CN111916755A - Preparation method of carbon film coated three-dimensional current collector - Google Patents
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- 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
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- 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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- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
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- H01M4/74—Meshes or woven material; Expanded metal
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Abstract
The invention provides a preparation method of a three-dimensional current collector coated by a carbon film, which comprises the following steps: s1) adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector; s2) carrying out high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain the carbon film-coated three-dimensional current collector. Compared with the prior art, the interface modification on the three-dimensional current collector is realized in an electropolymerization and carbonization mode, so that a conductive high polymer material which is beneficial to forming a stable SEI film is formed on the three-dimensional current collector, a certain space is formed between the three-dimensional current collector and a carbon film in a carbonization process, the expansion is relieved, the deposition of metal lithium in a limited region can be limited, and the lithium deposition is blocked by the carbon film in the limited region space, so that the contact between the lithium and an electrolyte can be reduced; meanwhile, the thickness of the carbon film precursor can be adjusted through concentration and electropolymerization conditions, so that the thickness of the carbon film can be adjusted.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a carbon film coated three-dimensional current collector.
Background
Commercial lithium ion batteries have been widely used since their introduction in 1991, and many researchers have therefore put more effort into the study of lithium ion batteries. However, due to the limitation of energy density of lithium ion batteries, the increasing demand of people cannot be met, the specific energy of the lithium ion battery is 250Wh/kg at present, and the specific energy of the lithium sulfur battery and the lithium air battery can reach 650Wh/kg and 950Wh/kg respectively, so that the metal lithium with high specific capacity (3860Wh/kg), low standard oxidation-reduction potential (-3.045V) and low atomic weight becomes an ideal negative electrode of the next-generation lithium secondary battery.
However, in the lithium battery, dendritic metallic lithium, i.e., lithium dendrite, is easily formed on the surface of the negative electrode during repeated deposition and precipitation of lithium ions during reduction thereof during charging. The uneven deposition of lithium metal in the circulation process leads to the formation of dendritic crystals to cause infinite volume expansion effect, so that the lithium metal body is broken, the SEI film is broken, fresh lithium reacts with electrolyte to regenerate, the electrolyte is consumed, and active metal lithium is lost.
Currently, the generation of lithium dendrites is often improved by: coating high molecules, such as PVDF, PEO, PVA, PAN and other high molecular materials on the plane copper; or coating the copper with an inorganic material such as LLZTO, MOF, etc. However, the coating of the polymer material is not favorable for forming a stable SEI film, is chemically active with respect to lithium, causes some side reactions, and is not easily controllable in thickness, and at the same time, the polymer material is easily oxidized under high voltage conditions, resulting in instability thereof, and moreover, the coating method is only suitable for realizing a uniform operation on a planar structure, and is not favorable for operating on a more optimized three-dimensional current collector.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing a continuous, uniform, non-equipotential carbon film-coated three-dimensional current collector.
The invention provides a preparation method of a three-dimensional current collector coated by a carbon film, which comprises the following steps:
s1) adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector;
s2) carrying out high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain the carbon film-coated three-dimensional current collector.
Preferably, the polymer precursor is selected from one or more of pyrrole, aniline, thiophene and acetylene.
Preferably, the concentration of the polymer precursor in the electrolyte is 0.05-0.5 mol/L.
Preferably, the electrolyte further comprises an electrolyte; the concentration of the electrolyte in the electrolyte is 0.05-1 mol/L.
Preferably, the electrolyte is selected from one or more of p-toluenesulfonic acid, sodium toluene sulfonate, phytic acid, dodecylbenzene sulfonic acid and sodium dodecylbenzene sulfonate; the three-dimensional current collector is selected from an iron net, a stainless steel net, a titanium net, a molybdenum net, foamed nickel, carbon fiber cloth or carbon cloth.
Preferably, the potential of the electrochemical polymerization is 0.5-1V; the time of the electrochemical polymerization is 1-60 min.
