CN110752376B - Preparation method and application of in-situ formed metal-amalgam active current collector - Google Patents

Preparation method and application of in-situ formed metal-amalgam active current collector Download PDF

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CN110752376B
CN110752376B CN201911064051.XA CN201911064051A CN110752376B CN 110752376 B CN110752376 B CN 110752376B CN 201911064051 A CN201911064051 A CN 201911064051A CN 110752376 B CN110752376 B CN 110752376B
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amalgam
current collector
situ
tin
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CN110752376A (en
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何广
丁轶
张琪
乌兰
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Tianjin University of Technology
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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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • H01M4/662—Alloys
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/665—Composites
    • H01M4/667—Composites in the form of layers, e.g. coatings
    • 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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Abstract

The invention provides a preparation method of a metal-amalgam active current collector formed in situ, which comprises the steps of uniformly coating liquid metal mercury on the surface of a metal material, standing for 1-24 hours, drying to obtain a metal cathode material with amalgam generated in situ on the surface, and applying the metal cathode material to a metal ion battery; wherein, the metal material is metal zinc and tin elements or the alloy thereof. According to the invention, the liquid metal mercury is directly coated on the surface of the metal material or the alloy of the metal material without additional electrochemical treatment, so that the integrated cathode/current collector with the in-situ amalgam on the surface can be obtained, the used mercury is liquid metal without additional treatment, the cost is low, the method is practical and effective, and meanwhile, the cathode material with the alloy structure with the concentration gradient is obtained and is applied to the corresponding metal ion battery, so that the metal ions can be reversibly de-intercalated, and the coulomb efficiency, the cycle life and the safety of the battery are improved.

Description

Preparation method and application of in-situ formed metal-amalgam active current collector
Technical Field
The invention belongs to the technical field of chemical power supplies, and particularly relates to a preparation method and application of a metal-amalgam active current collector formed in situ.
Background
Energy and environmental problems are the basis of human sustainable development, along with the rapid development of modern science and technology, the human demand for energy is increasing day by day, especially the development of clean and efficient green energy storage devices is receiving wide attention, for example, new cathode materials of high specific energy lithium ion and sodium ion batteries become research hotspots in the field of current secondary batteries. At present, the theoretical capacity of the commercial graphite cathode is only 372mAh g-1The theoretical capacity of the hard carbon of the cathode material of the sodium ion battery is lower and is only 300mAh g-1And they are all lithium-free negative electrodes, cannot matchA novel sulfur anode and an air anode are prepared. The alloy negative pole such as zinc base/tin base material has higher theoretical specific capacity (LiZn: 412mAh g)-1，Li4.4Sn：994mAh g-1) And the reserves are abundant, the low price. However, the metal-based negative electrode can generate large volume expansion in the charging and discharging processes, and the material is easy to break and pulverize, so that the high specific surface area and the 3D nano-skeleton structure are usually designed to relieve the volume expansion and improve the cycling stability of the negative electrode, but the preparation of the electrodes is often complicated and difficult to popularize on a large scale. In addition, the adhesion of the nanostructured negative electrode to the copper current collector is weaker than that of the graphite negative electrode. The current coating process is difficult to realize the efficient and stable attachment of the high-capacity metal-based material and the current collector, and the volume change of the negative electrode in the circulation process easily causes the electrode to fall off from the current collector, so that the battery fails.
The tin-based/zinc-based active current collector is a good electronic conductor, and has the advantages of good ductility, easy machining and the like. Ideally, the porous carbon material can be used as an active electrode material, can be used as a current collector by utilizing the high electron conduction characteristics of the porous carbon material, and does not have the problems of electrode falling off from the current collector and the like. However, practical tests find that the concentration change (or can be understood as the change of alloy components) of lithium/sodium plasma in these current collectors has a great influence on the dynamic behavior of intercalation and deintercalation of the lithium/sodium plasma, so that the utilization rate of active materials is extremely low, and the intercalated metal ions can not be reversibly deintercalated to rapidly reduce the coulombic efficiency, and the requirement on the cycle performance of the full cell can not be met. On the other hand, the alkali metal ions are enriched on the surface of the electrode/current collector to cause the problems of dendritic crystals and the like, thereby bringing about potential safety hazards.
