CN112909222B - Lithium metal negative electrode and preparation method and application thereof - Google Patents
Lithium metal negative electrode and preparation method and application thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention provides a preparation method of a lithium metal negative electrode, which comprises the following steps: mixing melamine foam and aniline solution, and standing to obtain a mixed solution; reacting the mixed solution with ammonium persulfate to obtain a reaction product; and rolling and compounding the reaction product and lithium foil to obtain the lithium metal cathode. The in-situ buffer layer material prepared by the method provided by the invention has stronger mechanical modulus, the fiber layer with weak conductivity can disperse the high current density at the tip of the dendritic crystal when the dendritic crystal contacts the fiber, inhibit the growth of the dendritic crystal and homogenize the concentration of lithium ions, and meanwhile, the elastically expandable buffer layer material has larger reserved space, can restrict a large amount of accumulated dead lithium and is suitable for volume expansion. The invention also provides a lithium metal negative electrode and application thereof.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a lithium metal negative electrode and a preparation method and application thereof.
Background
Along with the dependence of people on the use of energy storage equipment, the human life can not leave the benefits brought by the energy storage equipment, and meanwhile, the requirement on the energy density of the energy storage equipment is higher and higher, namely the energy storage equipment is small to small digital equipment and is large to a new energy automobile power battery. Because lithium metal has higher theoretical specific capacity, the lithium metal battery gradually enters the visual field of people in order to improve the energy density of the battery, but the cycle life and reversible capacity of the lithium metal battery can be reduced due to a series of side reactions caused by the growth of lithium dendrites in the lithium metal battery, including the consumption of electrolyte, and the generation of 'dead lithium', even if the growth of dendrites can pierce through a diaphragm to cause the short circuit of the battery, so that the safety problem is caused.
The lithium metal cathode buffer layer is prepared mainly by the following steps: the mode of coating the buffer layer to protect the lithium metal cathode is that firstly, the filler, the cross-linking agent and the like are mixed according to the mass proportion, the mixture is fully stirred to be uniformly mixed, then the mixed solution is coated on the cathode material, and the cathode material is dried in a vacuum oven to obtain the lithium metal cathode; the mode of growing the buffer layer on the cathode material in situ is that the buffer layer solution is generated on the electrode plate in situ after the raw materials are prepared.
The buffer layer is coated to protect the lithium metal negative electrode and the buffer layer material grown in situ on the negative electrode material from having an elastic function, so that the buffer layer material cannot accommodate volume expansion caused by large negative electrode deformation such as accumulation of 'dead lithium' in the long-time circulating process, and further the buffer layer material cannot be continuously contacted with the lithium metal to play a functional role; the buffer layer material coated with the buffer layer and grown in situ is generally non-conductive high polymer, and can promote lithium ion transmission, play a role in enhancing the mechanical strength of the negative electrode by high elastic modulus, but cannot disperse the tip current of the lithium dendrite and inhibit the growth of the dendrite.
Disclosure of Invention
In view of this, the present invention aims to provide a lithium metal negative electrode, a preparation method and an application thereof.
The invention provides a preparation method of a lithium metal negative electrode, which comprises the following steps:
mixing melamine foam and aniline solution, and standing to obtain a mixed solution;
reacting the mixed solution with ammonium persulfate to obtain a reaction product;
and rolling and compounding the reaction product and a lithium foil to obtain the lithium metal cathode.
Preferably, the melamine foam has a thickness of 1.8 to 2.5mm.
Preferably, the solvent in the aniline solution is a hydrochloric acid solution, and the concentration of the hydrochloric acid solution is 0.5-1.5 mol/L.
Preferably, the standing is performed under ice bath conditions.
Preferably, the standing time is 4 to 8 hours.
Preferably, the reaction is carried out in an ice bath.
Preferably, the reaction time is 10 to 12 hours.
Preferably, the mass ratio of the melamine foam to the aniline to the ammonium persulfate is 1: (3-7): (4-8).
The invention provides a lithium metal negative electrode prepared by the method in the technical scheme.
The invention provides application of the lithium metal negative electrode in the technical scheme in a battery.