Preferably, the temperature of the high-temperature carbonization is 400-1000 ℃; the high-temperature carbonization time is 1-2 h.
The invention also provides a carbon film coated three-dimensional current collector prepared by the preparation method; the surface of the three-dimensional current collector is coated with a continuous and uniform non-equipotential carbon film; and a gap is arranged between the non-equipotential carbon film and the three-dimensional current collector.
Preferably, the non-equipotential carbon film is doped with heteroatoms.
Preferably, the distance between the non-equipotential carbon film and the three-dimensional current collector is 1-5 μm.
The invention provides a preparation method of a three-dimensional current collector coated by a carbon film, which comprises the following steps: s1) adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector; s2) carrying out high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain the carbon film-coated three-dimensional current collector. Compared with the prior art, the interface modification on the three-dimensional current collector is realized by electropolymerization and carbonization, so that a continuous and uniform conductive high polymer material which is chemically inert to lithium and is beneficial to forming a stable SEI film is formed on the three-dimensional current collector, a certain space is formed between the three-dimensional current collector and a carbon film through the carbonization process, the expansion is relieved, the deposition of metallic lithium can be limited, the lithium deposition is blocked by the carbon film in the limited space, and the contact between the lithium and an electrolyte can be reduced; meanwhile, the preparation method is simple, and the thickness of the carbon film precursor can be adjusted through concentration and electropolymerization conditions, so that the thickness of the carbon film can be adjusted.
Drawings
Fig. 1 is a cross-sectional scanning electron microscope image of a carbon film-coated three-dimensional current collector obtained in example 1 of the present invention;
fig. 2 is a scanning electron microscope image of the carbon film-coated three-dimensional current collector obtained in example 1 of the present invention after lithium deposition;
FIG. 3 is a scanning electron microscope photograph of the stainless steel net after being washed in example 2 of the present invention;
fig. 4 is a coulomb efficiency test graph of the carbon film coated three-dimensional current collector and the uncoated three-dimensional current collector obtained in example 1 of the present invention;
fig. 5 is a scanning electron micrograph of an uncoated three-dimensional current collector after cycling in example 1 of the present invention;
fig. 6 is a scanning electron microscope image of the carbon film-coated three-dimensional current collector after circulation in example 1 of the present invention;
fig. 7 is a scanning electron microscope image of a carbon film-coated three-dimensional current collector obtained in example 2 of the present invention;
FIG. 8 is a scanning electron micrograph of nickel foam after cleaning in example 3 of the present invention;
fig. 9 is a scanning electron microscope image of the carbon film-coated three-dimensional current collector obtained in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, 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 embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a three-dimensional current collector coated by a carbon film, which comprises the following steps: s1) adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector; s2) carrying out high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain the carbon film-coated three-dimensional current collector.
In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available.
Adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector; the three-electrode system comprises a working electrode, a counter electrode and a reference electrode; the counter electrode is preferably a stainless steel sheet; the reference electrode is preferably silver/silver chloride; the working electrode is a three-dimensional current collector; the three-dimensional current collector is preferably a three-dimensional metal except copper or a conductive other non-metallic three-dimensional material, and more preferably an iron net, a stainless steel net, a titanium net, a molybdenum net, foamed nickel, carbon fiber cloth or carbon cloth; the polymer precursor is a conductive electropolymerizable polymer precursor, preferably contains one or more of pyrrole (Py), aniline, thiophene and acetylene, more preferably contains heteroatoms, and can realize doping of O, N, S and other different elements, so that the carbon film has heteroatom doping, the carbon film has polarity, and the lithium ion flux can be adjusted; the concentration of the polymer precursor in the electrolyte is 0.05-0.5 mol/L, more preferably 0.05-0.4 mol/L, still more preferably 0.1-0.3 mol/L, and most preferably 0.1-0.2 mol/L; deionized water is preferably used as a solvent for the electrolyte provided by the invention; the electrolyte preferably further comprises an electrolyte; the concentration of the electrolyte in the electrolyte is preferably 0.05-1 mol/L, more preferably 0.1-0.8 mol/L, still more preferably 0.1-0.6 mol/L, still more preferably 0.1-0.4 mol/L, and most preferably 0.2-0.3 mol/L; the electrolyte is preferably one or more of p-toluenesulfonic acid (PTs), sodium toluene sulfonate, phytic acid, dodecylbenzene sulfonic acid and sodium dodecylbenzene sulfonate; the electrochemical polymerization can be constant current polymerization or constant potential polymerization, and is preferably constant potential polymerization in the invention; the potential of the electrochemical polymerization is preferably 0.5-1V, and more preferably 0.6-0.8V; the time of the electrochemical polymerization is preferably 1-60 min, more preferably 5-50 min, still more preferably 6-40 min, still more preferably 6-30 min, still more preferably 6-20 min, and most preferably 6-15 min. Through electrochemical polymerization, a continuous and uniform conductive polymer film can be formed on the surface of the three-dimensional current collector.
Performing high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain a carbon film-coated three-dimensional current collector; the formed continuous and uniform conductive polymer film is carbonized, and a certain mass loss is generated due to the carbonization of a polymer material, so that the formed carbon film is randomly contacted with the three-dimensional current collector substrate to form an equipotential body, and lithium ions are easy to obtain electron deposition on the three-dimensional current collector substrate, namely in a gap between the carbon film and the three-dimensional current collector substrate, and the lithium is deposited in the space, so that the deposition of the lithium is limited, and the expansion can be relieved; the high-temperature carbonization temperature is preferably 400-1000 ℃, more preferably 600-900 ℃, and further preferably 650-800 ℃; the high-temperature carbonization time is preferably 1-2 h, and more preferably 1 h.
According to the invention, interface modification is carried out on the three-dimensional current collector in an electropolymerization and carbonization mode, so that a continuous and uniform conductive high polymer material which is chemically inert to lithium and is beneficial to forming a stable SEI film is formed on the three-dimensional current collector, a certain space is formed between the three-dimensional current collector and a carbon film in a carbonization process, expansion is relieved, the deposition of metal lithium can be limited, and the contact between lithium and electrolyte can be reduced because the lithium is deposited in the limited space and blocked by the carbon film; meanwhile, the preparation method is simple, and the thickness of the carbon film precursor can be adjusted through concentration and electropolymerization conditions, so that the thickness of the carbon film can be adjusted.
The invention also provides a carbon film coated three-dimensional current collector prepared by the method, wherein the surface of the three-dimensional current collector is coated with a continuous and uniform non-equipotential carbon film; a gap is arranged between the non-equipotential carbon film and the three-dimensional current collector; the non-equipotential carbon film coated on the surface of the three-dimensional current collector is preferably a tubular or shell-shaped uniform carbon film; gaps are formed between the non-equipotential carbon film and the three-dimensional current collector to form a lithium confinement space, and the distance between the non-equipotential carbon film and the three-dimensional current collector is preferably 1-5 micrometers.
According to the present invention, the non-equipotential carbon film is preferably doped with a heteroatom, and more preferably with an O atom, so that the carbon film has a C ═ O bond, which is advantageous for forming a stable SEI, thereby reducing side reactions of the electrolyte.
In order to further illustrate the present invention, the following describes in detail a method for preparing a carbon film coated three-dimensional current collector provided by the present invention with reference to examples.
The reagents used in the following examples are all commercially available.
Example 1
1) And ultrasonically cleaning the stainless steel net with ethanol.
2) Preparing electrolyte solution for electropolymerization, taking deionized water as a solvent, containing 0.1MPy and 0.2MPTs, adopting a three-electrode mode, taking a stainless steel net as a working electrode, a stainless steel sheet as a counter electrode and silver/silver chloride as a reference electrode, and carrying out 0.6V constant potential electropolymerization for 6 min.