Researchers have studied the above problems and proposed different solutions. Arumugam Manthiram et al (Joule 2019,3,1051-1063) adopt a melting method to prepare Zn-Sn alloy, and prepare alloy foil with a nano structure by a cold rolling technology, so that the reversible de-intercalation performance of lithium ions is improved. CN106058301A discloses that the porous foam tin-based current collector is used as the negative electrode of a lithium ion battery, which alleviates the problem of volume expansion of the negative electrode material of the lithium ion battery and improves the cycle performance of the battery. These methods can improve the electrochemical performance of the integrated current collector, but are limited by the substrate material or the complex preparation/modification process, the actual capacity of the electrode is very low, and it is difficult to apply in large scale in batteries.
Therefore, aiming at the found problems, a simple and efficient preparation technology is developed to enable alkali metal ions to be stably and reversibly deintercalated, and the method is very critical to engineering abnormity of active current collector materials such as zinc base/tin base and the like.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method and application of an in-situ formed metal-amalgam active current collector, which has the advantages of simple process, low cost, practicality and effectiveness, and the prepared alloy negative electrode material has excellent cycle performance, thereby providing a new idea for the design and application of an integrated active current collector.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a metal-amalgam active current collector formed in situ comprises the steps of uniformly coating liquid metal mercury on the surface of a metal material, standing for 1-24 hours, drying to obtain a metal negative electrode material with amalgam generated in situ on the surface, and applying the metal negative electrode material to a metal ion battery; wherein, the metal material is metal zinc and tin elements or the alloy thereof.
Further, the relation between the amount of the liquid metal mercury coated and the surface area of the metal material is 0 to 1.75 μ L cm-2。
Further, the thickness of the metal material is 30 μm to 1 mm.
Further, the thickness of the metal-amalgam is 30 μm-1 mm.
Further, the environment was an argon filled glove box with oxygen content values below 1 ppm.
Further, the drying temperature is 22-50 ℃.
The invention also provides an application of the in-situ formed metal-amalgam active current collector, which is used as an integrated negative electrode and a current collector of a lithium, sodium and potassium metal battery.
According to the method, liquid metal mercury is directly coated on the surface of a metal material through a simple and low-cost coating method, the liquid metal mercury can slowly permeate into a zinc/tin bulk phase to form an alloy structure with a concentration gradient, the alloy structure is favorable for rapid migration of ions, and lithium/sodium/potassium ions can be reversibly de-intercalated, so that the coulombic efficiency of a battery is improved, and the cycle life of the battery is prolonged.
Compared with the prior art, the preparation method and the application of the in-situ formed metal-amalgam active current collector have the following advantages:
according to the invention, the liquid metal mercury is directly coated on the surface of the metal material or the alloy of the metal material without additional electrochemical treatment, so that the integrated cathode/current collector with the in-situ amalgam on the surface can be obtained, the used mercury is liquid metal without additional treatment, the cost is low, the method is practical and effective, and meanwhile, the cathode material with the alloy structure with the concentration gradient is obtained and is applied to the corresponding metal ion battery, so that the metal ions can be reversibly de-intercalated, and the coulomb efficiency, the cycle life and the safety of the battery are improved.
Drawings
FIG. 1 is a scanning electron micrograph of the surface of a zinc-amalgam electrode synthesized in situ according to example 1;
fig. 2 is a cycle performance curve of 50 cycles of the battery assembled by the metal zinc-amalgam and the lithium iron phosphate obtained in example 1;
fig. 3 is a charge-discharge curve of the battery assembled by the metal zinc-amalgam and the lithium iron phosphate obtained in example 1;
fig. 4 is a cycle performance curve of 400 cycles of the battery assembled by the metallic tin-amalgam and the lithium iron phosphate obtained in example 2;
fig. 5 is a charge-discharge curve of the battery assembled by the metallic tin-amalgam and the lithium iron phosphate obtained in example 2;
fig. 6 is a cycle performance curve for 50 cycles of the metallic tin-amalgam and prussian blue assembled cell obtained in example 3;
FIG. 7 is a charge-discharge curve of a battery assembled by metallic tin-amalgam and Prussian blue obtained in example 3;
fig. 8 is a charge-discharge curve for 4 cycles of a mercury-free zinc foil versus lithium iron phosphate battery of comparative example 1;
fig. 9 is a graph of the cycle performance of 400 cycles of the mercury-free tin foil and lithium iron phosphate assembled battery of comparative example 2;
fig. 10 is a charge and discharge curve of the mercury-free tin foil and lithium iron phosphate assembled battery in comparative example 2;
fig. 11 is a cycle performance curve for 50 cycles of the mercury uncoated tin foil and prussian blue assembled cell of comparative example 3;
fig. 12 is a charge and discharge curve of the mercury-free tin foil and prussian blue assembled battery in comparative example 3.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1:
1) coating 5 μ L of liquid metal mercury on an area of 10cm2The electrode slice with an alloy structure is formed on the simple substance zinc foil in situ, the standing time in a glove box filled with argon is 24 hours, and the drying temperature is 25 ℃, so that the protected metal-amalgam cathode material is obtained.