The preparation method of the lithium cathode provided by the invention takes melamine foam as a framework, generates a buffer layer material after polyaniline grows in situ, and then rolls the buffer layer material and the lithium metal to obtain the buffer layer lithium metal cathode. The method provided by the invention can synthesize the buffer layer material in situ in a large area, has an elastic function, can expand and compress, adapts to larger volume expansion and weak conductivity, disperses dendritic crystal tip current, homogenizes the concentration of lithium ions, inhibits dendritic crystal growth, and rolls to prepare the lithium metal cathode of the buffer layer so as to enable the buffer layer to be tightly combined with lithium metal. The in-situ buffer layer material prepared by the invention has stronger mechanical modulus, the fiber layer with weak conductivity can disperse the high current density at the tip of the dendritic crystal when the dendritic crystal contacts the fiber, inhibit the growth of the dendritic crystal and homogenize the concentration of lithium ions, and meanwhile, the elastically expandable buffer layer material has larger reserved space, can constrain a large amount of accumulated 'dead lithium' and is suitable for volume expansion.
Drawings
FIG. 1 is a flow chart of a process for preparing a lithium metal anode according to an embodiment of the present invention;
FIG. 2 shows the performance test results of a battery using a lithium metal negative electrode prepared in example 1 of the present invention;
fig. 3 is an SEM picture of a lithium metal negative electrode prepared in example 2 of the present invention after rolling;
fig. 4 is an SEM picture of a lithium metal anode prepared in example 2 of the present invention after testing cycle performance;
fig. 5 shows the performance test results of the battery prepared by the lithium metal negative electrode prepared in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other examples, which may be modified or appreciated by those skilled in the art based on the description of the embodiments, are intended to be within the scope of the present invention. It should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention. In the examples, the methods used were all conventional methods unless otherwise specified.
The process flow for preparing the lithium metal negative electrode provided by the embodiment of the invention is shown in figure 1.
The invention provides a preparation method of a lithium metal negative electrode, which comprises the following steps:
mixing melamine foam and aniline solution, and standing to obtain a mixed solution;
reacting the mixed solution with ammonium persulfate to obtain a reaction product;
and rolling and compounding the reaction product and a lithium foil to obtain the lithium metal cathode.
In the present invention, the melamine foam is preferably a sheet. In the present invention, the melamine foam preferably has a thickness of 1.8 to 2.5mm, more preferably 2 to 2.2mm. In the present invention, the melamine foam is preferably melamine formaldehyde resin, preferably formed by the reaction of formaldehyde and melamine, and the porosity is preferably more than 99.9%. In the present invention, the melamine foam is preferably used in an amount of 15 to 35 pieces, more preferably 28 to 32 pieces, and most preferably 30 pieces.
In the present invention, it is preferable that the melamine foam is ultrasonically cleaned with acetone or alcohol and then used for the preparation of the lithium metal negative electrode. In the present invention, the time for the ultrasonic cleaning is preferably 25 to 35 minutes, more preferably 28 to 32 minutes, and most preferably 30 minutes. In the present invention, the washed melamine foam is preferably dried after the ultrasonic washing is completed, and the drying temperature is preferably 55 to 65 ℃, more preferably 58 to 62 ℃, and most preferably 60 ℃.
In the present invention, the solvent in the aniline solution is preferably a hydrochloric acid solution, more preferably an aqueous hydrochloric acid solution, and the concentration of the hydrochloric acid solution is preferably 0.5 to 1.5mol/L, more preferably 0.8 to 1.2mol/L, and most preferably 1mol/L.
In the present invention, the standing is preferably performed under ice bath conditions, and the standing time is preferably 4 to 8 hours, more preferably 5 to 7 hours, and most preferably 6 hours.
In the present invention, the reaction is preferably carried out in an ice bath, and the reaction time is preferably 10 to 12 hours.
In the present invention, the mass ratio of the melamine foam, aniline and ammonium persulfate is preferably 1: (3-7): (4 to 8), more preferably 1: (4-6): (5 to 7), most preferably 1:5:6.
in the present invention, the melamine foam and the hydrochloric acid solution are preferably used in a ratio of 1g: (350 to 450) mL, more preferably 1g: (380-420) mL, most preferably 1g:400mL.
Polyaniline is a conductive polymer with a single-double bond alternate conjugated structure of pi electrons, and is generated by standing reaction of aniline and ammonium persulfate under an acidic condition, wherein the whole reaction process is preferably carried out under an ice bath condition.