3) The obtained material is carbonized for 1h at 650 ℃ to obtain a uniform and continuous shell-shaped or tubular carbon film-coated three-dimensional current collector doped with heteroatoms and non-equipotential bodies.
The cross section of the carbon film-coated three-dimensional current collector obtained in example 1 was analyzed by scanning electron microscopy, and a scanning electron microscopy image thereof was obtained as shown in fig. 1.
The carbon film-coated three-dimensional current collector obtained in example 1 was assembled into a lithium/current collector half cell (lithium sheets purchased from tianjin, a 500 μm thick lithium sheet with a diameter of 16mm was used as a negative electrode, the diameter of the three-dimensional current collector was 14mm, the separator was commercially available as a separator, which was 25 μm thick, and the electrolyte was Li — S electrolyte containing 1% of LiNO3). The deposition of lithium was carried out, and an electron micrograph of the lithium deposited was observed by a scanning electron microscope, as shown in FIG. 2. As can be seen from fig. 2, lithium is deposited between the carbon film and the three-dimensional current collector substrate.
Three-dimensional current collector coated with carbon film obtained in example 1Assembling the half-cell of the lithium/current collector, and simultaneously, performing coulombic efficiency test on the half-cell of the lithium/current collector assembled by the three-dimensional current collector which is not coated by the carbon film as comparison, wherein the coulombic efficiency test condition is 0.5mAcm-2Current density deposition 0.5mAh cm-2Charging the lithium to 1V, dissolving out all the lithium, and testing the coulombic efficiency; a coulombic efficiency test graph was obtained as shown in fig. 3. As can be seen from fig. 3, the phenomenon of overcharge of the unmodified current collector indicates that the dendrite grows to decompose the electrolyte, the phenomenon of overcharge caused by side reactions causes the coulombic efficiency of the unmodified current collector to be greater than 100%, and the coulombic efficiency of the unmodified current collector fluctuates seriously, indicating that nucleation and growth of lithium and subsequent dissolution are very non-uniform. In contrast, for carbon film coated current collectors, coulombic efficiency was stable with no fluctuations, indicating a stable interface and more uniform deposition and dissolution of lithium.
The current collector subjected to the coulombic efficiency (50 cycles) test is analyzed by a scanning electron microscope, and scanning electron micrographs of the current collector are shown in fig. 4 and 5. As can be seen from fig. 4, dendritic growth occurs on the unmodified current collector, and the large volume expansion may destroy the original SEI layer, which may cause the side reaction between lithium and the electrolyte to be aggravated, and the result may also be known from coulombic efficiency; as can be seen from fig. 5, the surface of the current collector coated with the carbon film has no dendritic lithium, and maintains the original structure of the carbon film, which illustrates the stability of the interface. The side reaction of the electrolyte can be isolated, the coulombic efficiency structure comparison can be carried out, the contrast can also be obvious, the stability of the carbon film enables the growth limited range of lithium, so that the side reaction with the lithium is reduced, and the carbon film is kept stable after circulation.
Example 2
1) And ultrasonically cleaning the stainless steel net with ethanol.
2) Preparing electrolyte solution for electropolymerization, taking deionized water as a solvent, containing 0.1MPy and 0.2MPTs, adopting a three-electrode mode, taking a stainless steel net as a working electrode, a stainless steel sheet as a counter electrode and silver/silver chloride as a reference electrode, and carrying out 0.6V constant potential electropolymerization for 15 min.
3) Carbonizing the obtained material at 800 ℃ for 1h to obtain a uniform and continuous shell-shaped or tubular carbon film-coated three-dimensional current collector doped with heteroatoms and non-equipotential bodies.
The stainless steel mesh cleaned in example 2 was analyzed by scanning electron microscopy to obtain a scanning electron micrograph, which is shown in FIG. 6.