2) The in-situ protected metal zinc foil is applied to a lithium iron phosphate battery.
Wherein, the anode material is lithium iron phosphate (LiFePO)470 percent by mass), conductive agent carbon black (super P, 20 percent by mass) and adhesive polytetrafluoroethylene (PVDF, 10 percent by mass), and then coating the mixture on an aluminum foil current collector to be used as a positive pole piece; taking the obtained zinc-amalgam as a negative pole piece; a lithium iron phosphate battery, specifically a CR2032 button cell, is assembled by using 1M LiTFSI (DOL: DME ═ 1: 1) as an electrolyte.
The cycle performance curve for 50 cycles of the cell is shown in figure 2.
FIG. 1 is a scanning electron micrograph of the surface of the in-situ synthesized zinc-amalgam.
Fig. 2 is a cycle performance curve of 50 cycles of a battery assembled by in-situ synthesized zinc-amalgam and lithium iron phosphate. The battery is a CR2032 button cell battery. The abscissa represents the number of cycles in n and the ordinate represents the specific discharge capacity in mAh g-1The second ordinate represents the coulombic efficiency in%. It can be seen that the battery assembled by the in-situ synthesized zinc-amalgam as the negative electrode still has 25.2mAh g of capacity after 50 cycles-1。
Fig. 3 is a charge and discharge curve of the battery. The abscissa is the specific capacity and the ordinate is the voltage in V. The charge and discharge curve has a similar line shape to that of a conventional lithium iron phosphate battery.
Example 2:
1) 5uL of liquid metal mercury is coated on tin foil to form tin-amalgam, and the tin-amalgam is obtained after the tin-amalgam is kept still in a glove box filled with argon for 24 hours and the drying temperature is 25 ℃.
2) The tin-amalgam with in-situ protection is applied to the lithium iron phosphate battery.
Wherein, the anode material is lithium iron phosphate (LiFePO)470 percent by mass), conductive agent carbon black (super P, 20 percent by mass) and adhesive polytetrafluoroethylene (PVDF, 10 percent by mass), and then coating the mixture on an aluminum foil current collector to be used as a positive pole piece; taking the obtained in-situ synthesized tin-amalgam as a negative pole piece; a lithium iron phosphate battery, specifically a CR2032 button cell, is assembled by using 1M LiTFSI (DOL: DME ═ 1: 1) as an electrolyte.
The current density is 170mA g-1At this time, the cell still did not fail after 400 cycles.
The scanning electron microscope pictures of the in situ synthesized tin-amalgam were similar to those of example 1.
Fig. 4 is a charge-discharge curve of a lithium iron phosphate battery assembled with an in-situ protected metallic tin-amalgam negative electrode material. The lithium iron phosphate battery is a CR2025 button battery, and the metal-based amalgam is used as a negative electrode. The abscissa represents the specific capacity in mAh g-1The ordinate represents the voltage in V. It can be seen that at a current density of 170mA g-1In time, the battery can be circulated for more than 400 circles, and still has capacity and storageThe efficiency is stable. Fig. 5 is a corresponding charge-discharge curve of the battery.
Example 3:
1) 5uL of liquid metal mercury is coated on tin foil to form tin-amalgam, and the tin-amalgam is obtained after the tin-amalgam is kept still in a glove box filled with argon for 24 hours and the drying temperature is 25 ℃.
2) The metal-based negative electrode material with in-situ protection is applied to a Prussian blue battery.
Wherein Prussian blue (Na)xFe[Fe(CN)6]70% by mass, 10% by mass of binder Polytetrafluoroethylene (PVDF) and 20% by mass of conductive agent (Super P), and then coating the mixture on an aluminum foil current collector to serve as a positive electrode plate; taking the obtained in-situ protected metal tin-amalgam as a negative pole piece; adding 1M NaClO4(EC: PC ═ 1: 1) as electrolyte, and assembling into Prussian blue batteries, in particular to CR2032 button batteries.
At a current density of 170mA g-1The cycle performance curve of the gold tin-amalgam cathode material protected in situ is shown in figure 6, the cycle performance is excellent, and the metal-based cathode can be effectively protected.
The morphology of the metallic tin-amalgam resulting in-situ protection was similar to that of example 1.