In the present invention, after obtaining the reaction product, preferably, the reaction product is washed and then dried, and the washing reagent is preferably water, and more preferably deionized water; the drying is preferably carried out in a forced air oven; the drying temperature is preferably 55 to 65 ℃, more preferably 58 to 62 ℃, and most preferably 60 ℃.
In the present invention, the thickness of the lithium foil is preferably 30 to 120 micrometers, more preferably 50 to 100 micrometers, and most preferably 60 to 80 micrometers.
In the present invention, the rolling thickness in the rolling process is preferably 200 to 400 micrometers, more preferably 250 to 350 micrometers, and most preferably 300 micrometers. In the invention, the rolling can be single-side rolling or double-side rolling, the single-side rolling is to roll and compound one side surface of the lithium foil with the reaction product, the double-side rolling is to roll and compound two side surfaces of the lithium foil with the reaction product, and the thickness of the lithium foil during the single-side rolling is preferably 40-60 micrometers, more preferably 45-55 micrometers, and most preferably 50 micrometers; the thickness of the lithium foil at the time of double-side rolling is preferably 80 to 120 micrometers, more preferably 90 to 110 micrometers, and most preferably 100 micrometers. In the present invention, the method of double-side rolling preferably includes:
symmetrically placing the reaction product on two sides of the lithium foil to form a reaction product-lithium foil-reaction product structure;
adding an ET diaphragm on the outermost layer of the structure to form a PET-reaction product-lithium foil-reaction product-PET structure;
the rolling thickness of the rolling machine is adjusted to be 300-400 mu m, and the PET diaphragm is torn off after rolling.
In the present invention, the thickness of the PET separator is preferably 70 to 80 micrometers, more preferably 75 micrometers; the rolled thickness is preferably 320 to 380 microns, more preferably 340 to 360 microns, and most preferably 350 microns.
In the present invention, the method of single-side rolling preferably includes:
placing the reaction product on one side of a lithium foil, and adding a PET diaphragm on the outer layers of the lithium foil and the reaction product to form a PET-lithium foil reaction product-PET structure;
adjusting the rolling thickness of a roller press to be 200-300 mu m, and tearing off the PET diaphragm after rolling.
In the present invention, the thickness of the PET separator is the same as that of the PET separator described in the above technical solution, and the rolled thickness is preferably 220 to 280 micrometers, more preferably 240 to 260 micrometers, and most preferably 250 micrometers.
The invention provides a lithium metal cathode prepared by the method in the technical scheme.
The invention provides an application of the metal lithium negative electrode in the technical scheme in a battery, wherein the metal lithium negative electrode is used as a negative electrode in the battery, such as a half battery prepared by matching copper foil.
The preparation method of the lithium cathode provided by the invention takes melamine foam as a framework, generates a buffer layer material after polyaniline grows in situ, and then rolls the buffer layer material and the metal lithium to obtain the buffer layer metal lithium cathode. The method provided by the invention can synthesize the buffer layer material in situ in a large area, has an elastic function, can expand and compress, adapts to larger volume expansion and weak conductivity, disperses dendritic crystal tip current, homogenizes the concentration of lithium ions, inhibits dendritic crystal growth, and prepares the lithium metal cathode of the buffer layer by rolling so that the buffer layer and the lithium metal are tightly combined. The in-situ buffer layer material prepared by the invention has stronger mechanical modulus, the fiber layer with weak conductivity can disperse the high current density at the tip of the dendritic crystal when the dendritic crystal contacts the fiber, inhibit the growth of the dendritic crystal and homogenize the concentration of lithium ions, and meanwhile, the elastically expandable buffer layer material has larger reserved space, can restrict a large amount of accumulated dead lithium and is suitable for volume expansion.
All the raw materials used in the following examples of the present invention are commercially available products, and the melamine foam is melamine formaldehyde resin, which is provided by zheng zhong feng tai nano materials limited company, and has a porosity of more than 99.9%.
Example 1
30 pieces of melamine foam with the thickness of about 1.8mm, the area of 3 x 4cm and the total mass of 0.69g are ultrasonically cleaned by acetone and alcohol for 30 minutes and then placed in a blast drying agent at 60 ℃ for drying for later use, 3.70g of aniline is weighed by an analytical balance and dispersed in 280mL of 1moL/mL hydrochloric acid solution, the melamine foam is added, and the mixture is kept stand for 4 hours under the ice bath condition; weighing 4.10g of ammonium persulfate by using an analytical balance, adding the ammonium persulfate into a hydrochloric acid solution mixed by melamine foam and aniline, fully dissolving, and standing for reaction for 8 hours under an ice bath condition; and taking the elastic buffer layer material prepared after the reaction out of hydrochloric acid, washing the elastic buffer layer material by using deionized water for multiple times, washing excessive polyaniline particles except the surface of the melamine foam framework, and then drying the excessive polyaniline particles in a 60 ℃ blast oven for later use.