The carbon-film-coated three-dimensional current collector obtained in example 2 was analyzed by scanning electron microscopy to obtain a scanning electron micrograph, as shown in fig. 7.
Example 3
1) The foamed nickel was ultrasonically cleaned with ethanol.
2) Preparing electrolyte solution for electropolymerization, taking deionized water as a solvent, containing 0.1MPy and 0.2MPTs, adopting a three-electrode mode, taking foamed nickel as a working electrode, a stainless steel sheet as a counter electrode and silver chloride as reference electrodes, and carrying out 0.6V constant potential electropolymerization for 15 min.
3) The obtained material is carbonized at 800 ℃ to obtain a uniform and continuous shell-shaped or tubular carbon film-coated three-dimensional current collector doped with heteroatoms and non-equipotential bodies.
The stainless steel cleaned in example 3 was analyzed by scanning electron microscopy, and a scanning electron micrograph thereof was obtained as shown in fig. 8.
The carbon-film-coated three-dimensional current collector obtained in example 3 was analyzed by scanning electron microscopy to obtain a scanning electron microscopy image, as shown in fig. 9. It can be seen from fig. 9 that the surface of the carbon film-coated nickel foam is smoother.
Claims (10)
1. A method for preparing a carbon film coated three-dimensional current collector is characterized by comprising the following steps:
s1) adopting a three-electrode system, taking a three-dimensional current collector as a working electrode, and carrying out electrochemical polymerization in electrolyte containing a polymer precursor to obtain a polymer-coated three-dimensional current collector;
s2) carrying out high-temperature carbonization on the polymer-coated three-dimensional current collector to obtain the carbon film-coated three-dimensional current collector.
2. The method according to claim 1, wherein the polymer precursor is one or more selected from pyrrole, aniline, thiophene, and acetylene.
3. The preparation method according to claim 1, wherein the concentration of the polymer precursor in the electrolyte is 0.05-0.5 mol/L.
4. The method according to claim 1, wherein the electrolyte solution further comprises an electrolyte; the concentration of the electrolyte in the electrolyte is 0.05-1 mol/L.
5. The method according to claim 4, wherein the electrolyte is selected from one or more of p-toluenesulfonic acid, sodium toluenesulfonate, phytic acid, dodecylbenzenesulfonic acid and sodium dodecylbenzenesulfonate; the three-dimensional current collector is selected from an iron net, a stainless steel net, a titanium net, a molybdenum net, foamed nickel, carbon fiber cloth or carbon cloth.
6. The method according to claim 1, wherein the potential of the electrochemical polymerization is 0.5 to 1V; the time of the electrochemical polymerization is 1-60 min.
7. The preparation method according to claim 1, wherein the temperature of the high-temperature carbonization is 400 to 1000 ℃; the high-temperature carbonization time is 1-2 h.
8. The carbon film coated three-dimensional current collector prepared by any one of the preparation methods of claims 1 to 7, wherein the surface of the three-dimensional current collector is coated with a continuous and uniform non-equipotential carbon film; and a gap is arranged between the non-equipotential carbon film and the three-dimensional current collector.
9. The carbon film coated three-dimensional current collector of claim 8, wherein the non-equipotential carbon film is doped with heteroatoms.
10. The carbon film coated three-dimensional current collector as claimed in claim 8, wherein the distance between the non-equipotential carbon film and the three-dimensional current collector is 1-5 μm.
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| CN112599780A (en) * | 2020-12-14 | 2021-04-02 | 中国科学院过程工程研究所 | Method for modifying surface of current collector of lithium slurry battery |
| CN114068943A (en) * | 2021-09-24 | 2022-02-18 | 恒大新能源技术(深圳)有限公司 | Current collector, preparation method thereof and lithium ion battery |
| WO2022198583A1 (en) * | 2021-03-25 | 2022-09-29 | 宁德新能源科技有限公司 | Carbon current collector, electrochemical device comprising carbon current collector, and electronic device |
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