oxide aerogel;
and 5, performing high-temperature pyrolysis on the cellulose @ graphene oxide aerogel obtained in the step 4 to obtain cellulose @ graphene composite carbon aerogel, namely CCA.
2. The preparation method of cellulose @ graphene composite carbon aerogel according to claim 1, wherein the sodium hydroxide solution in the step 1 is specifically: 7.6g of NaOH is added into 32.4mL of water, and the mass ratio of the cotton cellulose to the NaOH in the sodium hydroxide solution in the step 1 is 1: 7.6.
3. The preparation method of cellulose @ graphene composite carbon aerogel according to claim 1, wherein the concentration of the graphene oxide solution in the step 2 is 2mg/mL, and the volume ratio of the mixed solution obtained in the step 1 to the graphene oxide solution is 1: 1.
4. The preparation method of cellulose @ graphene composite carbon aerogel according to claim 1, wherein the temperature for low-temperature placement in step 2 is-15 ℃ and the time is 12 hours.
5. The preparation method of cellulose @ graphene composite carbon aerogel according to claim 1, wherein the standing time in the step 3 is 48 hours.
6. The preparation method of cellulose @ graphene composite carbon aerogel according to claim 1, wherein the high-temperature pyrolysis in the step 5 specifically comprises: heating to 800 ℃ at the heating rate of 2 ℃/min under the Ar atmosphere, and pyrolyzing for 2 h.
7. The cellulose @ graphene composite carbon aerogel is characterized by being prepared by the preparation method of the cellulose @ graphene composite carbon aerogel as claimed in any one of claims 1 to 6.
8. The application of the cellulose @ graphene composite carbon aerogel in an electrode structure for inducing the directional growth of lithium dendrites according to claim 7 is characterized in that the cellulose @ graphene composite carbon aerogel is placed between a lithium metal negative electrode and a current collector to obtain the CCA-Li composite electrode.
9. The application of the cellulose @ graphene composite carbon aerogel in an electrode structure for inducing the directional growth of lithium dendrites according to claim 7 is characterized in that the cellulose @ graphene composite carbon aerogel is arranged between a battery diaphragm and a lithium metal negative electrode as an interlayer to obtain a Li-CCA electrode.
10. The use of the cellulose @ graphene composite carbon aerogel of claim 7 in an electrode structure for inducing directional growth of lithium dendrites, wherein the cellulose @ graphene composite carbon aerogel is soaked in 40mg/mL zinc acetate aqueous solution and subjected to N2Obtaining CCA @ ZnO composite material by pyrolysis at 600 ℃ in atmosphere, heating metal lithium to 350 ℃, melting and pouring the metal lithium into the CCA @ ZnO composite material to obtain a CCA @ Li composite electrode, wherein the content of lithium metal is 50mg/cm-2。
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| CN113471531A (en) * | 2021-07-28 | 2021-10-01 | 恒大新能源技术(深圳)有限公司 | Polymer solid electrolyte, preparation method thereof and solid battery |
| CN113921762A (en) * | 2021-09-13 | 2022-01-11 | 苏州科技大学 | Nano bismuth composite material and preparation method and application thereof |
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