Cutting the dried elastic buffer layer material into a round pole piece with the radius of 0.7cm and a lithium foil with the radius of 0.7cm and the thickness of 50 microns, rolling the round pole piece and the lithium foil on one side, assembling the round pole piece and the lithium foil into a PET (75 microns) -lithium foil-buffer layer-PET (75 microns) structure, adjusting the rolling thickness of a rolling machine to be 250 microns, and tearing off a PET diaphragm after rolling to obtain the lithium metal cathode of the single-side buffer layer.
The lithium metal negative electrode prepared in embodiment 1 of the invention is matched with copper foil to prepare a half cell:
the lithium metal negative electrode prepared in example 1 of the present invention was used as a negative electrode, a copper foil 18 μm thick with a radius of 0.7cm as a positive electrode, a PP separator 1cm thick with a radius of 25 μm was assembled (assembly press pressure was 50 MPa); at 1mA/cm 2 、5mAh/cm 2 Cycling test under Current conditions (at 1 mA/cm) 2 Constant current is discharged to 5mAh/cm under the current density 2 The area capacity is then charged by constant current until the voltage reaches 1V, the step is repeatedly circulated for many times, and the test equipment: blue battery test equipment), the detection result is shown in fig. 2, and as can be seen from fig. 2, the half-cell with the buffer layer has good cycling stability and has more stable and higher cycling efficiency compared with the half-cell without the buffer layer.
Example 2
20 pieces of melamine foam having a thickness of about 1.8mm, an area of 5 x 6cm and a total mass of 1.38g were ultrasonically cleaned with acetone or alcohol for 30 minutes, then dried in a blowing drier at 60 ℃ for use, 7.45g of aniline was weighed by an analytical balance and dispersed in 550mL of 1moL/mL hydrochloric acid solution, and melamine foam was added thereto and allowed to stand for 5 hours under ice bath conditions. 8.28g of ammonium persulfate is weighed by an analytical balance and added into a hydrochloric acid solution mixed by melamine foam and aniline, and the mixture is fully dissolved and kept stand for reaction for 10 hours under the ice bath condition. And taking the elastic buffer layer material prepared after the reaction out of hydrochloric acid, washing the elastic buffer layer material by using deionized water for multiple times, washing off excessive polyaniline particles except the surface of the melamine foam framework, and then drying the polyaniline particles in a 60 ℃ blast oven for later use.
Cutting the dried elastic buffer layer material into a lithium foil with the area of 4.7 x 5.7cm and the thickness of 100 microns, performing double-sided rolling, symmetrically placing buffer layers on two sides of the lithium foil to form a buffer layer-lithium foil-buffer layer structure, and adding a PET diaphragm with the thickness of 75 microns on the outermost layer to form a PET-buffer layer-lithium foil-buffer layer-PET structure; and adjusting the rolling thickness of a rolling machine to 350 mu m, and tearing off the PET diaphragm after rolling to obtain the lithium metal cathode with the double-sided buffer layer.
SEM examination was performed on the lithium metal negative electrode prepared after rolling in example 2 of the present invention, and the examination result is shown in fig. 3, and it can be seen from fig. 3 that the buffer layer and the lithium metal are completely roll-combined.
The lithium metal cathode prepared in embodiment 2 of the invention is prepared into a soft package battery with the capacity of 0.9Ah by matching with an NCM811 cathode material, and the cycle performance is detected, wherein the test method comprises the following steps: the soft package battery is cycled under the charge-discharge rate of 0.2C, the charge cut-off voltage is 4.3V, the discharge cut-off voltage is 2.6V, the cycle is repeated for multiple times, the metal lithium cathode after the cycle performance detection is subjected to SEM detection, the detection result is shown in figure 4, and as can be seen from figure 4, the buffer layer is still wrapped by lithium metal after the multiple cycles, and the buffer layer has the expanded elastic performance; as shown in fig. 5, a in fig. 5 is a cell without a buffer layer, and b is a cell with a buffer layer, it can be seen from fig. 5 that the lithium metal cell with a buffer layer has more cycle efficiency, and the lithium metal cell with a buffer layer has more discharge capacity under the condition of not much different cycle times.