Fig. 6 is a graph of cycling performance and coulombic efficiency for in situ protected tin-amalgam and prussian blue cells. The cell is a CR2032 button cell, and the tin-amalgam with in-situ protection is used as a negative electrode. The abscissa represents the number of cycles in n and the ordinate represents the specific capacity and coulombic efficiency in mAh g-1And%. It can be seen that at a current density of 170mA g-1Then, the specific discharge capacity of the second ring is 99.7mAh g-1The coulombic efficiency is 104.79 percent, and the specific discharge capacity after 50 cycles is 80.1mAh g-1The coulombic efficiency is 102.53%, and the cycle performance is good.
Comparative example 1:
1) the metallic zinc foil was not subjected to the treatment of step 1 of example 1, to obtain an untreated zinc foil.
2) Unprotected zinc foil was applied to lithium iron phosphate batteries.
Cycling performance of the battery as shown in fig. 8, the battery failed after only 4 cycles, although the battery could be cycled in the initial state.
The lithium iron phosphate battery is a CR2032 button cell battery, and the zinc foil is used as a negative electrode. The abscissa represents the number of cycles in n and the ordinate represents the specific discharge capacity in mAh g-1. It can be seen that the capacity of the untreated zinc foil in the first circle is very high, but the charging and discharging platform is much different from that of the traditional lithium iron phosphate battery.
Comparative example 2:
1) the metal tin foil was not subjected to the treatment of step 1 of example 2, to obtain an unprotected metal tin foil.
2) The unprotected metallic tin foil was applied to a lithium iron phosphate battery.
FIGS. 9 and 10 show the current density of lithium iron phosphate and tin foil at 170mA g-1A time cycle curve and a charge-discharge curve.
The lithium iron phosphate battery is a CR2032 button battery, and the metal tin foil is used as a negative electrode. The abscissa represents the specific capacity in mAh g-1The ordinate represents the voltage in V. It can be seen that at a current density of 170mA g-1The specific discharge capacity of the second ring is 29.8mAh g-1Cycling to 400 cycles, the cell had no capacity and was near failure.
Comparative example 3:
1) the metallic tin sheet was not subjected to the treatment of step 1 of example 3, and an unprotected metallic tin foil was obtained.
2) An unprotected metallic tin foil was applied to the prussian blue cell.
The cycle performance curve of the battery at 50 cycles is shown in fig. 11, and the charge-discharge curve is shown in fig. 12.
The Prussian blue battery is a CR2032 button battery, and the metal tin foil is used as a negative electrode. The abscissa represents the number of cycles in n and the ordinate represents the specific capacity in mAh g-1. It can be seen that the second circle of the prussian blue battery assembled by the unprotected metallic tin sheet has a specific discharge capacity of 37.1mAh g-1Coulombic efficiency was 145.7%; when the battery is circulated to the third circle, the battery has no capacity and the circulation performance is poor.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. A method of forming a metal-amalgam active current collector in-situ, comprising: uniformly coating liquid metal mercury on the surface of a metal material, standing for 1-24 hours, drying to obtain a metal cathode material with amalgam generated in situ on the surface, and applying the metal cathode material to a metal ion battery; wherein the metal material is metal zinc or metal tin, or an alloy thereof; the thickness of the metal-amalgam is 30 μm-1 mm.
2. The method of making an in situ forming metal-amalgam active current collector as claimed in claim 1, wherein: the relation between the amount of the coated liquid metal mercury and the surface area of the metal material is more than 0 and less than or equal to 1.75 mu L cm-2。
3. The method of making an in situ forming metal-amalgam active current collector as claimed in claim 1, wherein: the thickness of the metal material is 30 mu m-1 mm.
4. The method of making an in situ forming metal-amalgam active current collector as claimed in claim 1, wherein: the environment was a glove box filled with argon and the oxygen content was below 1 ppm.
5. The method of making an in situ forming metal-amalgam active current collector as claimed in claim 1, wherein: the drying temperature is 22-50 ℃.
6. Use of a metal-amalgam active current collector formed in situ according to the method of any one of claims 1-5, wherein: the lithium, sodium and potassium metal battery is used as an integrated negative electrode and current collector.
7. The method of making an in situ forming metal-amalgam active current collector as claimed in any one of claims 1-5 wherein: 5uL of liquid metal mercury is coated on tin foil to form tin-amalgam, and the tin-amalgam is obtained after the tin-amalgam is kept still in a glove box filled with argon for 24 hours and the drying temperature is 25 ℃.
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