The preparation method of the lithium metal cathode can synthesize the buffer layer material in situ in a large area, has an elastic function, can expand and compress, is suitable for larger volume expansion and weak conductivity, disperses dendritic crystal tip current, homogenizes lithium ion concentration, inhibits dendritic crystal growth, and prepares the lithium metal cathode of the buffer layer by rolling so that the buffer layer is tightly combined with lithium metal. The in-situ buffer layer material prepared by the invention has stronger mechanical modulus, the fiber layer with weak conductivity can disperse the high current density at the tip of the dendritic crystal when the dendritic crystal contacts the fiber, inhibit the growth of the dendritic crystal and homogenize the concentration of lithium ions, and meanwhile, the elastically expandable buffer layer material has larger reserved space, can constrain a large amount of accumulated 'dead lithium' and is suitable for volume expansion.
While only the preferred embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (3)
1. A method of making a lithium metal anode, comprising:
ultrasonically cleaning 20 melamine foam sheets with the thickness of 1.8mm, the area of 5 x 6cm and the total mass of 1.38g by using acetone and alcohol for 30 minutes, then placing the cleaned melamine foam sheets into a blowing drying agent at 60 ℃ for drying for later use, weighing 7.45g of aniline by using an analytical balance, dispersing the aniline into 550mL of 1moL/mL hydrochloric acid solution, adding the melamine foam, and standing for 5 hours under the ice bath condition; weighing 8.28g of ammonium persulfate by using an analytical balance, adding the ammonium persulfate into a hydrochloric acid solution mixed by melamine foam and aniline, fully dissolving, and standing for reaction for 10 hours under an ice bath condition; taking the elastic buffer layer material prepared after the reaction out of hydrochloric acid, washing the elastic buffer layer material with deionized water for multiple times, washing off excessive polyaniline particles except the surface of the melamine foam skeleton, and then drying the excessive polyaniline particles in a 60 ℃ blast oven for later use;
cutting the dried elastic buffer layer material to the size of 4.7 x 5.7cm, adopting a lithium foil with the thickness of 100 microns, symmetrically arranging buffer layers on two surfaces of the lithium foil to form a buffer layer-lithium foil-buffer layer structure, and adding a PET diaphragm with the thickness of 75 microns on the outermost layer to form a PET-buffer layer-lithium foil-buffer layer-PET structure; and (4) carrying out double-sided rolling, adjusting the rolling thickness of a rolling machine to be 350 mu m, and tearing off the PET diaphragm after rolling to obtain the lithium metal cathode with the double-sided buffer layer.
2. A lithium metal negative electrode prepared by the method of claim 1.
3. Use of the lithium metal anode of claim 2 in a battery.
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| CN102130323B (en) * | 2011-02-12 | 2013-02-13 | 中南大学 | Lithium ion battery film cathode containing porous polymer elastomer and preparation method thereof |
| CN106340616B (en) * | 2016-09-30 | 2019-08-06 | 上海空间电源研究所 | A kind of cathode of lithium and preparation method thereof with sandwich structure for lithium battery |
| CN107579204A (en) * | 2017-08-28 | 2018-01-12 | 珠海光宇电池有限公司 | Lithium anode piece and preparation method thereof and lithium metal secondary battery |
| CN108232117A (en) * | 2018-01-27 | 2018-06-29 | 浙江大学 | A kind of lithium metal battery negative material and its preparation method and application |
| CN109728242B (en) * | 2019-01-02 | 2021-06-01 | 重庆天齐锂业有限责任公司 | Three-dimensional alloy lithium negative electrode, preparation method thereof and lithium secondary battery |
| CN109817894B (en) * | 2019-02-28 | 2021-05-14 | 厦门大学 | Negative electrode for lithium metal battery and preparation method and application thereof |
| CN110649267B (en) * | 2019-08-20 | 2021-05-18 | 北京泰丰先行新能源科技有限公司 | Composite metal lithium cathode, preparation method and metal lithium battery |
| CN110931712B (en) * | 2019-12-10 | 2021-01-01 | 清华大学 | Composite metal lithium cathode with filler and preparation method thereof |
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